+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0011 started at 13:34:13 on 05-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0011 in P2(1) CELL 0.71073 9.3955 4.8267 10.9702 90.000 104.999 90.000 ZERR 2.00 0.0005 0.0002 0.0005 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 18 24 8 2 V = 480.54 F(000) = 204.0 Mu = 0.09 mm-1 Cell Wt = 384.45 Rho = 1.328 MERG 4 OMIT -3.00 55.00 DFIX 0.88 0.02 N4 H1N N4 H2N DFIX 0.84 0.02 O1 H1O O1 H2O FMAP 2 PLAN 5 SIZE 0.02 0.02 0.30 ACTA EQIV $1 x + 1, y, z EQIV $2 -x + 1, y -1/2, -z + 2 HTAB O1 N3 HTAB O1 N4_$2 HTAB N4 O1_$1 HTAB N4 O1_$2 BOND $H WGHT 0.00750 0.47020 L.S. 6 EXTI TEMP -153.00 FVAR 1.61265 MOLE 1 C1 1 0.373654 0.578675 0.752237 11.00000 0.02347 0.02865 = 0.03471 0.00347 0.00850 0.00331 AFIX 43 H1 2 0.300861 0.719023 0.743833 11.00000 -1.20000 AFIX 0 C2 1 0.505676 0.236312 0.822089 11.00000 0.02696 0.02867 = 0.02899 0.00118 0.00960 -0.00204 AFIX 43 H2 2 0.550290 0.081419 0.870611 11.00000 -1.20000 AFIX 0 C3 1 0.654607 0.230770 0.658964 11.00000 0.02524 0.02428 = 0.02275 -0.00593 0.00633 0.00292 AFIX 23 H3A 2 0.604587 0.180998 0.570727 11.00000 -1.20000 H3B 2 0.700431 0.060767 0.702470 11.00000 -1.20000 AFIX 0 C4 1 0.773216 0.441425 0.659217 11.00000 0.02252 0.02121 = 0.02639 -0.00076 0.01250 0.00554 C5 1 0.885784 0.493525 0.767815 11.00000 0.02057 0.02171 = 0.02549 0.00112 0.01007 0.00278 C6 1 0.990228 0.698536 0.764530 11.00000 0.02242 0.02436 = 0.02833 -0.00242 0.00640 -0.00128 AFIX 43 H6 2 1.066563 0.736358 0.838323 11.00000 -1.20000 AFIX 0 C7 1 0.983752 0.846003 0.655777 11.00000 0.02670 0.02249 = 0.03092 0.00269 0.01603 0.00475 AFIX 43 H7 2 1.055420 0.984461 0.655143 11.00000 -1.20000 AFIX 0 C8 1 0.873077 0.793386 0.547113 11.00000 0.03090 0.02766 = 0.02454 0.00400 0.01392 0.00727 AFIX 43 H8 2 0.868739 0.893741 0.471743 11.00000 -1.20000 AFIX 0 C9 1 0.769469 0.593000 0.550322 11.00000 0.02524 0.02769 = 0.02295 -0.00419 0.01000 0.00492 AFIX 43 H9 2 0.693331 0.557263 0.476135 11.00000 -1.20000 AFIX 0 N1 3 0.544400 0.335934 0.722109 11.00000 0.02072 0.02319 = 0.02073 -0.00160 0.00503 0.00002 N2 3 0.459721 0.559888 0.675305 11.00000 0.02504 0.02895 = 0.02974 0.00524 0.00963 0.00425 N3 3 0.395817 0.384173 0.844388 11.00000 0.02800 0.03430 = 0.03524 0.00168 0.01341 0.00206 N4 3 0.893109 0.359625 0.883318 11.00000 0.02554 0.01850 = 0.02482 0.00065 0.00769 0.00220 H1N 2 0.983013 0.334728 0.934093 11.00000 0.05501 H2N 2 0.850423 0.193694 0.878518 11.00000 0.03585 MOLE 2 O1 4 0.227679 0.336256 1.024444 11.00000 0.03122 0.02632 = 0.03060 -0.00166 0.01469 -0.00242 H1O 2 0.277332 0.317310 0.970029 11.00000 -1.50000 H2O 2 0.197876 0.174968 1.040203 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2007jmw0011 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - N2 N3 C2 - N3 N1 C3 - N1 C4 C4 - C9 C5 C3 C5 - C4 C6 N4 C6 - C7 C5 C7 - C6 C8 C8 - C9 C7 C9 - C8 C4 N1 - C2 N2 C3 N2 - C1 N1 N3 - C2 C1 N4 - C5 O1 - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+1, y-1/2, -z+2 Floating origin restraints generated 6107 Reflections read, of which 7 rejected -12 =< h =< 12, -6 =< k =< 5, -14 =< l =< 14, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1229 Unique reflections, of which 0 suppressed R(int) = 0.0569 R(sigma) = 0.0492 Friedel opposites merged Maximum memory for data reduction = 1601 / 12219 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 = 1983 / 178556 wR2 = 0.1124 before cycle 1 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.152; Restrained GooF = 1.150 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.61813 0.00639 0.859 OSF 2 0.01822 0.00699 2.607 EXTI Mean shift/esd = 0.188 Maximum = 2.607 for EXTI Max. shift = 0.039 A for H1O Max. dU =-0.002 for H2N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1983 / 178556 wR2 = 0.1109 before cycle 2 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.136; Restrained GooF = 1.134 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.62053 0.00641 0.375 OSF 2 0.02675 0.00763 1.119 EXTI Mean shift/esd = 0.063 Maximum = 1.119 for EXTI Max. shift = 0.009 A for H1O Max. dU =-0.001 for H2N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1983 / 178556 wR2 = 0.1107 before cycle 3 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.134; Restrained GooF = 1.132 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.62077 0.00645 0.036 OSF 2 0.02724 0.00796 0.061 EXTI Mean shift/esd = 0.006 Maximum = 0.061 for EXTI Max. shift = 0.001 A for H2O Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1983 / 178556 wR2 = 0.1107 before cycle 4 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.133; Restrained GooF = 1.131 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.62078 0.00645 0.002 OSF 2 0.02726 0.00798 0.002 EXTI Mean shift/esd = 0.002 Maximum = -0.008 for y H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1983 / 178556 wR2 = 0.1107 before cycle 5 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.133; Restrained GooF = 1.131 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.62078 0.00645 0.000 OSF 2 0.02726 0.00798 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for z H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1983 / 178556 wR2 = 0.1107 before cycle 6 for 1229 data and 142 / 142 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.133; Restrained GooF = 1.131 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.62078 0.00645 0.000 OSF 2 0.02726 0.00798 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H2N Largest correlation matrix elements 0.737 z H1O / x H1O 0.695 EXTI / OSF -0.546 y H2N / x H2N Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.3010 0.7192 0.7439 43 0.950 0.000 C1 N2 N3 H2 0.5506 0.0820 0.8708 43 0.950 0.000 C2 N3 N1 H3A 0.6047 0.1809 0.5708 23 0.990 0.000 C3 N1 C4 H3B 0.7006 0.0610 0.7026 23 0.990 0.000 C3 N1 C4 H6 1.0664 0.7367 0.8382 43 0.950 0.000 C6 C7 C5 H7 1.0555 0.9841 0.6552 43 0.950 0.000 C7 C6 C8 H8 0.8688 0.8940 0.4718 43 0.950 0.000 C8 C9 C7 H9 0.6934 0.5567 0.4760 43 0.950 0.000 C9 C8 C4 2007jmw0011 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37368 0.57875 0.75231 1.00000 0.02365 0.02878 0.03572 0.00348 0.00894 0.00373 0.02915 0.00744 0.00039 0.00092 0.00034 0.00000 0.00170 0.00214 0.00204 0.00193 0.00157 0.00177 0.00088 H1 0.30096 0.71922 0.74395 1.00000 0.03498 0.00000 0.00000 C2 0.50580 0.23659 0.82221 1.00000 0.02789 0.02884 0.02897 0.00154 0.00853 -0.00180 0.02835 0.00728 0.00039 0.00089 0.00034 0.00000 0.00181 0.00210 0.00182 0.00178 0.00149 0.00182 0.00085 H2 0.55060 0.08196 0.87083 1.00000 0.03402 0.00000 0.00000 C3 0.65471 0.23092 0.65904 1.00000 0.02443 0.02389 0.02343 -0.00596 0.00649 0.00263 0.02386 0.00691 0.00036 0.00085 0.00032 0.00000 0.00171 0.00194 0.00166 0.00166 0.00140 0.00168 0.00080 H3A 0.60471 0.18094 0.57082 1.00000 0.02863 0.00000 0.00000 H3B 0.70061 0.06104 0.70261 1.00000 0.02863 0.00000 0.00000 C4 0.77308 0.44135 0.65917 1.00000 0.02235 0.02117 0.02596 -0.00024 0.01248 0.00589 0.02201 0.00691 0.00037 0.00076 0.00032 0.00000 0.00167 0.00181 0.00174 0.00153 0.00143 0.00149 0.00079 C5 0.88582 0.49336 0.76790 1.00000 0.02016 0.02176 0.02512 0.00085 0.00968 0.00278 0.02164 0.00676 0.00037 0.00079 0.00032 0.00000 0.00163 0.00194 0.00172 0.00158 0.00141 0.00154 0.00079 C6 0.99013 0.69862 0.76444 1.00000 0.02139 0.02369 0.02885 -0.00238 0.00681 -0.00076 0.02459 0.00712 0.00038 0.00083 0.00033 0.00000 0.00173 0.00194 0.00183 0.00178 0.00143 0.00161 0.00082 H6 1.06639 0.73674 0.83825 1.00000 0.02950 0.00000 0.00000 C7 0.98378 0.84581 0.65579 1.00000 0.02633 0.02278 0.03094 0.00234 0.01617 0.00408 0.02506 0.00738 0.00037 0.00091 0.00032 0.00000 0.00165 0.00179 0.00176 0.00181 0.00147 0.00181 0.00077 H7 1.05554 0.98409 0.65517 1.00000 0.03007 0.00000 0.00000 C8 0.87318 0.79343 0.54715 1.00000 0.03019 0.02862 0.02505 0.00477 0.01403 0.00752 0.02668 0.00725 0.00038 0.00083 0.00032 0.00000 0.00184 0.00228 0.00170 0.00165 0.00147 0.00168 0.00088 H8 0.86884 0.89398 0.47183 1.00000 0.03202 0.00000 0.00000 C9 0.76945 0.59268 0.55027 1.00000 0.02616 0.02807 0.02297 -0.00364 0.00988 0.00553 0.02508 0.00721 0.00038 0.00085 0.00032 0.00000 0.00174 0.00206 0.00177 0.00168 0.00147 0.00181 0.00084 H9 0.69344 0.55673 0.47602 1.00000 0.03010 0.00000 0.00000 N1 0.54437 0.33605 0.72219 1.00000 0.02088 0.02388 0.02038 -0.00153 0.00522 -0.00002 0.02173 0.00549 0.00029 0.00072 0.00024 0.00000 0.00132 0.00154 0.00131 0.00146 0.00108 0.00139 0.00064 N2 0.45973 0.55995 0.67528 1.00000 0.02422 0.02864 0.03025 0.00610 0.00968 0.00426 0.02721 0.00622 0.00031 0.00073 0.00028 0.00000 0.00148 0.00180 0.00161 0.00156 0.00127 0.00148 0.00075 N3 0.39573 0.38417 0.84446 1.00000 0.02831 0.03362 0.03499 0.00117 0.01387 0.00189 0.03126 0.00631 0.00032 0.00078 0.00029 0.00000 0.00159 0.00219 0.00170 0.00162 0.00135 0.00164 0.00083 N4 0.89306 0.35946 0.88329 1.00000 0.02546 0.01886 0.02464 -0.00034 0.00752 0.00150 0.02280 0.00618 0.00033 0.00075 0.00028 0.00000 0.00152 0.00159 0.00145 0.00153 0.00125 0.00159 0.00066 H1N 0.98374 0.34331 0.93353 1.00000 0.05460 0.08165 0.00271 0.01370 0.00316 0.00000 0.01409 H2N 0.85044 0.19403 0.87812 1.00000 0.03360 0.05826 0.00408 0.00548 0.00375 0.00000 0.01186 O1 0.22774 0.33635 1.02449 1.00000 0.03116 0.02580 0.03154 -0.00125 0.01505 -0.00254 0.02822 0.00525 0.00028 0.00063 0.00024 0.00000 0.00139 0.00145 0.00139 0.00143 0.00108 0.00141 0.00063 H1O 0.27640 0.32668 0.96891 1.00000 0.04232 0.08527 0.00384 0.01196 0.00296 0.00000 0.00000 H2O 0.19703 0.17693 1.03934 1.00000 0.04232 0.07341 0.00456 0.00558 0.00407 0.00000 0.00000 Final Structure Factor Calculation for 2007jmw0011 in P2(1) Total number of l.s. parameters = 142 Maximum vector length = 511 Memory required = 1843 / 25046 wR2 = 0.1107 before cycle 7 for 1229 data and 2 / 142 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.133; Restrained GooF = 1.131 for 5 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0075 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0553 for 1014 Fo > 4sig(Fo) and 0.0755 for all 1229 data wR2 = 0.1107, GooF = S = 1.133, Restrained GooF = 1.131 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0372 0.0287 0.0215 C1 0.0308 0.0294 0.0249 C2 0.0310 0.0244 0.0162 C3 0.0305 0.0235 0.0120 C4 0.0271 0.0220 0.0159 C5 0.0298 0.0228 0.0211 C6 0.0369 0.0223 0.0159 C7 0.0395 0.0228 0.0178 C8 0.0331 0.0268 0.0153 C9 0.0245 0.0209 0.0198 N1 0.0364 0.0237 0.0216 N2 0.0378 0.0330 0.0230 N3 0.0261 0.0239 0.0184 N4 0.0373 0.0256 0.0217 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.036 0.048 0.060 0.072 0.090 0.111 0.139 0.202 1.000 Number in group 132. 116. 123. 126. 119. 130. 118. 120. 121. 124. GooF 1.178 1.322 1.310 1.228 1.095 1.106 1.090 0.896 1.020 1.016 K 1.715 1.336 1.037 1.055 1.020 0.996 0.987 0.993 1.016 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.34 1.71 inf Number in group 125. 125. 119. 124. 124. 122. 125. 119. 122. 124. GooF 1.261 1.401 1.314 1.232 1.052 1.133 0.952 0.828 0.955 1.066 K 1.026 1.175 1.106 1.042 1.009 0.995 0.981 0.989 1.030 1.001 R1 0.228 0.215 0.174 0.115 0.083 0.073 0.044 0.035 0.035 0.023 Recommended weighting scheme: WGHT 0.0000 0.4718 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 5 7 2.85 15.67 3.74 0.063 0.78 3 2 11 18.89 4.73 3.27 0.035 0.81 -6 3 9 0.19 8.38 2.95 0.046 0.89 -9 3 6 34.05 11.59 2.90 0.055 0.85 7 1 8 21.88 11.50 2.87 0.054 0.81 -4 3 12 4.94 15.61 2.81 0.063 0.79 -8 3 6 18.50 4.71 2.79 0.035 0.90 8 3 1 -2.40 4.98 2.78 0.036 0.91 -2 5 6 23.04 2.95 2.78 0.028 0.85 5 3 7 14.68 0.47 2.73 0.011 0.87 11 2 0 18.51 4.31 2.72 0.033 0.78 -2 0 13 15.13 2.38 2.69 0.025 0.84 6 3 6 31.74 16.49 2.67 0.065 0.86 0 1 13 8.57 0.38 2.56 0.010 0.80 -12 0 6 -1.66 5.40 2.55 0.037 0.77 1 5 1 98.42 78.63 2.54 0.142 0.95 3 0 1 1.24 5.84 2.50 0.039 2.73 9 0 0 267.27 224.00 2.47 0.240 1.01 8 0 7 5.81 0.11 2.43 0.005 0.81 -3 1 13 1.02 7.04 2.40 0.043 0.83 -3 1 14 -3.12 9.94 2.39 0.051 0.77 -3 6 3 -1.16 7.76 2.37 0.045 0.77 8 1 5 32.66 22.22 2.35 0.076 0.89 -1 1 3 60.98 76.18 2.35 0.140 2.90 2 2 0 97.48 80.04 2.33 0.143 2.13 5 0 7 4.91 0.50 2.29 0.011 1.04 -8 2 5 2.87 7.79 2.26 0.045 1.02 -8 4 6 22.74 37.18 2.25 0.098 0.81 -8 2 7 1.06 4.97 2.23 0.036 0.96 -5 3 11 26.42 15.65 2.23 0.063 0.82 -5 2 12 60.46 44.84 2.22 0.107 0.83 -4 1 10 65.82 82.34 2.22 0.145 1.05 -9 3 8 18.15 3.76 2.20 0.031 0.80 5 1 10 34.48 23.14 2.17 0.077 0.81 -9 4 5 0.05 6.51 2.16 0.041 0.78 -2 2 11 119.30 97.91 2.16 0.159 0.92 -4 0 9 1.24 7.89 2.14 0.045 1.18 8 2 0 5.79 11.92 2.13 0.055 1.03 -7 3 4 50.19 64.28 2.13 0.129 1.01 -6 3 7 1.23 5.66 2.13 0.038 0.98 -10 3 2 -0.14 6.13 2.11 0.040 0.81 -4 0 10 25.94 38.85 2.10 0.100 1.07 2 2 11 5.20 13.39 2.10 0.059 0.84 -8 4 2 -1.41 2.93 2.09 0.027 0.84 6 2 5 -2.17 1.33 2.07 0.018 1.00 -5 1 13 29.11 17.62 2.06 0.067 0.82 4 2 10 6.55 0.07 2.04 0.004 0.82 8 2 4 12.78 6.23 2.03 0.040 0.89 4 1 9 2.79 7.67 1.99 0.044 0.93 -3 4 6 10.04 4.29 1.99 0.033 0.99 Bond lengths and angles C1 - Distance Angles N2 1.3151 (0.0045) N3 1.3559 (0.0052) 115.50 (0.34) H1 0.9500 122.25 122.25 C1 - N2 N3 C2 - Distance Angles N3 1.3294 (0.0047) N1 1.3310 (0.0044) 110.42 (0.35) H2 0.9500 124.79 124.79 C2 - N3 N1 C3 - Distance Angles N1 1.4778 (0.0041) C4 1.5059 (0.0049) 112.05 (0.31) H3A 0.9900 109.20 109.20 H3B 0.9900 109.20 109.20 107.90 C3 - N1 C4 H3A C4 - Distance Angles C9 1.3931 (0.0048) C5 1.3977 (0.0045) 118.85 (0.32) C3 1.5059 (0.0049) 119.91 (0.32) 121.22 (0.30) C4 - C9 C5 C5 - Distance Angles C4 1.3977 (0.0045) C6 1.4010 (0.0050) 119.00 (0.32) N4 1.4072 (0.0047) 122.32 (0.32) 118.54 (0.31) C5 - C4 C6 C6 - Distance Angles C7 1.3756 (0.0049) C5 1.4010 (0.0050) 120.99 (0.34) H6 0.9500 119.50 119.50 C6 - C7 C5 C7 - Distance Angles C6 1.3756 (0.0049) C8 1.3868 (0.0049) 120.36 (0.36) H7 0.9500 119.82 119.82 C7 - C6 C8 C8 - Distance Angles C9 1.3810 (0.0053) C7 1.3868 (0.0049) 118.90 (0.33) H8 0.9500 120.55 120.55 C8 - C9 C7 C9 - Distance Angles C8 1.3810 (0.0053) C4 1.3931 (0.0048) 121.89 (0.33) H9 0.9500 119.05 119.05 C9 - C8 C4 N1 - Distance Angles C2 1.3310 (0.0044) N2 1.3614 (0.0044) 109.93 (0.28) C3 1.4778 (0.0041) 129.52 (0.33) 120.49 (0.28) N1 - C2 N2 N2 - Distance Angles C1 1.3151 (0.0045) N1 1.3614 (0.0044) 102.01 (0.29) N2 - C1 N3 - Distance Angles C2 1.3294 (0.0047) C1 1.3559 (0.0052) 102.13 (0.30) N3 - C2 N4 - Distance Angles C5 1.4072 (0.0047) H1N 0.8903 (0.0194) 114.38 (3.13) H2N 0.8885 (0.0197) 116.05 (2.68) 107.71 (4.87) N4 - C5 H1N O1 - Distance Angles H1O 0.8528 (0.0190) H2O 0.8522 (0.0200) 110.97 (4.86) O1 - H1O Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.853(19) 2.00(2) 2.839(4) 169(6) O1-H1O...N3 0.85(2) 2.04(2) 2.864(4) 163(4) O1-H2O...N4_$2 0.890(19) 2.25(2) 3.127(4) 168(4) N4-H1N...O1_$1 0.89(2) 2.25(3) 3.046(5) 149(4) N4-H2N...O1_$2 FMAP and GRID set by program FMAP 2 2 14 GRID -4.545 -2 -2 4.545 2 2 R1 = 0.0755 for 1229 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.4397 0.1779 0.6497 [ 1.33 A from N1 ] Deepest hole -0.26 at 0.6021 0.1371 0.6726 [ 0.71 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1998 / 15897 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4397 0.1779 0.6497 1.00000 0.05 0.24 1.33 N1 1.71 H9 1.85 C2 1.87 N2 Q2 1 0.5691 0.2970 0.5558 1.00000 0.05 0.23 0.65 H3A 1.25 C3 1.91 N1 2.06 H9 Q3 1 0.4761 0.3571 0.8886 1.00000 0.05 0.22 0.80 N3 1.03 C2 1.54 H2 1.89 C1 Q4 1 0.7024 0.3667 0.6628 1.00000 0.05 0.22 0.77 C4 0.79 C3 1.48 H3A 1.54 H3B Q5 1 1.0800 0.6733 0.7785 1.00000 0.05 0.21 0.76 H6 0.83 C6 1.64 C7 1.99 H7 Shortest distances between peaks (including symmetry equivalents) 2 4 1.52 1 2 1.88 1 4 2.60 1 3 2.70 2 2 2.86 1 2 2.89 Time profile in seconds ----------------------- 0.10: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.01: 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. 0.62: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.46: Structure factors and derivatives 0.48: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.04: Apply other restraints 0.26: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0011 finished at 13:34:23 Total CPU time: 2.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++