+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 12:00:54 on 02-Mar-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC273 in Pna2(1) CELL 0.71073 13.3686 10.4704 8.7799 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0004 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O P CL UNIT 12 24 12 8 12 16 V = 1228.96 F(000) = 696.0 Mu = 1.34 mm-1 Cell Wt = 1403.27 Rho = 1.896 MERG 2 OMIT -3.00 55.00 OMIT 5 4 7 OMIT 2 2 5 EXTI 0.00182 FMAP 2 PLAN 10 SIZE 0.04 0.04 0.30 ACTA BOND $H CONF WGHT 0.00000 0.29790 L.S. 20 TEMP -153.00 FVAR 1.57552 C1 1 0.521531 0.144118 0.194380 11.00000 0.03226 0.04046 = 0.02494 -0.00249 0.00459 -0.01079 AFIX 23 H1A 2 0.556415 0.226255 0.211655 11.00000 -1.20000 H1B 2 0.506069 0.136952 0.084440 11.00000 -1.20000 AFIX 0 C2 1 0.587795 0.034787 0.242730 11.00000 0.02567 0.05499 = 0.02261 -0.00028 0.00037 -0.00037 AFIX 23 H2A 2 0.603971 0.043260 0.352300 11.00000 -1.20000 H2B 2 0.651240 0.037845 0.184688 11.00000 -1.20000 AFIX 0 C3 1 0.536439 -0.092129 0.214983 11.00000 0.02742 0.03977 = 0.03362 0.00002 0.00452 0.00972 AFIX 23 H3A 2 0.524786 -0.103669 0.104484 11.00000 -1.20000 H3B 2 0.579972 -0.162538 0.250626 11.00000 -1.20000 AFIX 0 AFIX 1 N1 3 0.313154 0.004381 0.110180 11.00000 0.02483 0.03772 = 0.02342 -0.00438 -0.00151 0.00051 AFIX 0 N2 3 0.128664 -0.036962 0.232592 11.00000 0.02449 0.04095 = 0.02815 -0.00175 -0.00099 0.00164 AFIX 1 N3 3 0.291146 0.015055 0.415743 11.00000 0.02463 0.04549 = 0.02314 0.00351 -0.00158 0.00047 AFIX 0 O1 4 0.428725 0.140565 0.283079 11.00000 0.02866 0.02778 = 0.03066 -0.00205 0.00194 -0.00266 O2 4 0.440359 -0.096556 0.296564 11.00000 0.02585 0.02967 = 0.03612 0.00546 0.00299 0.00452 P1 5 0.364122 0.015979 0.274274 11.00000 0.02321 0.02639 = 0.02277 0.00039 -0.00022 0.00019 P2 5 0.197938 -0.019941 0.086821 11.00000 0.02480 0.02740 = 0.02345 -0.00225 -0.00152 0.00029 P3 5 0.174508 -0.028029 0.397159 11.00000 0.02446 0.03088 = 0.02555 0.00125 0.00260 0.00009 CL1 6 0.170744 -0.165765 -0.053894 11.00000 0.04053 0.03548 = 0.03579 0.00805 -0.00056 0.00457 CL2 6 0.146639 0.126017 -0.036114 11.00000 0.03489 0.03495 = 0.04131 -0.01187 -0.00457 -0.00262 CL3 6 0.109117 0.114639 0.510417 11.00000 0.04057 0.04097 = 0.04694 0.01067 0.01059 -0.00564 CL4 6 0.127702 -0.178104 0.517992 11.00000 0.03781 0.03988 = 0.03284 -0.00734 0.00155 0.00496 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 02SRC273 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - O1 C2 C2 - C1 C3 C3 - O2 C2 N1 - P2 P1 N2 - P3 P2 N3 - P1 P3 O1 - C1 P1 O2 - C3 P1 P1 - O1 O2 N3 N1 P2 - N1 N2 Cl2 Cl1 P3 - N2 N3 Cl3 Cl4 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 8 -1 45.70 11.42 observed but should be systematically absent 5397 Reflections read, of which 252 rejected -17 =< h =< 14, -11 =< k =< 13, -9 =< l =< 11, Max. 2-theta = 54.94 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 9 2 229.31 20.92 2 125.37 1 3 3 30361.06 686.12 3 7734.15 2 2 4 2071.07 13.01 2 3465.10 3 3 5 2777.37 104.36 2 1091.03 3 4 5 4715.04 141.11 2 2074.84 4 4 6 1934.35 65.23 2 925.13 4 5 6 1509.04 27.56 3 468.99 5 5 7 292.30 9.65 2 420.70 2 0 9 1078.85 9.69 3 1986.01 2 1 9 77.25 4.75 5 25.74 10 Inconsistent equivalents 2403 Unique reflections, of which 0 suppressed R(int) = 0.0369 R(sigma) = 0.0483 Friedel opposites not merged Maximum memory for data reduction = 1524 / 24321 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 = 1853 / 154035 wR2 = 0.6264 before cycle 1 for 2403 data and 119 / 119 parameters GooF = S = 18.463; Restrained GooF = 18.458 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/esd from 15.51 to 15.00 N value esd shift/esd parameter 1 1.36649 0.02679 -7.803 OSF 2 0.00027 0.00945 -0.164 EXTI 25 0.10625 0.02173 3.059 U22 C3 47 -0.04004 0.01050 -3.561 U12 O1 49 -0.10936 0.00239 -5.360 y O2 58 0.00565 0.00092 -11.250 y P1 61 0.05794 0.00477 6.611 U22 P1 90 -0.00874 0.00502 -3.343 U23 Cl1 99 0.00490 0.00480 3.497 U23 Cl2 Mean shift/esd = 1.235 Maximum = -11.250 for y P1 Max. shift = 0.153 A for O2 Max. dU = 0.025 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.5020 before cycle 2 for 2403 data and 119 / 119 parameters GooF = S = 10.214; Restrained GooF = 10.212 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/esd from 19.82 to 15.00 N value esd shift/esd parameter 1 1.45834 0.02000 4.593 OSF 2 0.00000 0.00620 -0.389 EXTI 4 0.11772 0.00366 -4.503 y C1 13 0.01628 0.00358 -3.346 y C2 16 0.23605 0.03204 3.956 U22 C2 25 0.22360 0.02779 4.223 U22 C3 29 0.12785 0.01952 3.776 U12 C3 39 0.43425 0.00157 3.130 x O1 40 0.12116 0.00210 -6.228 y O1 43 0.11092 0.01175 4.570 U22 O1 47 -0.07059 0.00976 -3.131 U12 O1 49 -0.12091 0.00188 -6.136 y O2 58 -0.00709 0.00085 -15.000 y P1 61 0.07321 0.00455 3.355 U22 P1 Mean shift/esd = 1.113 Maximum = -15.000 for y P1 Max. shift = 0.181 A for C1 Max. dU = 0.052 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.3793 before cycle 3 for 2403 data and 119 / 119 parameters GooF = S = 7.151; Restrained GooF = 7.150 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.54862 0.01477 6.113 OSF 2 0.00000 0.00387 -0.035 EXTI 4 0.08744 0.00359 -8.440 y C1 5 0.21498 0.00381 3.020 z C1 13 -0.02314 0.00410 -9.611 y C2 16 0.48666 0.04807 5.213 U22 C2 21 0.52512 0.00217 -4.607 x C3 22 -0.13369 0.00393 -6.659 y C3 23 0.20392 0.00278 -3.044 z C3 25 0.35754 0.03969 3.375 U22 C3 31 -0.03731 0.00170 -3.594 y N2 39 0.44469 0.00129 8.085 x O1 40 0.09780 0.00194 -12.053 y O1 49 -0.13670 0.00166 -9.489 y O2 58 -0.01568 0.00062 -13.868 y P1 61 0.04824 0.00371 -6.731 U22 P1 67 -0.01984 0.00043 -4.461 y P2 76 -0.02804 0.00043 -3.395 y P3 Mean shift/esd = 1.797 Maximum = -13.868 for y P1 Max. shift = 0.417 A for C2 Max. dU = 0.079 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.2828 before cycle 4 for 2403 data and 119 / 119 parameters GooF = S = 5.284; Restrained GooF = 5.283 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.52501 0.01085 -2.175 OSF 2 0.00000 0.00265 -0.846 EXTI 4 0.09434 0.00216 3.190 y C1 6 0.02104 0.01315 -3.303 U11 C1 7 0.00001 0.01556 -8.196 U22 C1 9 0.02528 0.01127 6.265 U23 C1 10 -0.02696 0.00965 -5.583 U13 C1 11 0.01928 0.01205 7.070 U12 C1 12 0.58638 0.00167 -3.408 x C2 16 0.00001 0.07577 -9.571 U22 C2 21 0.51940 0.00187 -3.061 x C3 22 -0.15209 0.00386 -4.775 y C3 23 0.19310 0.00232 -4.657 z C3 24 0.01048 0.01594 -4.993 U11 C3 25 0.00270 0.04723 -7.513 U22 C3 27 -0.01777 0.02045 -6.532 U23 C3 28 -0.00866 0.01195 -5.652 U13 C3 29 -0.00945 0.02552 -7.488 U12 C3 43 0.04101 0.01006 -6.472 U22 O1 47 -0.00264 0.00611 8.081 U12 O1 52 0.03396 0.00705 -5.782 U22 O2 61 0.02498 0.00209 -11.120 U22 P1 65 0.00021 0.00145 -3.798 U12 P1 94 0.12631 0.00032 -3.198 y Cl2 Mean shift/esd = 1.815 Maximum = -11.120 for U22 P1 Max. shift = 0.228 A for C3 Max. dU =-0.161 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.2733 before cycle 5 for 2403 data and 119 / 119 parameters GooF = S = 5.337; Restrained GooF = 5.335 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48897 0.01033 -3.490 OSF 2 0.00000 0.00265 -1.830 EXTI 13 -0.02732 0.00077 -6.051 y C2 16 0.02120 0.00351 6.036 U22 C2 39 0.44080 0.00062 -3.105 x O1 Mean shift/esd = 0.876 Maximum = -6.051 for y C2 Max. shift = 0.050 A for C2 Max. dU = 0.008 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.2252 before cycle 6 for 2403 data and 119 / 119 parameters GooF = S = 4.211; Restrained GooF = 4.210 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.50484 0.00839 1.891 OSF 2 0.00000 0.00218 -2.511 EXTI 7 0.02256 0.00328 4.328 U22 C1 9 0.00536 0.00318 -4.206 U23 C1 10 -0.00363 0.00358 3.927 U13 C1 11 -0.00503 0.00342 -4.598 U12 C1 13 -0.03305 0.00077 -7.391 y C2 16 0.05772 0.00411 8.886 U22 C2 18 0.00754 0.00366 -3.172 U23 C2 22 -0.14665 0.00079 4.525 y C3 25 0.02955 0.00341 4.912 U22 C3 Mean shift/esd = 0.828 Maximum = 8.886 for U22 C2 Max. shift = 0.062 A for C2 Max. dU = 0.011 for C2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1954 before cycle 7 for 2403 data and 119 / 119 parameters GooF = S = 3.612; Restrained GooF = 3.612 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51111 0.00729 0.860 OSF 2 0.00000 0.00184 -2.808 EXTI Mean shift/esd = 0.430 Maximum = -2.808 for EXTI Max. shift = 0.021 A for C2 Max. dU = 0.003 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1927 before cycle 8 for 2403 data and 119 / 119 parameters GooF = S = 3.525; Restrained GooF = 3.525 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51301 0.00722 0.263 OSF 2 0.00000 0.00179 -2.798 EXTI Mean shift/esd = 0.105 Maximum = -2.798 for EXTI Max. shift = 0.004 A for H1A Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 9 for 2403 data and 119 / 119 parameters GooF = S = 3.525; Restrained GooF = 3.524 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51200 0.00722 -0.139 OSF 2 0.00000 0.00179 -2.791 EXTI Mean shift/esd = 0.040 Maximum = -2.791 for EXTI Max. shift = 0.001 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 10 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.521 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51170 0.00722 -0.042 OSF 2 0.00000 0.00179 -2.792 EXTI Mean shift/esd = 0.029 Maximum = -2.792 for EXTI Max. shift = 0.000 A for O1 Max. dU = 0.000 for N2 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 11 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 -0.002 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.027 Maximum = -2.793 for EXTI Max. shift = 0.000 A for H1A Max. dU = 0.000 for C2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 12 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 13 for 2403 data and 119 / 119 parameters GooF = S = 3.520; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for O1 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 14 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 15 for 2403 data and 119 / 119 parameters GooF = S = 3.520; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 16 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for O1 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 17 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for Cl2 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 18 for 2403 data and 119 / 119 parameters GooF = S = 3.520; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 19 for 2403 data and 119 / 119 parameters GooF = S = 3.520; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1853 / 154035 wR2 = 0.1925 before cycle 20 for 2403 data and 119 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51168 0.00722 0.000 OSF 2 0.00000 0.00179 -2.793 EXTI Mean shift/esd = 0.026 Maximum = -2.793 for EXTI Max. shift = 0.000 A for C2 Max. dU = 0.000 for Cl2 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5803 0.1619 0.2495 23 0.990 0.000 C1 O1 C2 H1B 0.5249 0.1020 0.1043 23 0.990 0.000 C1 O1 C2 H2A 0.6034 -0.0432 0.3534 23 0.990 0.000 C2 C1 C3 H2B 0.6515 -0.0382 0.1864 23 0.990 0.000 C2 C1 C3 H3A 0.5066 -0.1392 0.0846 23 0.990 0.000 C3 O2 C2 H3B 0.5560 -0.2277 0.2138 23 0.990 0.000 C3 O2 C2 02SRC273 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.53655 0.09136 0.21492 1.00000 0.02629 0.02842 0.02788 -0.00436 0.00102 -0.01157 0.02753 0.01395 0.00061 0.00079 0.00101 0.00000 0.00466 0.00406 0.00437 0.00337 0.00339 0.00355 0.00185 H1A 0.58033 0.16188 0.24955 1.00000 0.03304 0.00000 0.00000 H1B 0.52485 0.10204 0.10431 1.00000 0.03304 0.00000 0.00000 C2 0.58779 -0.03511 0.24365 1.00000 0.02405 0.06153 0.01915 0.00076 0.00622 -0.00363 0.03491 0.01614 0.00066 0.00085 0.00115 0.00000 0.00453 0.00597 0.00462 0.00425 0.00373 0.00421 0.00211 H2A 0.60344 -0.04323 0.35343 1.00000 0.04189 0.00000 0.00000 H2B 0.65153 -0.03816 0.18636 1.00000 0.04189 0.00000 0.00000 C3 0.52163 -0.14549 0.19474 1.00000 0.02598 0.03234 0.02658 -0.00345 0.00588 0.00923 0.02830 0.01550 0.00061 0.00083 0.00097 0.00000 0.00412 0.00419 0.00477 0.00344 0.00344 0.00360 0.00185 H3A 0.50664 -0.13923 0.08457 1.00000 0.03396 0.00000 0.00000 H3B 0.55600 -0.22771 0.21377 1.00000 0.03396 0.00000 0.00000 N1 0.31315 0.00438 0.11018 1.00000 0.02483 0.03772 0.02342 -0.00438 -0.00151 0.00051 0.02866 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 N2 0.12783 -0.03805 0.23421 1.00000 0.02266 0.04632 0.02659 0.00120 0.00408 0.00158 0.03185 0.01370 0.00054 0.00070 0.00099 0.00000 0.00380 0.00443 0.00413 0.00345 0.00299 0.00315 0.00172 N3 0.29115 0.01506 0.41574 1.00000 0.02463 0.04549 0.02314 0.00351 -0.00158 0.00047 0.03109 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 O1 0.44125 0.09742 0.29577 1.00000 0.02037 0.03318 0.03417 -0.00625 0.00108 -0.00751 0.02924 0.00941 0.00040 0.00055 0.00069 0.00000 0.00301 0.00307 0.00345 0.00259 0.00252 0.00227 0.00136 O2 0.42832 -0.13888 0.28382 1.00000 0.03216 0.02755 0.02362 0.00199 0.00143 -0.00409 0.02778 0.00958 0.00042 0.00050 0.00066 0.00000 0.00336 0.00281 0.00306 0.00247 0.00248 0.00238 0.00129 P1 0.36403 -0.01585 0.27449 1.00000 0.02096 0.02489 0.02186 -0.00260 -0.00012 0.00042 0.02257 0.00356 0.00015 0.00019 0.00027 0.00000 0.00108 0.00100 0.00118 0.00093 0.00084 0.00080 0.00050 P2 0.19797 -0.01961 0.08641 1.00000 0.02339 0.02871 0.02161 0.00381 -0.00153 0.00042 0.02457 0.00380 0.00016 0.00020 0.00027 0.00000 0.00107 0.00112 0.00112 0.00094 0.00092 0.00082 0.00052 P3 0.17402 -0.02795 0.39675 1.00000 0.02241 0.03400 0.02288 -0.00085 0.00258 0.00170 0.02643 0.00392 0.00016 0.00021 0.00026 0.00000 0.00110 0.00121 0.00117 0.00089 0.00090 0.00088 0.00054 Cl1 0.17073 -0.16548 -0.05404 1.00000 0.03735 0.03510 0.03333 -0.00649 -0.00081 -0.00416 0.03526 0.00362 0.00016 0.00020 0.00026 0.00000 0.00115 0.00111 0.00124 0.00101 0.00096 0.00093 0.00055 Cl2 0.14669 0.12634 -0.03650 1.00000 0.03182 0.03260 0.03967 0.01171 -0.00541 0.00372 0.03470 0.00393 0.00016 0.00020 0.00026 0.00000 0.00111 0.00108 0.00129 0.00102 0.00097 0.00085 0.00055 Cl3 0.10919 0.11535 0.50981 1.00000 0.03878 0.04346 0.04359 -0.00924 0.00901 0.00673 0.04194 0.00434 0.00017 0.00023 0.00030 0.00000 0.00127 0.00135 0.00141 0.00111 0.00108 0.00103 0.00063 Cl4 0.12776 -0.17795 0.51799 1.00000 0.03443 0.04180 0.03164 0.00906 0.00216 -0.00621 0.03596 0.00398 0.00016 0.00023 0.00026 0.00000 0.00117 0.00129 0.00118 0.00101 0.00093 0.00091 0.00058 Final Structure Factor Calculation for 02SRC273 in Pna2(1) Total number of l.s. parameters = 119 Maximum vector length = 511 Memory required = 1736 / 27090 wR2 = 0.1925 before cycle 21 for 2403 data and 2 / 119 parameters GooF = S = 3.521; Restrained GooF = 3.520 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0667 for 2284 Fo > 4sig(Fo) and 0.0702 for all 2403 data wR2 = 0.1925, GooF = S = 3.521, Restrained GooF = 3.520 for all data Flack x parameter = 0.0149 with esd 0.2404 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0402 0.0270 0.0153 C1 0.0619 0.0281 0.0148 C2 0.0390 0.0306 0.0153 C3 0.0390 0.0253 0.0216 N1 0.0465 0.0290 0.0201 N2 0.0460 0.0255 0.0217 N3 0.0417 0.0293 0.0167 O1 0.0346 0.0269 0.0218 O2 0.0264 0.0209 0.0203 P1 0.0304 0.0240 0.0193 P2 0.0343 0.0252 0.0198 P3 0.0424 0.0368 0.0266 Cl1 0.0487 0.0350 0.0205 Cl2 0.0531 0.0476 0.0251 Cl3 0.0485 0.0356 0.0238 Cl4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.029 0.043 0.055 0.071 0.084 0.100 0.123 0.153 0.208 1.000 Number in group 242. 253. 241. 239. 233. 239. 237. 247. 231. 241. GooF 2.117 2.513 3.827 3.218 3.375 3.770 3.790 4.416 4.329 3.361 K 1.225 0.984 1.012 0.964 1.003 1.011 1.034 1.056 1.065 1.049 Resolution(A) 0.77 0.81 0.85 0.89 0.94 1.00 1.08 1.19 1.36 1.71 inf Number in group 243. 245. 237. 236. 246. 238. 241. 237. 238. 242. GooF 1.584 1.901 2.060 2.203 2.554 3.181 3.742 4.289 5.038 5.952 K 0.978 1.007 1.008 1.035 1.037 1.036 1.048 1.053 1.052 1.053 R1 0.104 0.092 0.088 0.075 0.083 0.069 0.063 0.057 0.059 0.059 Recommended weighting scheme: WGHT 0.1142 7.0922 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) 1 4 0 241.09 785.72 10.48 0.133 2.57 4 3 0 219.61 670.90 8.75 0.123 2.41 2 3 -3 421.22 118.60 6.38 0.052 2.13 2 5 3 932.69 373.05 6.34 0.091 1.65 2 3 3 438.38 117.79 6.27 0.051 2.13 2 5 -3 959.64 374.33 5.65 0.092 1.65 3 6 0 651.50 1144.05 5.32 0.160 1.62 3 6 -3 406.54 700.26 5.17 0.125 1.42 3 4 0 3439.11 1837.52 4.61 0.203 2.26 6 5 0 70.55 225.37 4.27 0.071 1.53 3 6 3 397.11 700.79 4.17 0.125 1.42 1 2 0 1916.66 943.00 4.17 0.145 4.87 7 4 -3 247.33 101.20 4.13 0.048 1.36 6 7 0 453.02 153.98 4.06 0.059 1.24 0 7 -3 915.83 1528.74 3.97 0.185 1.33 7 4 1 63.24 180.19 3.92 0.064 1.52 2 7 3 838.16 492.06 3.90 0.105 1.31 7 6 -3 200.11 376.54 3.89 0.092 1.18 3 8 3 101.48 241.16 3.85 0.074 1.15 6 5 2 96.04 14.70 3.79 0.018 1.44 1 6 0 13260.06 9432.18 3.78 0.460 1.73 2 5 -1 2143.21 1360.36 3.78 0.175 1.95 0 7 3 971.44 1545.71 3.71 0.186 1.33 9 6 0 514.47 890.94 3.68 0.141 1.13 0 5 3 2877.52 1588.95 3.65 0.189 1.70 2 3 -1 1704.12 1036.66 3.65 0.153 2.92 7 6 -1 156.18 296.55 3.65 0.082 1.27 7 6 3 201.73 369.75 3.53 0.091 1.18 1 6 -4 266.79 420.01 3.51 0.097 1.36 2 7 -3 834.29 480.18 3.49 0.104 1.31 2 5 1 2071.24 1348.84 3.48 0.174 1.95 7 4 -1 75.36 181.81 3.44 0.064 1.52 3 4 -1 116.52 214.88 3.39 0.069 2.19 6 5 -2 85.14 17.14 3.37 0.020 1.44 3 4 1 116.10 221.05 3.36 0.070 2.19 7 8 -3 151.42 301.69 3.31 0.082 1.01 3 8 -3 117.79 240.52 3.26 0.073 1.15 2 5 0 1437.46 1951.13 3.23 0.209 2.00 4 9 2 28.50 106.89 3.21 0.049 1.07 3 8 4 1201.91 761.75 3.20 0.131 1.09 1 6 6 201.62 48.11 3.18 0.033 1.12 8 5 0 351.64 552.99 3.17 0.111 1.31 4 9 -2 33.67 108.14 3.15 0.049 1.07 1 6 2 2947.16 2164.51 3.15 0.220 1.61 2 5 -5 234.41 131.68 3.13 0.054 1.32 4 7 -3 2349.62 1637.28 3.12 0.192 1.24 1 8 -2 838.08 508.04 3.12 0.107 1.25 1 6 4 255.22 425.13 3.08 0.098 1.36 0 5 -1 2587.71 1576.74 3.06 0.188 2.04 3 2 0 1783.34 1154.80 3.05 0.161 3.39 Bond lengths and angles C1 - Distance Angles O1 1.4599 (0.0096) C2 1.5120 (0.0124) 110.63 (0.68) H1A 0.9900 109.52 109.52 H1B 0.9900 109.52 109.52 108.08 C1 - O1 C2 H1A C2 - Distance Angles C1 1.5120 (0.0124) C3 1.5173 (0.0119) 110.84 (0.75) H2A 0.9900 109.47 109.47 H2B 0.9900 109.47 109.47 108.06 C2 - C1 C3 H2A C3 - Distance Angles O2 1.4739 (0.0094) C2 1.5173 (0.0119) 107.90 (0.67) H3A 0.9900 110.12 110.12 H3B 0.9900 110.12 110.12 108.44 C3 - O2 C2 H3A N1 - Distance Angles P2 1.5741 (0.0021) P1 1.6089 (0.0023) 120.76 (0.11) N1 - P2 N2 - Distance Angles P3 1.5586 (0.0089) P2 1.6126 (0.0083) 119.89 (0.47) N2 - P3 N3 - Distance Angles P1 1.6100 (0.0023) P3 1.6378 (0.0022) 116.42 (0.11) N3 - P1 O1 - Distance Angles C1 1.4599 (0.0096) P1 1.5833 (0.0058) 118.63 (0.49) O1 - C1 O2 - Distance Angles C3 1.4739 (0.0094) P1 1.5508 (0.0059) 118.69 (0.51) O2 - C3 P1 - Distance Angles O1 1.5833 (0.0058) O2 1.5508 (0.0059) 104.75 (0.33) N3 1.6100 (0.0023) 98.81 (0.24) 117.49 (0.25) N1 1.6089 (0.0023) 106.43 (0.25) 113.01 (0.25) 114.10 (0.12) P1 - O1 O2 N3 P2 - Distance Angles N1 1.5741 (0.0021) N2 1.6126 (0.0083) 118.77 (0.31) Cl2 1.9924 (0.0029) 106.62 (0.12) 109.12 (0.29) Cl1 1.9964 (0.0031) 112.48 (0.13) 107.42 (0.30) 100.92 (0.14) P2 - N1 N2 Cl2 P3 - Distance Angles N2 1.5586 (0.0089) N3 1.6378 (0.0022) 119.38 (0.31) Cl3 1.9968 (0.0032) 109.53 (0.31) 99.08 (0.13) Cl4 1.9956 (0.0031) 108.20 (0.30) 117.28 (0.14) 101.05 (0.14) P3 - N2 N3 Cl3 Cl1 - Distance Angles P2 1.9964 (0.0031) Cl1 - Cl2 - Distance Angles P2 1.9924 (0.0029) Cl2 - Cl3 - Distance Angles P3 1.9968 (0.0032) Cl3 - Cl4 - Distance Angles P3 1.9956 (0.0031) Cl4 - Selected torsion angles 58.01 ( 0.97) O1 - C1 - C2 - C3 -59.95 ( 0.92) C1 - C2 - C3 - O2 -51.65 ( 0.88) C2 - C1 - O1 - P1 58.00 ( 0.81) C2 - C3 - O2 - P1 43.46 ( 0.68) C1 - O1 - P1 - O2 165.06 ( 0.55) C1 - O1 - P1 - N3 -76.48 ( 0.59) C1 - O1 - P1 - N1 -47.21 ( 0.68) C3 - O2 - P1 - O1 -155.61 ( 0.50) C3 - O2 - P1 - N3 68.23 ( 0.60) C3 - O2 - P1 - N1 150.87 ( 0.24) P3 - N3 - P1 - O1 -97.34 ( 0.28) P3 - N3 - P1 - O2 38.36 ( 0.16) P3 - N3 - P1 - N1 -139.67 ( 0.25) P2 - N1 - P1 - O1 105.89 ( 0.27) P2 - N1 - P1 - O2 -31.80 ( 0.17) P2 - N1 - P1 - N3 11.72 ( 0.34) P1 - N1 - P2 - N2 135.35 ( 0.13) P1 - N1 - P2 - Cl2 -114.93 ( 0.15) P1 - N1 - P2 - Cl1 1.79 ( 0.63) P3 - N2 - P2 - N1 -120.60 ( 0.45) P3 - N2 - P2 - Cl2 130.80 ( 0.44) P3 - N2 - P2 - Cl1 5.91 ( 0.64) P2 - N2 - P3 - N3 118.98 ( 0.44) P2 - N2 - P3 - Cl3 -131.71 ( 0.42) P2 - N2 - P3 - Cl4 -26.64 ( 0.37) P1 - N3 - P3 - N2 -145.22 ( 0.12) P1 - N3 - P3 - Cl3 107.27 ( 0.16) P1 - N3 - P3 - Cl4 FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.0702 for 1494 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 3.59 at 0.7109 0.0354 0.9133 [ 0.53 A from N3 ] Deepest hole -3.14 at 0.2919 0.0369 0.4160 [ 0.23 A from N3 ] Mean = 0.00, Rms deviation from mean = 0.18 e/A^3, Highest memory used = 1955 / 17820 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2891 -0.0354 0.4133 1.00000 0.05 3.59 0.53 N3 1.55 P3 1.59 P1 2.44 O2 Q2 1 0.3136 -0.0308 0.0842 1.00000 0.05 1.98 0.43 N1 1.55 P2 1.81 P1 2.44 H2A Q3 1 0.2874 -0.1037 0.5198 1.00000 0.05 0.54 1.54 N3 2.02 P3 2.24 H2B 2.27 CL4 Q4 1 0.4203 0.0841 0.2894 1.00000 0.05 0.50 0.32 O1 1.30 P1 1.69 C1 2.15 H1B Q5 1 0.2975 -0.1689 -0.0671 1.00000 0.05 0.50 1.70 CL1 2.29 H1A 2.40 N1 2.46 P2 Q6 1 0.2494 -0.0265 0.2627 1.00000 0.05 0.47 1.52 N3 1.54 P1 1.55 P3 1.62 N1 Q7 1 0.7104 0.0401 0.1133 1.00000 0.05 0.45 1.30 H2B 1.83 N3 2.15 C2 2.45 P3 Q8 1 0.2100 0.1724 0.0985 1.00000 0.05 0.45 1.53 CL2 2.02 P2 2.24 N1 2.74 N2 Q9 1 0.2741 -0.0998 0.1820 1.00000 0.05 0.44 1.36 N1 1.56 P2 1.70 P1 2.11 N2 Q10 1 0.2636 0.1085 -0.0616 1.00000 0.05 0.44 1.59 CL2 1.98 N1 2.05 H2A 2.06 P2 Shortest distances between peaks (including symmetry equivalents) 3 7 1.06 6 9 1.09 1 3 1.18 2 9 1.24 1 6 1.43 8 10 1.71 1 7 1.76 2 6 1.79 2 5 1.97 2 10 2.05 1 9 2.15 5 9 2.32 1 4 2.41 3 8 2.44 3 6 2.45 2 8 2.54 4 6 2.57 6 8 2.59 2 4 2.59 4 9 2.90 1 2 2.91 5 10 2.94 3 9 2.97 Time profile in seconds ----------------------- 0.16: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 1.56: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.23: Structure factors and derivatives 1.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.14: Apply other restraints 1.11: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:01:06 Total CPU time: 7.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++