+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0178 started at 13:44:30 on 08-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0178 in P2(1)/n CELL 0.71073 7.1493 18.6099 8.8649 90.000 113.221 90.000 ZERR 2.00 0.0001 0.0006 0.0002 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 32 52 4 6 4 4 V = 1083.91 F(000) = 444.0 Mu = 0.43 mm-1 Cell Wt = 842.94 Rho = 1.291 MERG 2 OMIT -3.00 55.00 EXTI 0.13649 SHEL 7 0.77 EQIV $1 -X+1, -Y, -Z+1 FREE O2 O2_$1 EQIV $2 X+0.5, -Y+0.5, Z+0.5 HTAB O1 CL1_$2 FMAP 2 PLAN 10 SIZE 0.06 0.12 0.18 ACTA HTAB 2.00000 BOND $H WGHT 0.06680 0.19550 L.S. 20 TEMP -153.00 FVAR 1.18289 C1 1 0.398721 0.158622 0.670136 11.00000 0.02129 0.01734 = 0.01849 0.00007 0.00529 -0.00004 C2 1 0.328723 0.171916 0.794413 11.00000 0.02766 0.02045 = 0.01727 -0.00030 0.00785 -0.00135 AFIX 43 H2 2 0.421983 0.174007 0.905844 11.00000 -1.20000 AFIX 0 C3 1 0.124665 0.181897 0.754204 11.00000 0.03031 0.02404 = 0.02671 -0.00023 0.01588 -0.00180 AFIX 43 H3 2 0.075623 0.190720 0.837706 11.00000 -1.20000 AFIX 0 C4 1 -0.011297 0.179012 0.589149 11.00000 0.01942 0.02851 = 0.03170 -0.00007 0.01018 -0.00047 AFIX 43 H4 2 -0.152672 0.186743 0.559756 11.00000 -1.20000 AFIX 0 C5 1 0.061358 0.165027 0.471558 11.00000 0.01943 0.02116 = 0.02211 0.00176 0.00364 -0.00072 AFIX 43 H5 2 -0.030371 0.162781 0.359686 11.00000 -1.20000 AFIX 0 C6 1 0.336917 0.138829 0.380144 11.00000 0.02082 0.02452 = 0.01356 0.00139 0.00470 -0.00014 AFIX 23 H6A 2 0.474979 0.159316 0.411715 11.00000 -1.20000 H6B 2 0.246031 0.163303 0.278479 11.00000 -1.20000 AFIX 0 C7 1 0.087844 0.001714 0.274035 11.00000 0.03516 0.02117 = 0.06008 0.00267 0.01673 -0.00057 AFIX 137 H7A 2 0.084920 -0.047262 0.232543 11.00000 -1.50000 H7B 2 -0.009298 0.031722 0.187746 11.00000 -1.50000 H7C 2 0.050660 0.000749 0.369251 11.00000 -1.50000 AFIX 0 C8 1 0.437937 0.034333 0.167592 11.00000 0.06717 0.03886 = 0.04149 -0.01033 0.03608 -0.00511 AFIX 137 H8A 2 0.576235 0.053874 0.205884 11.00000 -1.50000 H8B 2 0.347592 0.062416 0.073581 11.00000 -1.50000 H8C 2 0.438725 -0.015870 0.134470 11.00000 -1.50000 AFIX 0 N1 3 0.264525 0.154169 0.512225 11.00000 0.01950 0.01780 = 0.01693 -0.00002 0.00583 -0.00005 O1 4 0.590819 0.149344 0.694338 11.00000 0.01830 0.03675 = 0.01640 -0.00365 0.00220 0.00325 AFIX 147 H1 2 0.664066 0.154364 0.794574 11.00000 -1.50000 AFIX 0 O2 4 0.526006 0.004714 0.494661 10.50000 0.02668 0.02474 = 0.02132 0.00179 0.00316 0.00673 SI1 5 0.345937 0.039200 0.335274 11.00000 0.02472 0.02258 = 0.01490 0.00032 0.00485 0.00521 CL1 6 0.360449 0.329213 0.531325 11.00000 0.02519 0.02863 = 0.01638 0.00148 0.00188 -0.00447 HKLF 4 Covalent radii and connectivity table for 2007src0178 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C1 - O1 N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 N1 C6 - N1 Si1 C7 - Si1 C8 - Si1 N1 - C1 C5 C6 O1 - C1 O2 - Si1 Si1_$1 Si1 - O2 O2_$1 C7 C8 C6 Cl1 - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 x+1/2, -y+1/2, z+1/2 16491 Reflections read, of which 267 rejected -9 =< h =< 9, -24 =< k =< 24, -11 =< l =< 11, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2475 Unique reflections, of which 0 suppressed R(int) = 0.0511 R(sigma) = 0.0384 Friedel opposites merged Maximum memory for data reduction = 1557 / 24865 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 = 1913 / 157470 wR2 = 0.1267 before cycle 1 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01031 0.000 EXTI Mean shift/esd = 0.003 Maximum = -0.016 for U23 Si1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for Cl1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 2 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18290 0.00460 0.001 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.006 for U13 Cl1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for Cl1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 3 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18290 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y Cl1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 4 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for Cl1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 5 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 6 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 7 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for O2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 8 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 9 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 10 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 11 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for O2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 12 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 13 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13648 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 14 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 15 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 16 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for O2 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 17 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 18 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 19 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1913 / 157470 wR2 = 0.1266 before cycle 20 for 2475 data and 122 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18289 0.00460 0.000 OSF 2 0.13649 0.01030 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Largest correlation matrix elements -0.948 U11 O2 / x O2 -0.721 U13 O2 / U33 O2 0.616 U13 C8 / U33 C8 -0.930 U22 O2 / y O2 0.711 z O2 / x O2 0.610 U33 Cl1 / OSF -0.920 U13 O2 / z O2 -0.704 U23 O2 / x O2 0.607 U33 O2 / x O2 -0.848 U12 O2 / y O2 -0.671 U23 O2 / U33 O2 0.606 U11 Cl1 / OSF 0.837 U33 O2 / z O2 0.667 EXTI / OSF 0.591 U33 Si1 / OSF 0.831 U12 O2 / U22 O2 -0.644 U11 O2 / z O2 0.586 U22 Cl1 / OSF -0.792 U23 O2 / z O2 0.643 U13 C8 / U11 C8 0.583 U33 Cl1 / U33 Si1 0.745 U13 O2 / U23 O2 0.637 U23 O2 / U11 O2 -0.581 U33 O2 / U11 O2 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4220 0.1740 0.9058 43 0.950 0.000 C2 C3 C1 H3 0.0756 0.1907 0.8377 43 0.950 0.000 C3 C2 C4 H4 -0.1527 0.1867 0.5598 43 0.950 0.000 C4 C5 C3 H5 -0.0304 0.1628 0.3597 43 0.950 0.000 C5 C4 N1 H6A 0.4750 0.1593 0.4117 23 0.990 0.000 C6 N1 Si1 H6B 0.2460 0.1633 0.2785 23 0.990 0.000 C6 N1 Si1 H7A 0.0849 -0.0473 0.2325 137 0.980 0.000 C7 Si1 H7A H7B -0.0093 0.0317 0.1877 137 0.980 0.000 C7 Si1 H7A H7C 0.0507 0.0007 0.3693 137 0.980 0.000 C7 Si1 H7A H8A 0.5762 0.0539 0.2059 137 0.980 0.000 C8 Si1 H8A H8B 0.3476 0.0624 0.0736 137 0.980 0.000 C8 Si1 H8A H8C 0.4387 -0.0159 0.1345 137 0.980 0.000 C8 Si1 H8A H1 0.6641 0.1544 0.7946 147 0.840 0.000 O1 C1 H1 2007src0178 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.39872 0.15862 0.67014 1.00000 0.02129 0.01734 0.01849 0.00007 0.00529 -0.00004 0.01984 0.00338 0.00025 0.00009 0.00020 0.00000 0.00081 0.00077 0.00079 0.00058 0.00065 0.00058 0.00036 C2 0.32872 0.17192 0.79441 1.00000 0.02766 0.02045 0.01727 -0.00030 0.00785 -0.00135 0.02211 0.00358 0.00027 0.00009 0.00021 0.00000 0.00091 0.00087 0.00081 0.00058 0.00070 0.00060 0.00038 H2 0.42198 0.17401 0.90584 1.00000 0.02653 0.00000 0.00000 C3 0.12467 0.18190 0.75420 1.00000 0.03031 0.02404 0.02671 -0.00023 0.01588 -0.00180 0.02557 0.00378 0.00028 0.00009 0.00023 0.00000 0.00095 0.00086 0.00092 0.00067 0.00078 0.00068 0.00040 H3 0.07562 0.19072 0.83771 1.00000 0.03069 0.00000 0.00000 C4 -0.01130 0.17901 0.58915 1.00000 0.01942 0.02851 0.03170 -0.00007 0.01018 -0.00047 0.02651 0.00374 0.00027 0.00010 0.00023 0.00000 0.00084 0.00096 0.00101 0.00070 0.00076 0.00065 0.00041 H4 -0.15267 0.18674 0.55976 1.00000 0.03181 0.00000 0.00000 C5 0.06136 0.16503 0.47156 1.00000 0.01943 0.02116 0.02211 0.00176 0.00364 -0.00072 0.02231 0.00352 0.00026 0.00009 0.00022 0.00000 0.00083 0.00083 0.00085 0.00062 0.00068 0.00060 0.00038 H5 -0.03037 0.16278 0.35969 1.00000 0.02678 0.00000 0.00000 C6 0.33692 0.13883 0.38014 1.00000 0.02082 0.02452 0.01356 0.00139 0.00470 -0.00014 0.02028 0.00330 0.00025 0.00009 0.00019 0.00000 0.00079 0.00085 0.00072 0.00059 0.00062 0.00061 0.00036 H6A 0.47498 0.15932 0.41171 1.00000 0.02433 0.00000 0.00000 H6B 0.24603 0.16330 0.27848 1.00000 0.02433 0.00000 0.00000 C7 0.08784 0.00171 0.27404 1.00000 0.03516 0.02117 0.06008 0.00267 0.01673 -0.00057 0.03944 0.00450 0.00032 0.00011 0.00029 0.00000 0.00104 0.00096 0.00141 0.00089 0.00100 0.00076 0.00051 H7A 0.08492 -0.04726 0.23254 1.00000 0.05916 0.00000 0.00000 H7B -0.00930 0.03172 0.18775 1.00000 0.05916 0.00000 0.00000 H7C 0.05066 0.00075 0.36925 1.00000 0.05916 0.00000 0.00000 C8 0.43794 0.03433 0.16759 1.00000 0.06717 0.03886 0.04149 -0.01033 0.03608 -0.00511 0.04461 0.00528 0.00042 0.00013 0.00030 0.00000 0.00157 0.00124 0.00124 0.00091 0.00119 0.00103 0.00057 H8A 0.57623 0.05387 0.20588 1.00000 0.06692 0.00000 0.00000 H8B 0.34759 0.06242 0.07358 1.00000 0.06692 0.00000 0.00000 H8C 0.43872 -0.01587 0.13447 1.00000 0.06692 0.00000 0.00000 N1 0.26452 0.15417 0.51223 1.00000 0.01950 0.01780 0.01693 -0.00002 0.00583 -0.00005 0.01850 0.00276 0.00021 0.00007 0.00016 0.00000 0.00068 0.00067 0.00066 0.00051 0.00055 0.00051 0.00031 O1 0.59082 0.14934 0.69434 1.00000 0.01830 0.03675 0.01640 -0.00365 0.00220 0.00325 0.02526 0.00246 0.00018 0.00007 0.00014 0.00000 0.00060 0.00074 0.00059 0.00050 0.00047 0.00049 0.00031 H1 0.66407 0.15436 0.79457 1.00000 0.03789 0.00000 0.00000 O2 0.52601 0.00471 0.49466 0.50000 0.02668 0.02474 0.02132 0.00179 0.00316 0.00673 0.02621 0.02555 0.00149 0.00071 0.00166 0.00000 0.00461 0.00312 0.00175 0.00180 0.00275 0.00293 0.00142 Si1 0.34594 0.03920 0.33527 1.00000 0.02472 0.02258 0.01490 0.00032 0.00485 0.00521 0.02165 0.00095 0.00007 0.00003 0.00005 0.00000 0.00031 0.00030 0.00028 0.00016 0.00021 0.00017 0.00020 Cl1 0.36045 0.32921 0.53133 1.00000 0.02519 0.02863 0.01638 0.00148 0.00188 -0.00447 0.02537 0.00079 0.00006 0.00002 0.00005 0.00000 0.00029 0.00029 0.00027 0.00014 0.00019 0.00015 0.00020 Final Structure Factor Calculation for 2007src0178 in P2(1)/n Total number of l.s. parameters = 122 Maximum vector length = 511 Memory required = 1791 / 25039 wR2 = 0.1266 before cycle 21 for 2475 data and 0 / 122 parameters GooF = S = 1.279; Restrained GooF = 1.279 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0668 * P )^2 + 0.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0435 for 2253 Fo > 4sig(Fo) and 0.0499 for all 2475 data wR2 = 0.1266, GooF = S = 1.279, Restrained GooF = 1.279 for all data Occupancy sum of asymmetric unit = 12.50 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0245 0.0177 0.0173 C1 0.0289 0.0202 0.0172 C2 0.0324 0.0242 0.0201 C3 0.0322 0.0285 0.0188 C4 0.0291 0.0205 0.0173 C5 0.0250 0.0225 0.0133 C6 0.0626 0.0349 0.0209 C7 0.0714 0.0408 0.0217 C8 0.0210 0.0178 0.0167 N1 0.0395 0.0224 0.0139 O1 0.0374 0.0249 0.0164 O2 0.0311 0.0192 0.0147 Si1 0.0367 0.0246 0.0148 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.036 0.054 0.074 0.095 0.119 0.150 0.194 0.273 1.000 Number in group 249. 246. 261. 238. 249. 242. 246. 248. 247. 249. GooF 1.261 1.217 1.322 1.227 1.112 0.933 0.901 0.817 0.803 2.398 K 1.502 1.034 1.001 0.989 0.984 0.989 0.992 1.015 1.011 1.054 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 255. 245. 249. 245. 246. 246. 247. 246. 250. 246. GooF 0.945 0.996 0.875 0.959 0.894 0.851 1.015 1.003 1.306 2.750 K 1.024 1.032 1.026 1.007 1.016 1.020 1.044 1.027 1.058 1.030 R1 0.069 0.064 0.049 0.043 0.036 0.029 0.035 0.030 0.040 0.084 Recommended weighting scheme: WGHT 0.0668 0.1955 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 0 1 -0.66 5144.17 17.89 0.692 6.52 -1 2 1 931.86 5488.92 12.57 0.715 5.34 0 2 1 276.88 845.54 7.88 0.280 6.13 1 1 0 508.56 1204.17 6.07 0.335 6.20 -1 0 3 8.92 28.96 5.51 0.052 2.95 1 2 3 63.75 31.55 5.44 0.054 2.16 3 3 0 54.24 97.18 4.81 0.095 2.07 3 0 1 3479.64 7239.48 4.18 0.821 1.93 -1 3 4 50.94 80.95 3.83 0.087 2.08 1 3 2 10481.46 7396.85 3.74 0.829 2.68 0 3 1 10.76 21.50 3.67 0.045 4.94 2 7 2 28.22 16.26 3.66 0.039 1.68 -4 6 2 8.90 2.35 3.57 0.015 1.55 -2 7 1 18.56 31.34 3.28 0.054 2.13 1 2 4 233.15 169.20 3.28 0.125 1.73 -4 0 2 6.07 15.79 3.20 0.038 1.79 -1 3 7 7.37 1.28 3.18 0.011 1.21 1 9 2 7914.15 6082.14 3.14 0.752 1.70 1 8 4 1.14 5.79 3.07 0.023 1.40 -1 6 3 8.42 3.16 2.93 0.017 2.14 -6 12 5 22.06 10.17 2.89 0.031 0.92 3 10 0 69.12 95.24 2.81 0.094 1.42 2 7 0 5901.73 4654.53 2.81 0.658 2.07 0 4 1 5508.72 10751.70 2.73 1.000 4.04 0 7 2 17.53 10.57 2.73 0.031 2.23 -6 4 5 3.84 0.07 2.73 0.003 1.11 0 10 0 5997.73 4764.56 2.70 0.666 1.86 1 7 1 5130.69 4099.74 2.66 0.618 2.27 1 1 2 6281.21 4867.06 2.63 0.673 2.94 0 5 3 57.25 77.92 2.60 0.085 2.19 -2 10 2 53.46 72.84 2.60 0.082 1.62 -3 4 6 84.69 63.16 2.59 0.077 1.37 1 2 1 4175.09 3310.04 2.58 0.555 3.94 -4 2 1 325.01 257.54 2.49 0.155 1.72 -6 6 5 9.75 3.25 2.47 0.017 1.07 -3 5 3 9.04 16.17 2.46 0.039 1.88 2 5 6 34.87 24.20 2.46 0.047 1.06 0 13 7 8.97 3.55 2.43 0.018 0.90 1 0 1 13.24 6.00 2.42 0.024 4.35 -1 6 2 4444.01 3611.68 2.40 0.580 2.52 1 1 1 4182.42 3324.65 2.36 0.556 4.23 0 10 1 2533.84 2078.64 2.35 0.440 1.81 -4 5 5 16.68 10.43 2.35 0.031 1.38 -6 5 4 2.46 0.04 2.34 0.002 1.12 -3 16 7 2.03 10.38 2.30 0.031 0.85 -1 23 1 61.76 92.77 2.29 0.093 0.80 -7 5 1 3.09 9.37 2.29 0.030 0.95 2 2 7 112.44 144.83 2.22 0.116 0.98 -2 1 2 5925.85 4816.05 2.21 0.669 3.21 -3 0 5 345.26 439.22 2.20 0.202 1.66 Bond lengths and angles C1 - Distance Angles O1 1.3152 (0.0020) N1 1.3520 (0.0022) 115.46 (0.15) C2 1.4001 (0.0024) 124.69 (0.15) 119.85 (0.15) C1 - O1 N1 C2 - Distance Angles C3 1.3711 (0.0026) C1 1.4001 (0.0024) 119.55 (0.16) H2 0.9500 120.22 120.22 C2 - C3 C1 C3 - Distance Angles C2 1.3711 (0.0026) C4 1.4026 (0.0027) 119.65 (0.17) H3 0.9500 120.17 120.17 C3 - C2 C4 C4 - Distance Angles C5 1.3606 (0.0026) C3 1.4026 (0.0027) 119.32 (0.16) H4 0.9500 120.34 120.34 C4 - C5 C3 C5 - Distance Angles C4 1.3606 (0.0025) N1 1.3666 (0.0022) 120.88 (0.16) H5 0.9500 119.56 119.56 C5 - C4 N1 C6 - Distance Angles N1 1.4826 (0.0021) Si1 1.9027 (0.0018) 113.82 (0.11) H6A 0.9900 108.79 108.79 H6B 0.9900 108.79 108.79 107.67 C6 - N1 Si1 H6A C7 - Distance Angles Si1 1.8429 (0.0021) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - Si1 H7A H7B C8 - Distance Angles Si1 1.8497 (0.0022) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - Si1 H8A H8B N1 - Distance Angles C1 1.3520 (0.0022) C5 1.3666 (0.0022) 120.70 (0.15) C6 1.4826 (0.0021) 120.22 (0.14) 119.06 (0.13) N1 - C1 C5 O1 - Distance Angles C1 1.3152 (0.0020) H1 0.8400 109.47 O1 - C1 O2 - Distance Angles Si1 1.6221 (0.0137) Si1_$1 1.6403 (0.0136) 164.03 (0.40) O2 - Si1 Si1 - Distance Angles O2 1.6221 (0.0137) O2_$1 1.6403 (0.0136) 15.97 (0.40) C7 1.8429 (0.0021) 117.74 (0.26) 102.32 (0.25) C8 1.8497 (0.0022) 105.61 (0.35) 117.89 (0.37) 112.13 (0.11) C6 1.9027 (0.0018) 106.51 (0.48) 110.24 (0.48) 108.54 (0.09) 105.53 (0.09) Si1 - O2 O2_$1 C7 C8 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.04 2.8738(12) 174.9 O1-H1...Cl1_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)