+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0116p started at 17:34:41 on 07-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0116 in P2(1)/c CELL 0.71073 9.3511 14.5157 10.4670 90.000 90.778 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N O UNIT 28 56 20 4 40 V = 1420.64 F(000) = 672.0 Mu = 0.13 mm-1 Cell Wt = 1304.97 Rho = 1.525 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 ACTA EQIV $1 -x, -y, -z+2 EQIV $2 x, -y+1/2, z-1/2 EQIV $3 x, -y+1/2, z+1/2 EQIV $4 x+1, y, z EQIV $5 x+1, -y+1/2, z-1/2 EQIV $6 x, y, z-1 EQIV $7 -x+1, -y, -z+1 htab O7 O1_$1 htab O8 O4_$2 htab O9 O3_$3 htab O10 O7_$4 htab N1 O8_$5 htab N1 O5_$6 htab N1 O9_$6 htab N1 O6_$7 SIZE 0.16 0.16 0.14 HTAB 2.00000 BOND $H WGHT 0.02650 0.94850 L.S. 9 TEMP -153.00 FVAR 0.73128 MOLE 1 B1 3 0.208089 0.136688 0.899754 11.00000 0.00992 0.01510 = 0.01471 0.00095 -0.00066 -0.00009 B2 3 -0.053217 0.116198 0.905799 11.00000 0.01289 0.01578 = 0.01269 -0.00208 0.00025 0.00061 B3 3 0.041519 0.232411 0.772393 11.00000 0.01399 0.01494 = 0.01330 -0.00180 -0.00023 -0.00040 B4 3 0.382912 0.196887 1.058824 11.00000 0.01450 0.01640 = 0.01631 0.00174 -0.00027 0.00013 B5 3 0.461394 0.089417 0.900768 11.00000 0.01284 0.01477 = 0.01510 0.00203 0.00019 -0.00052 O1 5 0.080383 0.080571 0.924094 11.00000 0.00975 0.01624 = 0.01820 0.00350 -0.00022 0.00011 O2 5 -0.073524 0.197272 0.839496 11.00000 0.01190 0.01651 = 0.01789 0.00262 0.00127 0.00217 O3 5 0.177025 0.203557 0.796816 11.00000 0.01153 0.01742 = 0.01533 0.00393 -0.00018 -0.00048 O4 5 0.244789 0.185492 1.019116 11.00000 0.01154 0.01859 = 0.01466 -0.00187 0.00008 0.00169 O5 5 0.494510 0.156178 0.992197 11.00000 0.01035 0.01872 = 0.01860 -0.00230 -0.00027 0.00020 O6 5 0.323215 0.075533 0.861728 11.00000 0.01077 0.01593 = 0.01622 -0.00089 -0.00028 0.00012 O7 5 -0.169421 0.071261 0.951687 11.00000 0.01079 0.01803 = 0.02044 0.00474 0.00004 0.00066 AFIX 147 H7 2 -0.143265 0.021727 0.986292 11.00000 -1.50000 AFIX 0 O8 5 0.009209 0.295917 0.679852 11.00000 0.01407 0.01981 = 0.01755 0.00521 0.00047 0.00085 AFIX 147 H8 2 0.082813 0.307577 0.637665 11.00000 -1.50000 AFIX 0 O9 5 0.420212 0.246069 1.163645 11.00000 0.01442 0.02809 = 0.02225 -0.00912 -0.00164 0.00208 AFIX 147 H9 2 0.346127 0.264708 1.200061 11.00000 -1.50000 AFIX 0 O10 5 0.563365 0.034929 0.850599 11.00000 0.01084 0.02364 = 0.02551 -0.00717 -0.00066 0.00073 AFIX 147 H10 2 0.644285 0.052798 0.876096 11.00000 -1.50000 AFIX 0 MOLE 2 C1 1 0.640267 0.131201 0.331968 11.00000 0.02661 0.03149 = 0.01941 -0.00026 0.00396 0.00958 AFIX 23 H1D 2 0.647746 0.196957 0.356256 11.00000 -1.20000 H1E 2 0.537548 0.114969 0.326323 11.00000 -1.20000 AFIX 0 C2 1 0.712382 0.072886 0.432640 11.00000 0.02536 0.02082 = 0.01773 -0.00134 0.00396 0.00452 C3 1 0.668868 -0.017680 0.451504 11.00000 0.02791 0.02593 = 0.02580 -0.00535 0.00489 -0.00227 AFIX 43 H3 2 0.594083 -0.042991 0.400174 11.00000 -1.20000 AFIX 0 C4 1 0.734650 -0.071081 0.545272 11.00000 0.04584 0.01846 = 0.03010 0.00087 0.01026 0.00069 AFIX 43 H4 2 0.703978 -0.132656 0.558864 11.00000 -1.20000 AFIX 0 C5 1 0.844700 -0.034769 0.618864 11.00000 0.05314 0.02803 = 0.02104 0.00369 0.00155 0.01307 AFIX 43 H5 2 0.888419 -0.071143 0.683953 11.00000 -1.20000 AFIX 0 C6 1 0.891320 0.053975 0.598265 11.00000 0.04107 0.03044 = 0.02105 -0.00535 -0.00682 0.00533 AFIX 43 H6 2 0.969611 0.077793 0.646705 11.00000 -1.20000 AFIX 0 C7 1 0.823962 0.108549 0.506811 11.00000 0.03512 0.02009 = 0.02139 -0.00194 0.00010 0.00003 AFIX 43 H7A 2 0.854061 0.170414 0.494773 11.00000 -1.20000 AFIX 0 N1 4 0.707965 0.116834 0.203833 11.00000 0.01711 0.01971 = 0.01731 -0.00039 -0.00175 0.00011 AFIX 137 H1A 2 0.798467 0.139885 0.205585 11.00000 -1.50000 H1B 2 0.655474 0.146406 0.142550 11.00000 -1.50000 H1C 2 0.710876 0.055524 0.185905 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009src0116 in P2(1)/c C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O6 O1 O4 O3 B2 - O7 O1 O2 B3 - O3 O8 O2 B4 - O9 O4 O5 B5 - O10 O6 O5 O1 - B2 B1 O2 - B2 B3 O3 - B3 B1 O4 - B4 B1 O5 - B5 B4 O6 - B5 B1 O7 - B2 O8 - B3 O9 - B4 O10 - B5 C1 - C2 N1 C2 - C3 C7 C1 C3 - C4 C2 C4 - C5 C3 C5 - C6 C4 C6 - C5 C7 C7 - C6 C2 N1 - C1 Operators for generating equivalent atoms: $1 -x, -y, -z+2 $2 x, -y+1/2, z-1/2 $3 x, -y+1/2, z+1/2 $4 x+1, y, z $5 x+1, -y+1/2, z-1/2 $6 x, y, z-1 $7 -x+1, -y, -z+1 16121 Reflections read, of which 484 rejected -12 =< h =< 11, -18 =< k =< 15, -13 =< l =< 13, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 3244 Unique reflections, of which 0 suppressed R(int) = 0.0375 R(sigma) = 0.0323 Friedel opposites merged Maximum memory for data reduction = 2312 / 32266 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 = 2885 / 264920 wR2 = 0.0922 before cycle 1 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.030 OSF Mean shift/esd = 0.004 Maximum = 0.030 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 2 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.002 OSF Mean shift/esd = 0.002 Maximum = -0.006 for U12 O8 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 3 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 4 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H10 Max. dU = 0.000 for B1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 5 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for B1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 6 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O3 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 7 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O3 Max. shift = 0.000 A for H10 Max. dU = 0.000 for B1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 8 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O3 Max. shift = 0.000 A for H7 Max. dU = 0.000 for C6 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2885 / 264920 wR2 = 0.0922 before cycle 9 for 3244 data and 213 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73132 0.00117 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O3 Max. shift = 0.000 A for H1A Max. dU = 0.000 for C4 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 -0.1433 0.0217 0.9863 147 0.840 0.000 O7 B2 H7 H8 0.0828 0.3076 0.6377 147 0.840 0.000 O8 B3 H8 H9 0.3461 0.2647 1.2001 147 0.840 0.000 O9 B4 H9 H10 0.6443 0.0528 0.8761 147 0.840 0.000 O10 B5 H10 H1D 0.6477 0.1970 0.3563 23 0.990 0.000 C1 C2 N1 H1E 0.5375 0.1150 0.3263 23 0.990 0.000 C1 C2 N1 H3 0.5941 -0.0430 0.4002 43 0.950 0.000 C3 C4 C2 H4 0.7040 -0.1327 0.5589 43 0.950 0.000 C4 C5 C3 H5 0.8884 -0.0711 0.6840 43 0.950 0.000 C5 C6 C4 H6 0.9696 0.0778 0.6467 43 0.950 0.000 C6 C5 C7 H7A 0.8541 0.1704 0.4948 43 0.950 0.000 C7 C6 C2 H1A 0.7985 0.1399 0.2056 137 0.910 0.000 N1 C1 H1A H1B 0.6555 0.1464 0.1425 137 0.910 0.000 N1 C1 H1A H1C 0.7109 0.0555 0.1859 137 0.910 0.000 N1 C1 H1A 2009src0116 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.20809 0.13669 0.89975 1.00000 0.00992 0.01510 0.01471 0.00095 -0.00066 -0.00009 0.01325 0.00253 0.00015 0.00011 0.00014 0.00000 0.00062 0.00077 0.00066 0.00055 0.00050 0.00053 0.00029 B2 -0.05322 0.11620 0.90580 1.00000 0.01289 0.01579 0.01268 -0.00208 0.00025 0.00061 0.01379 0.00255 0.00015 0.00011 0.00014 0.00000 0.00065 0.00077 0.00064 0.00055 0.00051 0.00054 0.00029 B3 0.04152 0.23241 0.77239 1.00000 0.01400 0.01494 0.01330 -0.00180 -0.00023 -0.00040 0.01408 0.00255 0.00015 0.00011 0.00014 0.00000 0.00066 0.00075 0.00064 0.00056 0.00051 0.00055 0.00029 B4 0.38291 0.19689 1.05882 1.00000 0.01451 0.01640 0.01631 0.00175 -0.00027 0.00014 0.01574 0.00271 0.00016 0.00011 0.00014 0.00000 0.00067 0.00080 0.00069 0.00058 0.00054 0.00056 0.00031 B5 0.46139 0.08942 0.90077 1.00000 0.01285 0.01477 0.01509 0.00203 0.00019 -0.00052 0.01424 0.00263 0.00015 0.00011 0.00014 0.00000 0.00065 0.00076 0.00066 0.00056 0.00052 0.00054 0.00029 O1 0.08038 0.08057 0.92409 1.00000 0.00976 0.01624 0.01820 0.00350 -0.00021 0.00011 0.01474 0.00162 0.00009 0.00007 0.00009 0.00000 0.00042 0.00051 0.00046 0.00037 0.00034 0.00035 0.00021 O2 -0.07352 0.19727 0.83950 1.00000 0.01191 0.01651 0.01789 0.00262 0.00128 0.00217 0.01543 0.00165 0.00009 0.00007 0.00009 0.00000 0.00043 0.00052 0.00046 0.00038 0.00035 0.00035 0.00021 O3 0.17702 0.20356 0.79682 1.00000 0.01153 0.01742 0.01533 0.00393 -0.00018 -0.00048 0.01476 0.00163 0.00009 0.00007 0.00009 0.00000 0.00043 0.00052 0.00044 0.00037 0.00034 0.00035 0.00021 O4 0.24479 0.18549 1.01912 1.00000 0.01154 0.01859 0.01466 -0.00187 0.00008 0.00169 0.01493 0.00162 0.00010 0.00007 0.00009 0.00000 0.00043 0.00052 0.00044 0.00037 0.00033 0.00035 0.00021 O5 0.49451 0.15618 0.99220 1.00000 0.01035 0.01871 0.01860 -0.00230 -0.00027 0.00020 0.01589 0.00161 0.00009 0.00007 0.00009 0.00000 0.00041 0.00053 0.00046 0.00039 0.00034 0.00036 0.00021 O6 0.32322 0.07553 0.86173 1.00000 0.01077 0.01592 0.01622 -0.00089 -0.00028 0.00012 0.01431 0.00158 0.00009 0.00007 0.00009 0.00000 0.00042 0.00050 0.00044 0.00037 0.00033 0.00035 0.00020 O7 -0.16942 0.07126 0.95169 1.00000 0.01080 0.01803 0.02044 0.00474 0.00004 0.00066 0.01642 0.00168 0.00009 0.00007 0.00009 0.00000 0.00042 0.00054 0.00048 0.00039 0.00035 0.00036 0.00021 H7 -0.14326 0.02173 0.98630 1.00000 0.02463 0.00000 0.00000 O8 0.00921 0.29592 0.67985 1.00000 0.01407 0.01981 0.01755 0.00521 0.00047 0.00084 0.01714 0.00172 0.00010 0.00007 0.00009 0.00000 0.00045 0.00054 0.00047 0.00039 0.00036 0.00038 0.00022 H8 0.08281 0.30758 0.63767 1.00000 0.02571 0.00000 0.00000 O9 0.42021 0.24607 1.16365 1.00000 0.01442 0.02810 0.02225 -0.00912 -0.00164 0.00208 0.02160 0.00169 0.00010 0.00008 0.00009 0.00000 0.00046 0.00061 0.00051 0.00044 0.00038 0.00041 0.00023 H9 0.34613 0.26471 1.20006 1.00000 0.03241 0.00000 0.00000 O10 0.56336 0.03493 0.85060 1.00000 0.01084 0.02364 0.02552 -0.00717 -0.00066 0.00073 0.02001 0.00169 0.00010 0.00007 0.00010 0.00000 0.00043 0.00058 0.00052 0.00043 0.00037 0.00038 0.00023 H10 0.64428 0.05279 0.87611 1.00000 0.03001 0.00000 0.00000 C1 0.64027 0.13120 0.33197 1.00000 0.02661 0.03149 0.01941 -0.00027 0.00397 0.00957 0.02580 0.00295 0.00017 0.00012 0.00014 0.00000 0.00076 0.00092 0.00070 0.00062 0.00058 0.00065 0.00034 H1D 0.64774 0.19696 0.35625 1.00000 0.03096 0.00000 0.00000 H1E 0.53755 0.11497 0.32632 1.00000 0.03096 0.00000 0.00000 C2 0.71238 0.07289 0.43264 1.00000 0.02536 0.02082 0.01772 -0.00134 0.00396 0.00452 0.02127 0.00266 0.00016 0.00011 0.00014 0.00000 0.00073 0.00078 0.00065 0.00057 0.00054 0.00058 0.00031 C3 0.66887 -0.01768 0.45150 1.00000 0.02791 0.02593 0.02579 -0.00535 0.00489 -0.00228 0.02650 0.00285 0.00017 0.00012 0.00015 0.00000 0.00077 0.00087 0.00075 0.00064 0.00061 0.00064 0.00034 H3 0.59409 -0.04299 0.40017 1.00000 0.03181 0.00000 0.00000 C4 0.73465 -0.07108 0.54527 1.00000 0.04584 0.01846 0.03010 0.00087 0.01027 0.00069 0.03138 0.00319 0.00020 0.00012 0.00016 0.00000 0.00100 0.00083 0.00083 0.00066 0.00073 0.00070 0.00038 H4 0.70397 -0.13265 0.55887 1.00000 0.03766 0.00000 0.00000 C5 0.84470 -0.03477 0.61887 1.00000 0.05314 0.02803 0.02104 0.00369 0.00156 0.01307 0.03406 0.00335 0.00021 0.00013 0.00015 0.00000 0.00108 0.00095 0.00075 0.00068 0.00071 0.00079 0.00040 H5 0.88842 -0.07114 0.68395 1.00000 0.04087 0.00000 0.00000 C6 0.89132 0.05397 0.59826 1.00000 0.04108 0.03045 0.02105 -0.00535 -0.00682 0.00533 0.03092 0.00296 0.00019 0.00012 0.00015 0.00000 0.00093 0.00094 0.00074 0.00066 0.00066 0.00074 0.00037 H6 0.96961 0.07779 0.64670 1.00000 0.03711 0.00000 0.00000 C7 0.82396 0.10855 0.50681 1.00000 0.03513 0.02008 0.02139 -0.00194 0.00010 0.00003 0.02554 0.00276 0.00017 0.00011 0.00014 0.00000 0.00085 0.00081 0.00071 0.00061 0.00061 0.00064 0.00033 H7A 0.85406 0.17042 0.49478 1.00000 0.03064 0.00000 0.00000 N1 0.70796 0.11683 0.20383 1.00000 0.01712 0.01971 0.01732 -0.00039 -0.00175 0.00010 0.01807 0.00204 0.00012 0.00009 0.00011 0.00000 0.00055 0.00065 0.00056 0.00047 0.00044 0.00046 0.00025 H1A 0.79847 0.13988 0.20559 1.00000 0.02710 0.00000 0.00000 H1B 0.65547 0.14641 0.14255 1.00000 0.02710 0.00000 0.00000 H1C 0.71087 0.05552 0.18590 1.00000 0.02710 0.00000 0.00000 Final Structure Factor Calculation for 2009src0116 in P2(1)/c Total number of l.s. parameters = 213 Maximum vector length = 511 Memory required = 2672 / 24017 wR2 = 0.0922 before cycle 10 for 3244 data and 0 / 213 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0391 for 2877 Fo > 4sig(Fo) and 0.0457 for all 3244 data wR2 = 0.0922, GooF = S = 1.074, Restrained GooF = 1.074 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0159 0.0140 0.0098 B1 0.0169 0.0129 0.0115 B2 0.0161 0.0142 0.0120 B3 0.0181 0.0150 0.0141 B4 0.0170 0.0132 0.0125 B5 0.0209 0.0136 0.0097 O1 0.0204 0.0148 0.0110 O2 0.0205 0.0123 0.0115 O3 0.0197 0.0140 0.0111 O4 0.0210 0.0164 0.0103 O5 0.0170 0.0152 0.0107 O6 0.0241 0.0144 0.0107 O7 0.0241 0.0141 0.0132 O8 0.0352 0.0156 0.0140 O9 0.0319 0.0174 0.0108 O10 0.0391 0.0222 0.0161 C1 0.0287 0.0206 0.0145 C2 0.0346 0.0249 0.0200 C3 0.0504 0.0253 0.0184 C4 0.0588 0.0247 0.0187 C5 0.0465 0.0286 0.0177 C6 0.0351 0.0228 0.0187 C7 0.0199 0.0190 0.0153 N1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.036 0.051 0.066 0.082 0.103 0.135 0.200 1.000 Number in group 334. 327. 314. 347. 319. 312. 325. 317. 323. 326. GooF 1.192 1.092 1.137 1.078 1.070 1.034 0.988 0.935 1.036 1.145 K 1.981 1.158 0.997 0.976 0.999 0.993 1.002 1.001 1.009 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 337. 327. 309. 329. 319. 329. 320. 327. 320. 327. GooF 1.176 1.117 1.047 1.005 1.027 0.963 0.921 0.860 1.088 1.422 K 1.056 1.043 1.016 1.009 0.993 0.993 0.992 0.989 1.012 1.005 R1 0.096 0.092 0.081 0.069 0.055 0.043 0.029 0.028 0.030 0.028 Recommended weighting scheme: WGHT 0.0265 0.9479 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) -6 3 3 11.36 0.11 4.49 0.002 1.37 -2 2 1 572.60 703.02 3.84 0.194 3.69 4 0 0 29.91 13.24 3.60 0.027 2.34 -4 11 10 -0.58 12.58 3.45 0.026 0.78 3 3 0 150.13 201.52 3.41 0.104 2.62 2 0 2 451.15 547.97 3.41 0.171 3.46 1 4 3 1995.13 1734.69 3.35 0.304 2.42 -1 1 3 1249.80 1450.14 3.27 0.278 3.20 -5 4 1 85.87 123.64 3.27 0.081 1.64 0 15 8 29.50 0.59 3.27 0.006 0.78 8 8 7 87.36 55.28 3.22 0.054 0.82 -1 10 10 16.63 2.71 3.19 0.012 0.85 0 0 12 71.93 113.25 3.08 0.078 0.87 1 3 1 2436.14 2822.42 3.04 0.388 3.97 2 9 2 55.58 84.53 3.03 0.067 1.46 9 6 1 141.02 186.76 3.01 0.100 0.95 4 13 8 87.63 56.63 3.00 0.055 0.80 3 1 0 25.45 12.72 3.00 0.026 3.05 -3 3 2 1221.02 1070.35 2.95 0.239 2.35 -1 7 2 5.97 0.00 2.95 0.000 1.89 -1 1 1 1609.51 1815.47 2.91 0.311 6.32 3 11 4 17.77 35.79 2.90 0.044 1.10 3 2 0 162.18 205.42 2.84 0.105 2.86 0 1 4 326.70 389.68 2.81 0.144 2.58 2 15 0 26.25 48.50 2.80 0.051 0.95 -3 3 3 24.16 12.48 2.77 0.026 2.11 -4 15 1 27.00 7.82 2.77 0.020 0.89 0 4 0 923.54 1062.41 2.72 0.238 3.63 3 7 7 103.27 138.32 2.70 0.086 1.13 1 8 9 20.10 36.79 2.69 0.044 0.97 -2 9 11 8.45 0.44 2.69 0.005 0.81 3 0 0 3.87 0.02 2.67 0.001 3.12 -3 13 2 2.41 12.60 2.66 0.026 1.03 0 4 4 514.53 442.71 2.65 0.154 2.12 3 5 4 4.44 0.24 2.63 0.004 1.64 2 2 1 1273.08 1426.40 2.63 0.276 3.67 2 10 9 18.36 38.16 2.61 0.045 0.89 2 1 2 514.57 591.29 2.58 0.178 3.37 0 2 13 36.51 60.90 2.58 0.057 0.80 -5 0 10 8.29 20.94 2.56 0.033 0.92 2 1 1 87.46 64.56 2.55 0.059 4.08 3 12 9 21.18 8.06 2.55 0.021 0.81 5 0 0 154.52 121.48 2.55 0.081 1.87 5 7 11 15.00 5.15 2.54 0.017 0.78 -5 15 5 28.74 9.91 2.52 0.023 0.80 -2 8 12 13.93 2.01 2.52 0.010 0.78 0 11 8 28.23 52.26 2.51 0.053 0.93 -6 2 1 27.15 15.49 2.50 0.029 1.51 11 2 5 418.22 339.44 2.48 0.135 0.78 5 2 6 999.10 1133.91 2.48 0.246 1.25 Bond lengths and angles B1 - Distance Angles O6 1.4550 (0.0017) O1 1.4706 (0.0017) 108.36 (0.11) O4 1.4727 (0.0017) 111.15 (0.10) 107.45 (0.10) O3 1.4761 (0.0017) 109.91 (0.10) 109.78 (0.10) 110.13 (0.11) B1 - O6 O1 O4 B2 - Distance Angles O7 1.3606 (0.0017) O1 1.3632 (0.0017) 120.22 (0.13) O2 1.3781 (0.0018) 118.81 (0.12) 120.96 (0.12) B2 - O7 O1 B3 - Distance Angles O3 1.3556 (0.0017) O8 1.3680 (0.0018) 122.59 (0.12) O2 1.3897 (0.0017) 121.29 (0.12) 116.11 (0.12) B3 - O3 O8 B4 - Distance Angles O9 1.3508 (0.0018) O4 1.3615 (0.0017) 123.06 (0.13) O5 1.3944 (0.0018) 116.32 (0.12) 120.61 (0.12) B4 - O9 O4 B5 - Distance Angles O10 1.3506 (0.0018) O6 1.3649 (0.0017) 117.88 (0.13) O5 1.3938 (0.0018) 121.51 (0.12) 120.59 (0.12) B5 - O10 O6 O1 - Distance Angles B2 1.3632 (0.0017) B1 1.4706 (0.0017) 120.68 (0.11) O1 - B2 O2 - Distance Angles B2 1.3781 (0.0018) B3 1.3897 (0.0017) 117.75 (0.11) O2 - B2 O3 - Distance Angles B3 1.3556 (0.0017) B1 1.4761 (0.0017) 121.00 (0.11) O3 - B3 O4 - Distance Angles B4 1.3615 (0.0017) B1 1.4727 (0.0017) 121.77 (0.11) O4 - B4 O5 - Distance Angles B5 1.3938 (0.0018) B4 1.3944 (0.0018) 118.50 (0.11) O5 - B5 O6 - Distance Angles B5 1.3649 (0.0017) B1 1.4550 (0.0017) 121.94 (0.11) O6 - B5 O7 - Distance Angles B2 1.3606 (0.0017) H7 0.8400 109.47 O7 - B2 O8 - Distance Angles B3 1.3680 (0.0018) H8 0.8400 109.47 O8 - B3 O9 - Distance Angles B4 1.3508 (0.0018) H9 0.8400 109.47 O9 - B4 O10 - Distance Angles B5 1.3506 (0.0018) H10 0.8400 109.47 O10 - B5 C1 - Distance Angles C2 1.5041 (0.0021) N1 1.5053 (0.0018) 110.87 (0.12) H1D 0.9900 109.47 109.47 H1E 0.9900 109.47 109.47 108.05 C1 - C2 N1 H1D C2 - Distance Angles C3 1.3910 (0.0023) C7 1.3919 (0.0022) 119.39 (0.14) C1 1.5041 (0.0021) 120.14 (0.14) 120.47 (0.14) C2 - C3 C7 C3 - Distance Angles C4 1.3878 (0.0024) C2 1.3910 (0.0023) 120.04 (0.15) H3 0.9500 119.98 119.98 C3 - C4 C2 C4 - Distance Angles C5 1.3816 (0.0026) C3 1.3878 (0.0024) 120.05 (0.16) H4 0.9500 119.97 119.97 C4 - C5 C3 C5 - Distance Angles C6 1.3778 (0.0026) C4 1.3816 (0.0026) 120.29 (0.16) H5 0.9500 119.86 119.86 C5 - C6 C4 C6 - Distance Angles C5 1.3778 (0.0026) C7 1.3872 (0.0022) 120.02 (0.16) H6 0.9500 119.99 119.99 C6 - C5 C7 C7 - Distance Angles C6 1.3872 (0.0022) C2 1.3919 (0.0021) 120.16 (0.16) H7A 0.9500 119.92 119.92 C7 - C6 C2 N1 - Distance Angles C1 1.5053 (0.0018) H1A 0.9100 109.47 H1B 0.9100 109.47 109.47 H1C 0.9100 109.47 109.47 109.47 N1 - C1 H1A H1B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.85 2.6855(14) 174.5 O7-H7...O1_$1 0.84 1.97 2.8030(13) 169.1 O8-H8...O4_$2 0.84 1.94 2.7812(13) 173.8 O9-H9...O3_$3 0.84 1.92 2.7513(13) 168.9 O10-H10...O7_$4 0.91 2.20 3.1019(15) 171.0 N1-H1A...O8_$5 0.91 2.17 3.0162(15) 154.9 N1-H1B...O5_$6 0.91 2.64 3.3024(16) 129.8 N1-H1B...O9_$6 0.91 1.99 2.8892(16) 168.8 N1-H1C...O6_$7 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)