+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:27:55 on 19-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0010 in P-4 New: P-421m CELL 0.71073 10.6034 10.6034 6.3943 90.000 90.000 90.000 ZERR 2.00 0.0001 0.0001 0.0002 0.000 0.000 0.000 LATT -1 SYMM Y, - X, - Z SYMM - X, - Y, Z SYMM - Y, X, - Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM 1/2 - Y, 1/2 - X, Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + Y, 1/2 + X, Z SFAC C H SE SN UNIT 20 44 2 4 V = 718.92 F(000) = 432.0 Mu = 5.97 mm-1 Cell Wt = 917.23 Rho = 2.119 MERG 2 TWIN BASF 0.11974 EXTI 0.03282 FMAP 2 PLAN 20 ACTA BOND $H CONF WGHT 0.05240 0.73270 L.S. 4 TEMP -153.00 FVAR 1.82381 SN1 4 0.270572 0.229428 0.388307 10.50000 0.01988 0.01988 = 0.02927 -0.00036 0.00036 0.00220 SE1 3 0.500000 0.000000 0.539933 10.25000 0.02502 0.02502 = 0.02531 0.00000 0.00000 0.00504 C1 1 0.410662 0.089338 0.334174 10.50000 0.02226 0.02226 = 0.03673 -0.00137 0.00137 0.00334 C2 1 0.452897 0.047103 0.145322 10.50000 0.02379 0.02379 = 0.03272 0.00200 -0.00200 0.00719 AFIX 23 H2A 2 0.485755 0.120514 0.066691 10.50000 -1.20000 H2B 2 0.379486 0.014245 0.066691 10.50000 -1.20000 AFIX 0 C3 1 0.245522 0.254478 0.717902 10.50000 0.02732 0.02732 = 0.04401 -0.00467 0.00467 0.00204 AFIX 137 H3A 2 0.230663 0.172382 0.783846 10.50000 -1.50000 H3B 2 0.172950 0.309656 0.743095 10.50000 -1.50000 H3C 2 0.321485 0.292864 0.777648 10.50000 -1.50000 AFIX 0 C4 1 0.101915 0.161309 0.246663 11.00000 0.02792 0.03525 = 0.03914 -0.00480 -0.00537 0.00018 AFIX 137 H4A 2 0.116342 0.076240 0.191735 11.00000 -1.50000 H4B 2 0.077506 0.217566 0.131998 11.00000 -1.50000 H4C 2 0.034325 0.158791 0.351112 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04src0010 in P-4 New: P-421m C 0.770 H 0.320 SE 1.170 SN 1.400 Sn1 - C1 C4 C4_$2 C3 Se1 - C1_$1 C1 C1 - C2 Se1 Sn1 C2 - C1 C2_$1 C3 - Sn1 C4 - Sn1 Operators for generating equivalent atoms: $1 -x+1, -y, z $2 -y+1/2, -x+1/2, z h k l Fo^2 Sigma Why rejected 0 11 0 121.69 20.32 observed but should be systematically absent 0 9 0 261.88 63.40 observed but should be systematically absent 0 9 0 743.49 105.81 observed but should be systematically absent 0 9 0 202.75 32.91 observed but should be systematically absent 0 9 0 85.26 17.96 observed but should be systematically absent 0 9 0 395.93 52.86 observed but should be systematically absent 0 7 0 87.07 15.38 observed but should be systematically absent 0 7 0 149.90 24.20 observed but should be systematically absent 0 7 0 129.10 14.93 observed but should be systematically absent 0 5 0 400.21 21.22 observed but should be systematically absent 0 5 0 228.25 26.01 observed but should be systematically absent 0 5 0 215.46 16.25 observed but should be systematically absent 0 5 0 322.54 22.34 observed but should be systematically absent 0 3 0 150.46 11.21 observed but should be systematically absent 0 3 0 146.88 11.38 observed but should be systematically absent 0 3 0 167.89 10.96 observed but should be systematically absent 0 3 0 59.30 10.79 observed but should be systematically absent 0 3 0 189.56 11.00 observed but should be systematically absent 0 3 0 144.89 11.20 observed but should be systematically absent 0 3 0 135.58 11.37 observed but should be systematically absent 0 3 0 91.65 10.81 observed but should be systematically absent 0 5 0 150.44 20.79 observed but should be systematically absent 0 5 0 416.02 21.23 observed but should be systematically absent 0 5 0 150.82 10.84 observed but should be systematically absent 0 5 0 394.85 22.39 observed but should be systematically absent 0 7 0 116.05 14.53 observed but should be systematically absent 0 7 0 87.07 15.38 observed but should be systematically absent 0 7 0 94.35 9.95 observed but should be systematically absent 0 7 0 72.55 16.75 observed but should be systematically absent 0 9 0 230.16 49.34 observed but should be systematically absent 0 9 0 193.57 35.22 observed but should be systematically absent 0 11 0 110.04 15.74 observed but should be systematically absent 0 13 0 114.07 14.77 observed but should be systematically absent 10020 Reflections read, of which 46 rejected -13 =< h =< 13, -13 =< k =< 13, -8 =< l =< 8, Max. 2-theta = 55.14 33 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 2 3 0 99.06 1.81 16 9.57 4 8 0 14366.87 111.08 17 583.03 0 10 0 132.37 4.56 10 34.89 1 11 0 546.28 9.36 18 68.09 -1 1 1 37584.92 407.99 8 3717.51 1 1 1 30248.74 411.26 7 2066.01 -2 2 1 67835.30 828.73 7 4962.93 -1 2 1 4390.60 36.77 18 212.31 2 2 1 66640.04 825.62 7 4507.53 5 7 1 930.67 5.75 15 55.67 -6 10 1 3814.79 56.23 6 316.05 0 0 2 470.00 10.98 4 130.28 -2 2 2 9109.45 109.11 9 785.24 -1 2 2 7730.14 68.38 18 405.17 -3 3 2 39345.54 441.95 9 2474.39 -1 3 2 41465.44 335.56 18 1912.28 -8 8 2 7311.22 148.87 3 998.36 -6 10 2 5137.77 73.19 6 481.18 -4 11 2 9874.78 136.88 7 980.19 -4 12 2 2759.23 59.95 5 337.60 -3 13 2 545.70 17.04 4 96.78 0 0 3 3552.85 69.60 4 400.56 -1 1 3 30971.17 374.19 8 2095.79 -2 2 3 4031.26 52.92 9 325.91 -1 3 3 35289.42 284.26 18 1681.41 -2 4 3 20300.34 167.00 18 852.91 -2 6 3 1062.14 11.02 18 55.51 -8 8 3 3323.07 101.54 2 661.91 -7 9 3 3646.91 77.79 4 475.22 -5 9 3 1146.31 20.18 8 103.48 -4 10 3 3177.30 46.22 8 268.85 -4 11 3 8282.95 164.34 5 930.13 -3 12 3 2189.31 55.54 4 408.79 0 0 4 12132.83 219.99 4 1437.55 -1 1 4 3999.18 52.75 8 330.90 0 1 4 2211.63 22.55 16 126.30 -2 2 4 13138.19 166.59 8 1049.25 -1 2 4 5081.83 50.28 16 260.00 0 2 4 24870.67 221.31 15 1206.02 -3 3 4 2378.37 30.98 9 176.26 -2 3 4 2128.38 20.12 18 105.16 -3 4 4 9808.74 84.35 18 437.30 -2 4 4 20678.83 167.17 18 965.95 -5 6 4 8659.47 82.34 14 465.35 -7 8 4 4445.77 96.59 4 571.33 -7 9 4 4492.19 95.07 4 573.90 -6 9 4 2497.33 59.80 4 307.32 -3 9 4 3461.80 45.24 9 253.54 -5 10 4 4916.10 110.53 4 603.41 -4 11 4 1805.54 40.71 5 278.81 ** etc. ** 122 Inconsistent equivalents 896 Unique reflections, of which 0 suppressed R(int) = 0.1260 R(sigma) = 0.0434 Friedel opposites not merged Maximum memory for data reduction = 1124 / 9365 Special position constraints for Sn1 y = -1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Se1 x = 0.5000 y = 0.0000 U22 = 1.0 * U11 U23 = 0 U13 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for C1 y = -1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C2 y = -1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C3 y = -1.0 * x + 0.5000 U22 = 1.0 * U11 U13 =-1.0 * U23 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1286 / 66906 wR2 = 0.0928 before cycle 1 for 896 data and 42 / 42 parameters GooF = S = 1.221; Restrained GooF = 1.221 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 0.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.82367 0.00941 -0.014 OSF 2 0.11974 0.03110 0.000 BASF 1 3 0.03279 0.00296 -0.009 EXTI Mean shift/su = 0.004 Maximum = 0.024 for U23 Sn1 Max. shift = 0.000 A for H3B Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1286 / 66906 wR2 = 0.0928 before cycle 2 for 896 data and 42 / 42 parameters GooF = S = 1.221; Restrained GooF = 1.221 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 0.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.82366 0.00941 -0.002 OSF 2 0.11974 0.03109 0.000 BASF 1 3 0.03279 0.00296 -0.002 EXTI Mean shift/su = 0.001 Maximum = 0.008 for U23 Sn1 Max. shift = 0.000 A for H3B Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1286 / 66906 wR2 = 0.0928 before cycle 3 for 896 data and 42 / 42 parameters GooF = S = 1.221; Restrained GooF = 1.221 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 0.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.82366 0.00941 0.000 OSF 2 0.11974 0.03110 0.000 BASF 1 3 0.03279 0.00296 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.001 for z C4 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1286 / 66906 wR2 = 0.0928 before cycle 4 for 896 data and 42 / 42 parameters GooF = S = 1.221; Restrained GooF = 1.221 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 0.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.82366 0.00941 0.000 OSF 2 0.11974 0.03110 0.000 BASF 1 3 0.03279 0.00296 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z Sn1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for C3 Largest correlation matrix elements 0.843 U11 Sn1 / OSF 0.664 U33 Sn1 / OSF 0.533 U11 Sn1 / EXTI 0.711 EXTI / OSF 0.586 U11 Se1 / OSF 0.519 U11 Se1 / U11 Sn1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4858 0.1205 0.0667 23 0.990 0.000 C2 C1 C2_$1 H2B 0.3795 0.0142 0.0667 23 0.990 0.000 C2 C1 C2_$1 H3A 0.2306 0.1724 0.7838 137 0.980 0.000 C3 Sn1 H3A H3B 0.1730 0.3097 0.7431 137 0.980 0.000 C3 Sn1 H3A H3C 0.3215 0.2928 0.7777 137 0.980 0.000 C3 Sn1 H3A H4A 0.1163 0.0762 0.1917 137 0.980 0.000 C4 Sn1 H4A H4B 0.0775 0.2176 0.1320 137 0.980 0.000 C4 Sn1 H4A H4C 0.0343 0.1588 0.3511 137 0.980 0.000 C4 Sn1 H4A 04src0010 in P-4 New: P-421m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Sn1 0.27057 0.22943 0.38831 0.50000 0.01988 0.01988 0.02926 -0.00036 0.00036 0.00220 0.02301 0.00053 0.00003 0.00003 0.00008 0.00000 0.00026 0.00026 0.00035 0.00012 0.00012 0.00016 0.00024 Se1 0.50000 0.00000 0.53993 0.25000 0.02502 0.02502 0.02530 0.00000 0.00000 0.00504 0.02511 0.00118 0.00000 0.00000 0.00018 0.00000 0.00035 0.00035 0.00050 0.00000 0.00000 0.00041 0.00029 C1 0.41066 0.08934 0.33416 0.50000 0.02225 0.02225 0.03676 -0.00138 0.00138 0.00335 0.02709 0.00838 0.00052 0.00052 0.00131 0.00000 0.00196 0.00196 0.00433 0.00221 0.00221 0.00285 0.00160 C2 0.45290 0.04710 0.14532 0.50000 0.02379 0.02379 0.03272 0.00200 -0.00200 0.00719 0.02677 0.00806 0.00049 0.00049 0.00126 0.00000 0.00219 0.00219 0.00379 0.00200 0.00200 0.00302 0.00157 H2A 0.48575 0.12051 0.06669 0.50000 0.03212 0.00000 0.00000 H2B 0.37949 0.01425 0.06669 0.50000 0.03212 0.00000 0.00000 C3 0.24552 0.25448 0.71790 0.50000 0.02731 0.02731 0.04404 -0.00466 0.00466 0.00203 0.03288 0.00962 0.00056 0.00056 0.00150 0.00000 0.00228 0.00228 0.00457 0.00274 0.00274 0.00283 0.00167 H3A 0.23065 0.17238 0.78384 0.50000 0.04933 0.00000 0.00000 H3B 0.17296 0.30967 0.74310 0.50000 0.04933 0.00000 0.00000 H3C 0.32149 0.29285 0.77765 0.50000 0.04933 0.00000 0.00000 C4 0.10192 0.16131 0.24667 1.00000 0.02792 0.03524 0.03913 -0.00480 -0.00536 0.00018 0.03410 0.01151 0.00058 0.00061 0.00114 0.00000 0.00267 0.00289 0.00337 0.00255 0.00256 0.00222 0.00127 H4A 0.11634 0.07624 0.19175 1.00000 0.05114 0.00000 0.00000 H4B 0.07751 0.21756 0.13201 1.00000 0.05114 0.00000 0.00000 H4C 0.03433 0.15879 0.35112 1.00000 0.05114 0.00000 0.00000 Final Structure Factor Calculation for 04src0010 in P-4 New: P-421m Total number of l.s. parameters = 42 Maximum vector length = 511 Memory required = 1246 / 25046 wR2 = 0.0928 before cycle 5 for 896 data and 2 / 42 parameters GooF = S = 1.221; Restrained GooF = 1.221 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0524 * P )^2 + 0.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0378 for 895 Fo > 4sig(Fo) and 0.0378 for all 896 data wR2 = 0.0928, GooF = S = 1.221, Restrained GooF = 1.221 for all data Occupancy sum of asymmetric unit = 3.25 for non-hydrogen and 5.50 for hydrogen atoms Principal mean square atomic displacements U 0.0293 0.0221 0.0177 Sn1 0.0301 0.0253 0.0200 Se1 0.0370 0.0256 0.0187 C1 0.0332 0.0310 0.0161 C2 0.0461 0.0293 0.0232 C3 0.0437 0.0331 0.0255 C4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.058 0.087 0.112 0.140 0.167 0.191 0.220 0.265 0.342 1.000 Number in group 93. 88. 92. 90. 86. 89. 89. 92. 87. 90. GooF 1.815 0.890 0.954 0.849 0.931 1.006 0.935 1.092 1.208 1.922 K 1.095 1.030 1.027 1.008 0.988 0.999 1.006 1.002 1.004 1.017 Resolution(A) 0.77 0.79 0.83 0.87 0.92 0.97 1.05 1.16 1.33 1.68 inf Number in group 90. 96. 90. 90. 84. 89. 90. 89. 88. 90. GooF 0.997 1.076 0.864 0.932 0.949 0.926 1.061 1.014 1.331 2.333 K 1.050 1.039 1.024 1.029 1.000 1.001 0.989 0.982 0.981 1.034 R1 0.047 0.042 0.034 0.031 0.025 0.021 0.024 0.027 0.036 0.065 Recommended weighting scheme: WGHT 0.0524 0.7331 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)/su Fc/Fc(max) Resolution(A) 0 0 1 23552.55 37460.49 6.13 1.000 6.39 0 1 2 65.65 122.13 4.51 0.057 3.06 3 5 0 63.98 33.98 3.79 0.030 1.82 4 4 0 33479.23 25268.96 3.75 0.821 1.87 3 9 0 21.58 5.50 3.64 0.012 1.12 0 4 0 40765.24 29764.55 3.61 0.891 2.65 0 1 4 673.32 936.26 3.45 0.158 1.58 0 2 0 17180.10 12551.19 3.45 0.579 5.30 4 10 0 20.09 6.22 3.39 0.013 0.98 2 11 0 15.15 1.11 3.39 0.005 0.95 1 4 0 7388.04 5982.44 3.21 0.400 2.57 2 13 0 10.68 1.37 3.14 0.006 0.81 0 4 1 24883.94 20039.10 3.10 0.731 2.45 2 3 0 29.80 12.32 3.09 0.018 2.94 0 5 4 31.73 14.01 3.01 0.019 1.28 0 3 1 4659.44 3786.80 2.98 0.318 3.09 1 3 0 7107.56 5856.58 2.96 0.395 3.35 1 2 0 2927.00 2378.71 2.93 0.252 4.74 0 6 0 5212.86 4201.01 2.88 0.335 1.77 0 4 7 7.04 0.13 2.83 0.002 0.86 0 10 0 39.80 3.13 2.79 0.009 1.06 1 13 0 477.01 356.55 2.75 0.098 0.81 2 9 0 19.78 8.20 2.70 0.015 1.15 1 1 2 19424.04 24054.92 2.64 0.801 2.94 1 4 1 3493.29 2922.87 2.64 0.279 2.39 0 1 1 517.13 655.60 2.63 0.132 5.48 1 1 3 10851.95 13313.97 2.58 0.596 2.05 -1 1 2 19926.46 24806.21 2.53 0.814 2.94 0 3 6 16.73 3.49 2.53 0.010 1.02 -1 2 4 1565.90 1944.12 2.45 0.228 1.51 1 2 4 1742.43 2112.60 2.41 0.237 1.51 -1 4 2 205.56 160.81 2.34 0.066 2.00 0 0 4 3904.33 5352.65 2.28 0.378 1.60 1 11 0 164.40 101.68 2.24 0.052 0.96 -1 4 1 3327.20 2847.40 2.23 0.276 2.39 6 8 0 18.02 8.40 2.22 0.015 1.06 2 4 1 3058.36 2618.82 2.20 0.264 2.22 1 1 4 1088.13 1339.89 2.14 0.189 1.56 2 3 1 1479.87 1248.02 2.14 0.183 2.67 0 2 4 8401.54 10059.06 2.14 0.518 1.53 1 6 1 5367.68 4636.75 2.12 0.352 1.68 1 4 2 214.31 170.78 2.10 0.068 2.00 0 2 3 8808.10 10285.03 2.09 0.524 1.98 1 6 0 8900.39 7722.94 2.09 0.454 1.74 -1 1 3 11324.80 13887.16 2.08 0.609 2.05 0 1 3 93.25 69.76 2.08 0.043 2.09 0 3 7 11.51 4.46 2.07 0.011 0.88 3 11 4 49.14 33.33 2.05 0.030 0.80 0 12 3 22.99 12.25 2.01 0.018 0.82 -1 1 4 1226.76 1532.84 1.97 0.202 1.56 Bond lengths and angles Sn1 - Distance Angles C1 2.1291 (0.0077) C4 2.1307 (0.0065) 106.26 (0.20) C4_$2 2.1307 (0.0065) 106.26 (0.20) 112.85 (0.38) C3 2.1407 (0.0094) 109.46 (0.33) 110.88 (0.23) 110.88 (0.22) Sn1 - C1 C4 C4_$2 Se1 - Distance Angles C1_$1 1.8777 (0.0082) C1 1.8777 (0.0082) 91.03 (0.49) Se1 - C1_$1 C1 - Distance Angles C2 1.3635 (0.0110) Se1 1.8777 (0.0082) 106.81 (0.53) Sn1 2.1291 (0.0077) 127.03 (0.58) 126.16 (0.42) C1 - C2 Se1 C2 - Distance Angles C1 1.3635 (0.0110) C2_$1 1.4127 (0.0147) 117.68 (0.44) H2A 0.9900 107.89 107.89 H2B 0.9900 107.89 107.89 107.19 C2 - C1 C2_$1 H2A C3 - Distance Angles Sn1 2.1407 (0.0094) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - Sn1 H3A H3B C4 - Distance Angles Sn1 2.1307 (0.0065) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - Sn1 H4A H4B Selected torsion angles 0.00 C1_$1 - Se1 - C1 - C2 180.00 C1_$1 - Se1 - C1 - Sn1 60.21 ( 0.21) C4 - Sn1 - C1 - C2 -60.21 ( 0.21) C4_$2 - Sn1 - C1 - C2 180.00 C3 - Sn1 - C1 - C2 -119.79 ( 0.21) C4 - Sn1 - C1 - Se1 119.79 ( 0.21) C4_$2 - Sn1 - C1 - Se1 0.00 C3 - Sn1 - C1 - Se1 0.00 ( 0.00) Se1 - C1 - C2 - C2_$1 180.00 ( 0.00) Sn1 - C1 - C2 - C2_$1 FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.0399 for 530 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.15 at 0.2592 0.2408 0.5204 [ 0.86 A from SN1 ] Deepest hole -1.66 at 0.3361 0.1639 0.3849 [ 0.98 A from SN1 ] Mean = 0.01, Rms deviation from mean = 0.28 e/A^3, Highest memory used = 1320 / 12849 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2592 0.2408 0.5204 0.50000 0.05 2.15 0.86 SN1 1.28 C3 1.84 H3B 1.86 H3C Q2 1 0.2701 0.2299 0.2605 0.50000 0.05 1.68 0.82 SN1 1.93 C4 2.16 C1 2.21 H4B Q3 1 0.5000 0.0000 0.6613 0.25000 0.05 1.40 0.78 SE1 2.48 C1 2.89 H2A 2.89 H2B Q4 1 0.5000 0.0000 0.4004 0.25000 0.05 0.84 0.89 SE1 1.40 C1 1.78 C2 2.49 H2A Q5 1 0.0192 0.2504 -0.0550 1.00000 0.05 0.56 1.39 H4B 1.42 H2A 1.42 H2B 1.95 H4A Q6 1 -0.0057 0.2619 0.2767 1.00000 0.05 0.55 1.27 H4C 1.36 H4B 1.57 C4 1.84 H3A Q7 1 0.2847 0.2153 0.8079 0.50000 0.05 0.54 0.75 H3A 0.82 C3 0.93 H3C 1.60 H3B Q8 1 0.0040 0.2506 0.1176 1.00000 0.05 0.54 0.86 H4B 1.63 C4 1.81 H4C 1.81 H2B Q9 1 0.2643 0.2357 0.8938 0.50000 0.05 0.51 1.04 H3A 1.13 H3C 1.16 C3 1.58 H3B Q10 1 0.1767 0.2282 0.3891 1.00000 0.05 0.46 1.00 SN1 1.40 C4 1.70 H4C 1.96 H4B Q11 1 0.2470 -0.0009 0.1797 1.00000 0.05 0.46 1.59 H2B 1.59 H2A 1.61 H4A 2.00 H3B Q12 1 -0.0508 0.2356 0.0174 1.00000 0.05 0.44 1.56 H4B 1.66 H2B 1.66 H2A 1.81 H3A Q13 1 0.4126 0.0874 0.0344 0.50000 0.05 0.43 0.88 H2A 0.88 H2B 0.88 H2A 0.88 H2B Q14 1 0.0164 0.2643 0.4408 1.00000 0.05 0.40 1.27 H4C 1.89 C4 2.14 H4B 2.40 C1 Q15 1 0.1413 0.1836 0.0915 1.00000 0.05 0.39 0.81 H4B 1.10 C4 1.33 H4A 2.03 H4C Q16 1 0.2507 0.0273 0.0126 1.00000 0.05 0.37 1.42 H2B 1.42 H2A 1.49 H4B 1.90 H4A Q17 1 0.2623 0.1427 0.1626 1.00000 0.05 0.36 1.71 H4A 1.71 SN1 1.79 C4 1.94 H2A Q18 1 0.1212 0.2728 0.0842 1.00000 0.05 0.36 0.81 H4B 1.59 C4 2.07 H2A 2.07 H2B Q19 1 0.0132 0.2267 0.0582 1.00000 0.05 0.36 0.83 H4B 1.68 C4 1.83 H2B 1.83 H2A Q20 1 0.0172 0.2531 0.5582 1.00000 0.05 0.35 1.67 H4C 2.12 H3B 2.13 C1 2.32 H3B Shortest distances between peaks (including symmetry equivalents) 12 16 0.35 8 19 0.47 5 16 0.56 7 9 0.63 16 19 0.67 12 19 0.73 14 20 0.76 5 19 0.77 5 11 0.82 8 12 0.88 5 12 0.89 8 16 0.90 15 18 0.97 6 8 1.03 6 14 1.08 11 16 1.11 5 8 1.11 2 17 1.12 1 10 1.22 18 19 1.26 8 18 1.28 2 10 1.29 11 12 1.38 5 18 1.42 17 17 1.42 10 10 1.43 15 17 1.43 15 19 1.45 6 19 1.46 12 17 1.53 11 17 1.54 11 19 1.54 16 17 1.56 18 18 1.59 8 15 1.63 3 4 1.67 1 2 1.67 11 20 1.69 16 18 1.71 5 15 1.75 6 12 1.75 10 14 1.77 2 15 1.81 6 20 1.82 6 18 1.83 13 16 1.84 5 17 1.85 12 15 1.86 6 16 1.87 1 7 1.88 13 17 1.89 9 15 1.90 8 11 1.90 12 18 1.91 10 17 1.93 12 13 1.94 9 17 1.98 9 18 1.98 2 18 1.99 10 15 2.00 10 20 2.02 15 16 2.04 5 13 2.06 9 12 2.06 8 14 2.08 15 16 2.08 10 18 2.09 6 10 2.09 17 18 2.10 6 15 2.13 11 18 2.13 7 12 2.14 5 6 2.14 12 15 2.16 11 13 2.20 8 13 2.20 17 19 2.21 15 18 2.26 6 7 2.30 13 19 2.32 11 15 2.32 9 16 2.34 2 9 2.35 8 17 2.38 11 15 2.38 1 9 2.39 7 15 2.39 9 13 2.40 7 8 2.40 7 13 2.40 10 17 2.40 15 17 2.40 7 17 2.41 7 16 2.41 11 14 2.44 5 15 2.45 17 20 2.46 15 19 2.47 5 20 2.47 14 19 2.48 1 17 2.51 2 11 2.51 8 10 2.54 14 18 2.54 8 9 2.55 7 18 2.55 3 6 2.56 10 18 2.58 2 13 2.58 17 18 2.58 1 20 2.58 3 14 2.59 13 13 2.62 5 9 2.62 2 12 2.63 15 15 2.63 12 17 2.63 1 14 2.64 4 20 2.64 7 19 2.64 8 15 2.66 6 9 2.67 2 16 2.68 16 17 2.68 4 13 2.68 9 19 2.69 6 13 2.69 4 14 2.70 3 13 2.72 12 18 2.73 14 15 2.73 10 19 2.74 8 18 2.74 1 14 2.74 5 18 2.74 10 20 2.74 13 18 2.77 10 15 2.78 1 20 2.78 16 20 2.79 18 19 2.79 11 17 2.79 10 14 2.80 1 6 2.81 12 14 2.82 8 20 2.82 9 11 2.83 9 19 2.86 17 19 2.87 2 20 2.87 10 11 2.87 5 9 2.90 2 7 2.90 7 10 2.92 6 11 2.92 7 14 2.93 14 16 2.94 2 6 2.95 2 14 2.95 2 5 2.96 10 14 2.96 5 7 2.97 5 7 2.97 2 8 2.97 3 20 2.98 16 18 2.98 8 17 2.98 3 8 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.42: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.33: Structure factors and derivatives 0.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:27:56 Total CPU time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++