+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 09:54:33 on 10-Mar-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pbcn CELL 0.71073 17.3346 12.8284 23.1071 90.000 90.000 90.000 ZERR 4.00 0.0025 0.0023 0.0043 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O CL MN UNIT 176 144 64 64 16 8 V = 5138.45 F(000) = 2632.0 Mu = 0.79 mm-1 Cell Wt = 5186.27 Rho = 1.676 MERG 2 OMIT -3.00 55.00 OMIT 2 0 16 OMIT 0 0 16 OMIT 0 0 12 SHEL 7 0.77 ACTA EQIV $1 -x-1/2, y+1/2, z EQIV $2 -x, y, -z+1/2 EQIV $3 x+1/2, y+1/2, -z+1/2 HTAB N3 O13_$1 HTAB N3 O11 HTAB N6 O1_$2 HTAB N6 O3_$3 FMAP 2 PLAN 5 SIZE 0.06 0.16 0.20 BOND $H WGHT 0.05140 5.85590 L.S. 12 TEMP -153.00 FVAR 0.19819 MOLE 1 C1 1 0.106881 0.700030 0.455356 11.00000 0.02374 0.02820 = 0.02773 -0.00114 0.00103 -0.00316 AFIX 43 H1 2 0.113540 0.773121 0.451029 11.00000 -1.20000 AFIX 0 C2 1 0.144129 0.650491 0.500596 11.00000 0.02167 0.03867 = 0.02455 -0.00261 0.00110 -0.00080 AFIX 43 H2 2 0.174579 0.688919 0.527304 11.00000 -1.20000 AFIX 0 C3 1 0.135926 0.542888 0.506063 11.00000 0.02312 0.03646 = 0.02498 0.00247 -0.00173 0.00704 AFIX 43 H3 2 0.162246 0.506264 0.535845 11.00000 -1.20000 AFIX 0 C4 1 0.088997 0.490148 0.467588 11.00000 0.02508 0.02593 = 0.02490 0.00090 0.00020 0.00278 AFIX 43 H4 2 0.082154 0.416933 0.471017 11.00000 -1.20000 AFIX 0 C5 1 0.051726 0.545287 0.423645 11.00000 0.01729 0.02277 = 0.01631 0.00096 0.00491 0.00222 C6 1 -0.001939 0.495083 0.381467 11.00000 0.01755 0.01962 = 0.02139 0.00087 0.00259 0.00205 C7 1 -0.018867 0.388504 0.380318 11.00000 0.02316 0.02037 = 0.02587 0.00541 0.00273 -0.00001 AFIX 43 H7 2 0.004489 0.342458 0.407333 11.00000 -1.20000 AFIX 0 C8 1 -0.070118 0.350864 0.339303 11.00000 0.02433 0.01526 = 0.03402 0.00358 0.00071 -0.00289 AFIX 43 H8 2 -0.082089 0.278641 0.337930 11.00000 -1.20000 AFIX 0 C9 1 -0.103896 0.419317 0.300204 11.00000 0.02144 0.02206 = 0.02809 -0.00296 -0.00075 -0.00280 AFIX 43 H9 2 -0.139732 0.395059 0.272166 11.00000 -1.20000 AFIX 0 C10 1 -0.083944 0.524419 0.303105 11.00000 0.01862 0.01815 = 0.02286 0.00082 0.00302 0.00002 C11 1 -0.109767 0.605999 0.261243 11.00000 0.01449 0.01869 = 0.02299 -0.00063 0.00153 0.00137 C12 1 0.104557 0.863671 0.264587 11.00000 0.01615 0.02021 = 0.02119 -0.00045 -0.00255 -0.00081 C13 1 0.079478 0.941765 0.309182 11.00000 0.01699 0.01972 = 0.01992 0.00065 -0.00182 0.00103 C14 1 0.100930 1.046019 0.309588 11.00000 0.02377 0.02377 = 0.02621 -0.00090 0.00074 -0.00308 AFIX 43 H14 2 0.137885 1.072136 0.282915 11.00000 -1.20000 AFIX 0 C15 1 0.066619 1.110948 0.350256 11.00000 0.03373 0.01870 = 0.03349 -0.00486 0.00015 -0.00337 AFIX 43 H15 2 0.080195 1.182647 0.351697 11.00000 -1.20000 AFIX 0 C16 1 0.012872 1.071668 0.388583 11.00000 0.02437 0.02182 = 0.02929 -0.00479 0.00002 0.00014 AFIX 43 H16 2 -0.011927 1.116282 0.415615 11.00000 -1.20000 AFIX 0 C17 1 -0.004509 0.965428 0.387039 11.00000 0.01929 0.02009 = 0.02043 -0.00184 -0.00305 0.00165 C18 1 -0.060331 0.912881 0.426555 11.00000 0.01747 0.02136 = 0.01984 -0.00053 -0.00279 0.00145 C19 1 -0.098078 0.963296 0.471548 11.00000 0.02451 0.03036 = 0.02520 -0.00343 -0.00070 0.00299 AFIX 43 H19 2 -0.089120 1.035261 0.478539 11.00000 -1.20000 AFIX 0 C20 1 -0.149267 0.907613 0.506449 11.00000 0.02393 0.04385 = 0.02542 -0.00049 0.00475 0.00621 AFIX 43 H20 2 -0.175868 0.941109 0.537209 11.00000 -1.20000 AFIX 0 C21 1 -0.160550 0.802607 0.495391 11.00000 0.02240 0.04103 = 0.03093 0.00944 0.00365 -0.00076 AFIX 43 H21 2 -0.194358 0.762515 0.518877 11.00000 -1.20000 AFIX 0 C22 1 -0.121825 0.757135 0.449640 11.00000 0.02591 0.02783 = 0.02719 0.00743 0.00033 -0.00028 AFIX 43 H22 2 -0.130510 0.685342 0.441944 11.00000 -1.20000 AFIX 0 N1 3 0.061495 0.649416 0.417043 11.00000 0.01858 0.02378 = 0.02264 -0.00028 0.00162 -0.00127 N2 3 -0.033729 0.560434 0.343154 11.00000 0.01899 0.01858 = 0.01951 0.00109 0.00151 -0.00066 N3 3 -0.150670 0.579256 0.214439 11.00000 0.02716 0.01939 = 0.02344 0.00096 -0.00671 -0.00246 AFIX 93 H3A 2 -0.162581 0.626646 0.188395 11.00000 -1.20000 H3B 2 -0.165662 0.514277 0.209700 11.00000 -1.20000 AFIX 0 N4 3 -0.084915 0.700034 0.272178 11.00000 0.01969 0.01764 = 0.01847 0.00105 0.00009 0.00082 N5 3 0.085244 0.767038 0.276480 11.00000 0.01969 0.01952 = 0.01713 -0.00044 -0.00106 -0.00102 N6 3 0.138724 0.894887 0.215827 11.00000 0.02365 0.01957 = 0.01968 0.00043 0.00188 -0.00087 AFIX 93 H6A 2 0.149960 0.849210 0.188694 11.00000 -1.20000 H6B 2 0.150020 0.961151 0.210805 11.00000 -1.20000 AFIX 0 N7 3 0.028791 0.902384 0.347939 11.00000 0.01710 0.01746 = 0.02190 -0.00034 -0.00041 -0.00233 N8 3 -0.072308 0.809670 0.415380 11.00000 0.01881 0.02181 = 0.02382 0.00102 -0.00025 -0.00025 MN1 6 -0.002543 0.731770 0.344640 11.00000 0.02195 0.01637 = 0.01883 0.00027 0.00009 -0.00235 MOLE 2 O1 4 -0.248177 0.746278 0.349517 11.00000 0.03611 0.04583 = 0.06460 0.02035 0.00348 -0.01218 O2 4 -0.324604 0.657568 0.414818 11.00000 0.07525 0.03894 = 0.06062 -0.00126 0.03936 0.00271 O3 4 -0.333327 0.615522 0.318170 11.00000 0.09374 0.03854 = 0.07229 -0.01893 -0.05177 0.01383 O4 4 -0.222906 0.569032 0.370702 11.00000 0.04022 0.05457 = 0.06823 0.01479 0.00146 0.02316 CL1 5 -0.281092 0.646617 0.363021 11.00000 0.02271 0.02661 = 0.02784 -0.00321 0.00013 0.00205 MOLE 3 O11 4 -0.241322 0.384059 0.190548 11.00000 0.03311 0.04703 = 0.03727 -0.01786 0.00914 -0.01387 O12 4 -0.273422 0.384853 0.091726 11.00000 0.04995 0.04007 = 0.05265 0.00665 -0.02265 0.00009 O13 4 -0.253698 0.224836 0.139481 11.00000 0.03878 0.02810 = 0.04139 -0.00014 0.00879 -0.01099 O14 4 -0.148892 0.336797 0.121659 11.00000 0.02734 0.03357 = 0.05431 0.00566 0.01715 0.00097 CL11 5 -0.229647 0.332848 0.135731 11.00000 0.02030 0.02333 = 0.02620 -0.00166 0.00323 -0.00133 HKLF 4 Covalent radii and connectivity table for s93 in Pbcn C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 MN 1.370 C1 - N1 C2 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C8 C10 C10 - N2 C9 C11 C11 - N4 N3 C10 C12 - N5 N6 C13 C13 - N7 C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - N7 C16 C18 C18 - N8 C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C22 C20 C22 - N8 C21 N1 - C1 C5 Mn1 N2 - C6 C10 Mn1 N3 - C11 N4 - C11 N5_$2 Mn1 N5 - C12 N4_$2 Mn1 N6 - C12 N7 - C17 C13 Mn1 N8 - C22 C18 Mn1 Mn1 - N5 N4 N7 N2 N8 N1 O1 - Cl1 O2 - Cl1 O3 - Cl1 O4 - Cl1 Cl1 - O2 O4 O3 O1 O11 - Cl11 O12 - Cl11 O13 - Cl11 O14 - Cl11 Cl11 - O12 O14 O11 O13 Operators for generating equivalent atoms: $1 -x-1/2, y+1/2, z $2 -x, y, -z+1/2 $3 x+1/2, y+1/2, -z+1/2 h k l Fo^2 Sigma Why rejected 5 10 0 8.88 2.22 observed but should be systematically absent 14 9 0 9.01 2.25 observed but should be systematically absent 0 7 14 20.26 3.04 observed but should be systematically absent 0 7 14 10.43 2.09 observed but should be systematically absent 0 7 0 9.99 2.22 observed but should be systematically absent 3 6 0 50.38 3.91 observed but should be systematically absent 0 3 2 3.09 0.77 observed but should be systematically absent 19 0 0 66.63 7.85 observed but should be systematically absent 19 0 0 54.20 6.51 observed but should be systematically absent 17 0 17 13.29 3.07 observed but should be systematically absent 17 0 0 18.35 3.24 observed but should be systematically absent 15 0 5 4.34 1.08 observed but should be systematically absent 15 0 0 117.54 14.58 observed but should be systematically absent 15 0 0 89.37 16.16 observed but should be systematically absent 13 0 0 61.28 11.67 observed but should be systematically absent 13 0 0 45.18 7.53 observed but should be systematically absent 11 0 11 130.30 9.13 observed but should be systematically absent 11 0 11 142.08 10.43 observed but should be systematically absent 9 0 9 13.27 2.85 observed but should be systematically absent 9 0 9 16.25 2.32 observed but should be systematically absent 9 0 9 7.33 1.83 observed but should be systematically absent 9 0 9 24.16 2.31 observed but should be systematically absent 7 0 7 13.48 2.07 observed but should be systematically absent 7 0 7 19.38 2.28 observed but should be systematically absent 7 0 7 12.55 1.79 observed but should be systematically absent 7 0 7 12.57 2.29 observed but should be systematically absent 7 0 0 14.96 2.14 observed but should be systematically absent 7 0 0 18.78 3.96 observed but should be systematically absent 6 0 3 4.46 1.11 observed but should be systematically absent 5 0 5 6.92 0.87 observed but should be systematically absent 5 0 3 4.12 1.03 observed but should be systematically absent 5 0 0 4.97 1.00 observed but should be systematically absent 5 0 0 6.36 1.06 observed but should be systematically absent 3 0 3 4.24 1.06 observed but should be systematically absent 0 0 13 152.23 10.55 observed but should be systematically absent 0 0 13 135.98 10.27 observed but should be systematically absent 0 0 11 79.52 7.44 observed but should be systematically absent 0 0 11 69.24 6.13 observed but should be systematically absent 0 0 9 10.70 2.14 observed but should be systematically absent 0 0 7 29.13 4.32 observed but should be systematically absent 0 0 7 30.42 4.06 observed but should be systematically absent 0 0 5 10.14 2.03 observed but should be systematically absent 0 0 5 13.03 2.17 observed but should be systematically absent 0 0 21 39.36 6.06 observed but should be systematically absent 0 0 23 19.04 4.01 observed but should be systematically absent 0 0 23 66.36 11.42 observed but should be systematically absent 0 0 27 158.27 12.98 observed but should be systematically absent 1 0 7 3.85 0.96 observed but should be systematically absent 1 0 23 86.63 12.25 observed but should be systematically absent 2 0 13 18.46 3.26 observed but should be systematically absent ** etc. ** 40312 Reflections read, of which 2338 rejected -19 =< h =< 22, -16 =< k =< 12, -27 =< l =< 29, Max. 2-theta = 54.65 82 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 2 0 1157.86 12.27 7 132.12 7 3 0 241.26 3.04 8 16.83 6 4 0 55.20 0.82 7 4.97 3 5 0 124.41 2.08 6 13.98 9 5 0 206.03 2.40 7 16.21 4 6 0 241.70 2.72 6 24.37 12 6 0 60.39 0.94 6 14.75 14 6 0 28.33 1.00 4 7.15 5 7 0 722.87 9.44 5 98.86 4 8 0 454.04 5.57 5 71.23 5 9 0 124.62 2.72 5 20.27 11 9 0 1513.11 32.03 3 169.37 4 10 0 260.25 5.87 4 42.61 3 11 0 637.68 13.02 4 78.68 7 3 1 91.29 0.71 17 4.78 3 4 1 47.12 0.60 12 3.34 9 4 1 74.86 0.64 14 5.27 9 5 1 328.07 1.88 14 23.08 4 6 1 367.59 2.10 10 24.37 12 6 1 76.97 0.70 12 9.24 5 7 1 194.45 1.76 10 20.47 13 7 1 59.80 1.45 7 8.37 4 8 1 208.66 2.42 10 19.67 3 9 1 259.06 3.86 9 20.03 4 10 1 203.36 3.53 8 19.03 7 0 2 416.90 4.71 9 23.78 2 2 2 350.37 3.06 14 15.77 12 2 2 135.65 0.91 13 9.21 2 4 2 199.42 1.64 11 9.59 4 5 2 73.50 0.81 13 4.58 10 5 2 191.53 2.01 11 15.57 9 6 2 234.11 1.85 11 15.29 12 6 2 98.92 0.89 12 11.58 4 7 2 200.73 2.22 9 21.71 1 2 3 5380.73 45.12 10 453.29 3 3 3 196.97 1.06 13 14.08 9 3 3 135.24 0.84 14 6.21 5 4 3 223.59 1.05 14 12.58 10 4 3 85.79 0.77 13 5.52 6 5 3 367.60 1.98 14 19.14 9 5 3 386.75 3.38 11 25.66 10 5 3 53.23 0.79 11 4.98 2 6 3 8.39 0.39 12 3.20 4 6 3 229.28 2.36 14 12.51 9 6 3 139.52 1.85 11 11.85 5 7 3 252.74 1.11 12 20.98 13 7 3 84.17 2.11 6 13.25 3 8 3 187.12 2.43 11 12.43 0 0 4 6894.67 126.82 2 3153.85 2 1 4 1890.63 14.82 16 92.32 ** etc. ** 453 Inconsistent equivalents 5772 Unique reflections, of which 0 suppressed R(int) = 0.1823 R(sigma) = 0.0859 Friedel opposites merged Maximum memory for data reduction = 3277 / 57588 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 = 4238 / 472554 wR2 = 0.1422 before cycle 1 for 5772 data and 370 / 370 parameters GooF = S = 1.065; Restrained GooF = 1.065 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19844 0.00040 0.625 OSF Mean shift/esd = 0.067 Maximum = 0.625 for OSF Max. shift = 0.001 A for O1 Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 2 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.071 OSF Mean shift/esd = 0.023 Maximum = 0.105 for U22 Mn1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 3 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.003 OSF Mean shift/esd = 0.002 Maximum = -0.011 for z O1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 4 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.004 for U33 C22 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C22 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 5 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z O1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C22 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 6 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for O14 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 7 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for N3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 8 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for N8 Max. dU = 0.000 for O4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 9 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for O3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 10 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for O4 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 11 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for O3 Max. dU = 0.000 for O3 Least-squares cycle 12 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1422 before cycle 12 for 5772 data and 370 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.19847 0.00040 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y Mn1 Max. shift = 0.000 A for O4 Max. dU = 0.000 for O12 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1135 0.7731 0.4511 43 0.950 0.000 C1 N1 C2 H2 0.1745 0.6889 0.5273 43 0.950 0.000 C2 C1 C3 H3 0.1622 0.5063 0.5359 43 0.950 0.000 C3 C4 C2 H4 0.0821 0.4169 0.4710 43 0.950 0.000 C4 C3 C5 H7 0.0045 0.3425 0.4073 43 0.950 0.000 C7 C8 C6 H8 -0.0821 0.2787 0.3380 43 0.950 0.000 C8 C7 C9 H9 -0.1397 0.3950 0.2722 43 0.950 0.000 C9 C8 C10 H14 0.1379 1.0721 0.2829 43 0.950 0.000 C14 C13 C15 H15 0.0802 1.1826 0.3517 43 0.950 0.000 C15 C16 C14 H16 -0.0120 1.1163 0.4156 43 0.950 0.000 C16 C15 C17 H19 -0.0891 1.0352 0.4785 43 0.950 0.000 C19 C18 C20 H20 -0.1759 0.9412 0.5372 43 0.950 0.000 C20 C21 C19 H21 -0.1944 0.7625 0.5189 43 0.950 0.000 C21 C22 C20 H22 -0.1305 0.6854 0.4420 43 0.950 0.000 C22 N8 C21 H3A -0.1625 0.6267 0.1884 93 0.880 0.000 N3 C11 N4 H3B -0.1657 0.5143 0.2097 93 0.880 0.000 N3 C11 N4 H6A 0.1499 0.8492 0.1887 93 0.880 0.000 N6 C12 N5 H6B 0.1500 0.9611 0.2108 93 0.880 0.000 N6 C12 N5 s93 in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10688 0.69998 0.45539 1.00000 0.02372 0.02834 0.02764 -0.00116 0.00109 -0.00321 0.02657 0.00522 0.00016 0.00024 0.00014 0.00000 0.00131 0.00153 0.00179 0.00127 0.00123 0.00119 0.00064 H1 0.11354 0.77307 0.45108 1.00000 0.03188 0.00000 0.00000 C2 0.14409 0.65047 0.50059 1.00000 0.02157 0.03874 0.02454 -0.00289 0.00108 -0.00100 0.02829 0.00545 0.00016 0.00025 0.00014 0.00000 0.00131 0.00177 0.00179 0.00131 0.00121 0.00124 0.00067 H2 0.17453 0.68891 0.52730 1.00000 0.03394 0.00000 0.00000 C3 0.13591 0.54287 0.50607 1.00000 0.02307 0.03655 0.02483 0.00248 -0.00174 0.00713 0.02815 0.00546 0.00016 0.00025 0.00014 0.00000 0.00133 0.00172 0.00175 0.00129 0.00123 0.00125 0.00066 H3 0.16222 0.50625 0.53586 1.00000 0.03378 0.00000 0.00000 C4 0.08897 0.49013 0.46758 1.00000 0.02516 0.02605 0.02466 0.00081 0.00001 0.00269 0.02529 0.00517 0.00015 0.00023 0.00014 0.00000 0.00134 0.00148 0.00169 0.00118 0.00119 0.00114 0.00062 H4 0.08212 0.41692 0.47100 1.00000 0.03035 0.00000 0.00000 C5 0.05173 0.54527 0.42365 1.00000 0.01708 0.02314 0.01618 0.00086 0.00502 0.00227 0.01880 0.00476 0.00014 0.00021 0.00012 0.00000 0.00114 0.00137 0.00145 0.00107 0.00104 0.00103 0.00055 C6 -0.00193 0.49509 0.38147 1.00000 0.01728 0.01985 0.02153 0.00075 0.00256 0.00195 0.01955 0.00493 0.00015 0.00021 0.00013 0.00000 0.00113 0.00131 0.00161 0.00107 0.00106 0.00101 0.00057 C7 -0.01886 0.38855 0.38029 1.00000 0.02296 0.02060 0.02556 0.00541 0.00272 0.00013 0.02304 0.00508 0.00015 0.00022 0.00013 0.00000 0.00126 0.00138 0.00170 0.00115 0.00118 0.00109 0.00061 H7 0.00453 0.34249 0.40729 1.00000 0.02765 0.00000 0.00000 C8 -0.07012 0.35089 0.33931 1.00000 0.02433 0.01549 0.03420 0.00346 0.00055 -0.00272 0.02467 0.00513 0.00016 0.00021 0.00014 0.00000 0.00135 0.00133 0.00186 0.00115 0.00122 0.00108 0.00064 H8 -0.08211 0.27867 0.33796 1.00000 0.02961 0.00000 0.00000 C9 -0.10387 0.41929 0.30021 1.00000 0.02130 0.02209 0.02809 -0.00303 -0.00083 -0.00270 0.02383 0.00493 0.00016 0.00022 0.00013 0.00000 0.00126 0.00140 0.00170 0.00119 0.00119 0.00108 0.00061 H9 -0.13968 0.39502 0.27215 1.00000 0.02859 0.00000 0.00000 C10 -0.08394 0.52438 0.30311 1.00000 0.01829 0.01833 0.02283 0.00063 0.00308 0.00002 0.01982 0.00475 0.00014 0.00020 0.00013 0.00000 0.00118 0.00135 0.00157 0.00108 0.00109 0.00100 0.00057 C11 -0.10979 0.60594 0.26124 1.00000 0.01455 0.01875 0.02311 -0.00059 0.00163 0.00146 0.01880 0.00469 0.00014 0.00020 0.00013 0.00000 0.00114 0.00136 0.00153 0.00107 0.00105 0.00099 0.00056 C12 0.10457 0.86371 0.26459 1.00000 0.01610 0.02039 0.02114 -0.00031 -0.00269 -0.00069 0.01921 0.00463 0.00015 0.00021 0.00013 0.00000 0.00114 0.00141 0.00153 0.00106 0.00106 0.00101 0.00057 C13 0.07947 0.94175 0.30919 1.00000 0.01690 0.01998 0.01988 0.00071 -0.00182 0.00116 0.01892 0.00463 0.00014 0.00021 0.00012 0.00000 0.00116 0.00132 0.00153 0.00106 0.00106 0.00099 0.00056 C14 0.10091 1.04599 0.30958 1.00000 0.02356 0.02389 0.02625 -0.00084 0.00085 -0.00317 0.02457 0.00496 0.00016 0.00022 0.00014 0.00000 0.00131 0.00144 0.00171 0.00118 0.00119 0.00112 0.00062 H14 0.13786 1.07211 0.28290 1.00000 0.02948 0.00000 0.00000 C15 0.06659 1.11092 0.35025 1.00000 0.03343 0.01865 0.03382 -0.00475 0.00000 -0.00341 0.02863 0.00520 0.00017 0.00023 0.00014 0.00000 0.00155 0.00141 0.00192 0.00122 0.00135 0.00122 0.00068 H15 0.08018 1.18262 0.35169 1.00000 0.03436 0.00000 0.00000 C16 0.01282 1.07168 0.38856 1.00000 0.02433 0.02216 0.02908 -0.00490 -0.00010 0.00015 0.02519 0.00503 0.00015 0.00023 0.00014 0.00000 0.00133 0.00141 0.00182 0.00120 0.00122 0.00112 0.00064 H16 -0.01201 1.11631 0.41557 1.00000 0.03023 0.00000 0.00000 C17 -0.00450 0.96543 0.38703 1.00000 0.01898 0.02020 0.02056 -0.00177 -0.00301 0.00163 0.01991 0.00469 0.00014 0.00021 0.00013 0.00000 0.00117 0.00132 0.00160 0.00110 0.00106 0.00105 0.00058 C18 -0.06033 0.91290 0.42655 1.00000 0.01734 0.02166 0.01982 -0.00050 -0.00278 0.00152 0.01960 0.00465 0.00014 0.00021 0.00013 0.00000 0.00118 0.00138 0.00152 0.00108 0.00108 0.00101 0.00056 C19 -0.09807 0.96326 0.47155 1.00000 0.02437 0.03060 0.02535 -0.00352 -0.00075 0.00300 0.02677 0.00523 0.00016 0.00024 0.00014 0.00000 0.00133 0.00158 0.00173 0.00125 0.00123 0.00117 0.00064 H19 -0.08909 1.03522 0.47855 1.00000 0.03213 0.00000 0.00000 C20 -0.14926 0.90764 0.50644 1.00000 0.02370 0.04429 0.02524 -0.00055 0.00481 0.00630 0.03107 0.00566 0.00016 0.00026 0.00014 0.00000 0.00136 0.00192 0.00180 0.00138 0.00125 0.00129 0.00071 H20 -0.17586 0.94115 0.53719 1.00000 0.03729 0.00000 0.00000 C21 -0.16055 0.80260 0.49538 1.00000 0.02249 0.04091 0.03109 0.00931 0.00352 -0.00070 0.03149 0.00583 0.00016 0.00026 0.00015 0.00000 0.00136 0.00181 0.00194 0.00143 0.00128 0.00129 0.00072 H21 -0.19437 0.76250 0.51886 1.00000 0.03779 0.00000 0.00000 C22 -0.12184 0.75717 0.44966 1.00000 0.02583 0.02816 0.02710 0.00745 0.00039 -0.00034 0.02703 0.00554 0.00016 0.00024 0.00015 0.00000 0.00141 0.00156 0.00181 0.00124 0.00126 0.00116 0.00066 H22 -0.13053 0.68538 0.44197 1.00000 0.03244 0.00000 0.00000 N1 0.06149 0.64941 0.41706 1.00000 0.01845 0.02376 0.02255 -0.00039 0.00165 -0.00123 0.02159 0.00404 0.00012 0.00018 0.00011 0.00000 0.00106 0.00124 0.00140 0.00096 0.00094 0.00091 0.00051 N2 -0.03373 0.56043 0.34316 1.00000 0.01895 0.01866 0.01963 0.00103 0.00159 -0.00065 0.01908 0.00397 0.00012 0.00018 0.00010 0.00000 0.00104 0.00115 0.00131 0.00089 0.00093 0.00089 0.00049 N3 -0.15066 0.57928 0.21446 1.00000 0.02729 0.01942 0.02349 0.00092 -0.00675 -0.00250 0.02340 0.00397 0.00013 0.00018 0.00011 0.00000 0.00116 0.00117 0.00142 0.00095 0.00103 0.00096 0.00052 H3A -0.16254 0.62669 0.18842 1.00000 0.02808 0.00000 0.00000 H3B -0.16567 0.51431 0.20970 1.00000 0.02808 0.00000 0.00000 N4 -0.08491 0.70004 0.27217 1.00000 0.01954 0.01791 0.01844 0.00123 0.00015 0.00091 0.01863 0.00394 0.00012 0.00017 0.00011 0.00000 0.00105 0.00111 0.00130 0.00091 0.00094 0.00088 0.00048 N5 0.08523 0.76702 0.27646 1.00000 0.01961 0.01962 0.01726 -0.00051 -0.00113 -0.00089 0.01883 0.00389 0.00012 0.00017 0.00011 0.00000 0.00106 0.00115 0.00132 0.00091 0.00096 0.00086 0.00049 N6 0.13872 0.89488 0.21584 1.00000 0.02367 0.01955 0.01980 0.00054 0.00184 -0.00086 0.02101 0.00399 0.00012 0.00018 0.00011 0.00000 0.00109 0.00118 0.00132 0.00092 0.00097 0.00092 0.00050 H6A 0.14994 0.84920 0.18871 1.00000 0.02521 0.00000 0.00000 H6B 0.15004 0.96114 0.21081 1.00000 0.02521 0.00000 0.00000 N7 0.02878 0.90238 0.34794 1.00000 0.01696 0.01770 0.02176 -0.00034 -0.00050 -0.00231 0.01881 0.00385 0.00012 0.00017 0.00010 0.00000 0.00100 0.00115 0.00135 0.00088 0.00093 0.00087 0.00049 N8 -0.07232 0.80967 0.41539 1.00000 0.01881 0.02210 0.02359 0.00099 -0.00016 -0.00015 0.02150 0.00405 0.00012 0.00018 0.00011 0.00000 0.00105 0.00119 0.00142 0.00096 0.00094 0.00090 0.00051 Mn1 -0.00254 0.73176 0.34464 1.00000 0.02194 0.01646 0.01882 0.00026 0.00009 -0.00233 0.01907 0.00073 0.00002 0.00003 0.00002 0.00000 0.00022 0.00022 0.00027 0.00016 0.00017 0.00016 0.00014 O1 -0.24819 0.74625 0.34947 1.00000 0.03604 0.04567 0.06468 0.02021 0.00332 -0.01214 0.04880 0.00508 0.00014 0.00021 0.00014 0.00000 0.00126 0.00150 0.00209 0.00130 0.00127 0.00113 0.00073 O2 -0.32459 0.65752 0.41481 1.00000 0.07535 0.03932 0.06064 -0.00108 0.03964 0.00291 0.05844 0.00556 0.00017 0.00021 0.00013 0.00000 0.00190 0.00147 0.00216 0.00131 0.00160 0.00134 0.00085 O3 -0.33332 0.61551 0.31817 1.00000 0.09379 0.03857 0.07281 -0.01887 -0.05222 0.01371 0.06839 0.00455 0.00019 0.00021 0.00014 0.00000 0.00223 0.00153 0.00232 0.00147 0.00189 0.00152 0.00099 O4 -0.22294 0.56901 0.37071 1.00000 0.04026 0.05466 0.06838 0.01495 0.00173 0.02315 0.05443 0.00537 0.00014 0.00022 0.00013 0.00000 0.00134 0.00168 0.00221 0.00146 0.00133 0.00125 0.00078 Cl1 -0.28109 0.64661 0.36302 1.00000 0.02271 0.02674 0.02787 -0.00323 0.00011 0.00204 0.02577 0.00122 0.00004 0.00005 0.00003 0.00000 0.00032 0.00036 0.00043 0.00028 0.00028 0.00026 0.00018 O11 -0.24130 0.38407 0.19056 1.00000 0.03313 0.04753 0.03716 -0.01773 0.00927 -0.01398 0.03928 0.00378 0.00012 0.00019 0.00011 0.00000 0.00114 0.00143 0.00150 0.00113 0.00104 0.00105 0.00059 O12 -0.27345 0.38486 0.09174 1.00000 0.05005 0.04021 0.05271 0.00664 -0.02297 0.00003 0.04766 0.00431 0.00014 0.00020 0.00012 0.00000 0.00143 0.00140 0.00184 0.00123 0.00128 0.00116 0.00068 O13 -0.25367 0.22486 0.13951 1.00000 0.03878 0.02804 0.04156 -0.00010 0.00886 -0.01096 0.03613 0.00412 0.00013 0.00017 0.00011 0.00000 0.00120 0.00120 0.00155 0.00101 0.00109 0.00098 0.00056 O14 -0.14889 0.33680 0.12166 1.00000 0.02727 0.03370 0.05439 0.00583 0.01716 0.00092 0.03845 0.00443 0.00012 0.00018 0.00012 0.00000 0.00108 0.00122 0.00176 0.00111 0.00109 0.00095 0.00060 Cl11 -0.22964 0.33285 0.13574 1.00000 0.02036 0.02339 0.02622 -0.00169 0.00324 -0.00132 0.02332 0.00119 0.00004 0.00005 0.00003 0.00000 0.00031 0.00034 0.00042 0.00027 0.00027 0.00025 0.00017 Final Structure Factor Calculation for s93 in Pbcn Total number of l.s. parameters = 370 Maximum vector length = 511 Memory required = 3868 / 25039 wR2 = 0.1422 before cycle 13 for 5772 data and 0 / 370 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0514 * P )^2 + 5.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0548 for 4484 Fo > 4sig(Fo) and 0.0745 for all 5772 data wR2 = 0.1422, GooF = S = 1.066, Restrained GooF = 1.066 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0307 0.0269 0.0220 C1 0.0394 0.0242 0.0212 C2 0.0398 0.0258 0.0189 C3 0.0284 0.0247 0.0227 C4 0.0248 0.0201 0.0115 C5 0.0234 0.0197 0.0156 C6 0.0299 0.0225 0.0168 C7 0.0348 0.0251 0.0141 C8 0.0294 0.0239 0.0182 C9 0.0244 0.0183 0.0167 C10 0.0234 0.0192 0.0138 C11 0.0223 0.0205 0.0148 C12 0.0208 0.0203 0.0156 C13 0.0278 0.0253 0.0206 C14 0.0357 0.0336 0.0166 C15 0.0316 0.0243 0.0196 C16 0.0243 0.0188 0.0166 C17 0.0230 0.0205 0.0154 C18 0.0334 0.0241 0.0228 C19 0.0461 0.0286 0.0185 C20 0.0466 0.0277 0.0202 C21 0.0351 0.0259 0.0201 C22 0.0244 0.0227 0.0177 N1 0.0210 0.0194 0.0169 N2 0.0329 0.0195 0.0178 N3 0.0202 0.0189 0.0168 N4 0.0206 0.0193 0.0166 N5 0.0245 0.0201 0.0184 N6 0.0218 0.0197 0.0149 N7 0.0241 0.0216 0.0188 N8 0.0228 0.0188 0.0156 Mn1 0.0779 0.0463 0.0222 O1 0.1083 0.0399 0.0271 O2 0.1415 0.0379 0.0258 O3 0.0836 0.0578 0.0219 O4 0.0308 0.0250 0.0215 Cl1 0.0687 0.0257 0.0234 O11 0.0751 0.0412 0.0268 O12 0.0517 0.0366 0.0201 O13 0.0638 0.0328 0.0188 O14 0.0285 0.0226 0.0188 Cl11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.033 0.044 0.057 0.074 0.097 0.146 1.000 Number in group 598. 603. 576. 564. 571. 580. 560. 561. 584. 575. GooF 1.140 1.106 0.979 1.047 0.996 1.081 1.105 1.055 1.023 1.111 K 4.199 1.327 1.080 1.002 1.016 1.007 1.016 1.011 1.001 0.981 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.32 1.66 inf Number in group 582. 573. 590. 570. 575. 571. 579. 576. 578. 578. GooF 0.952 0.973 0.972 1.008 0.950 1.016 1.067 0.984 1.213 1.425 K 1.009 1.041 1.028 1.023 1.021 1.009 0.989 0.979 0.946 0.998 R1 0.142 0.132 0.119 0.096 0.076 0.068 0.057 0.055 0.059 0.047 Recommended weighting scheme: WGHT 0.0571 5.8026 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) 12 3 12 4372.31 2272.45 8.22 0.098 1.12 9 6 3 3541.98 862.48 7.87 0.060 1.41 3 6 9 2699.80 476.02 7.78 0.045 1.58 3 3 3 5000.33 1960.82 7.18 0.091 3.14 6 12 0 1635.92 622.66 6.35 0.051 1.00 9 6 9 638.17 162.89 5.94 0.026 1.25 1 2 26 388.85 0.96 5.56 0.002 0.88 16 1 1 366.72 6.24 5.53 0.005 1.08 4 2 8 84.35 1.15 5.10 0.002 2.25 2 2 29 329.95 24.15 5.05 0.010 0.79 19 0 4 970.94 3.11 4.92 0.004 0.90 9 3 9 309.31 71.65 4.82 0.017 1.45 7 1 3 152.22 44.30 4.52 0.014 2.32 14 0 14 14215.91 10050.63 4.38 0.206 0.99 1 7 3 1653.29 1118.15 4.32 0.069 1.77 9 3 3 3433.20 2352.34 4.27 0.100 1.71 6 0 8 13124.05 10043.51 4.20 0.206 2.04 7 2 7 217.02 78.44 4.19 0.018 1.89 6 1 6 1997.23 1408.12 4.18 0.077 2.27 7 7 14 186.58 26.76 4.11 0.011 1.10 7 7 0 1259.90 812.15 4.08 0.059 1.47 2 1 23 1440.93 174.77 4.07 0.027 0.99 9 9 3 187.54 52.96 3.99 0.015 1.13 12 6 18 559.49 23.60 3.92 0.010 0.88 6 9 6 1652.77 1115.89 3.79 0.069 1.21 1 1 15 6236.88 21477.72 3.76 0.301 1.52 16 0 0 1057.79 620.85 3.75 0.051 1.08 6 6 12 756.61 421.89 3.74 0.042 1.28 12 0 12 8566.68 946.24 3.72 0.063 1.16 19 3 1 1366.78 919.73 3.69 0.062 0.89 15 6 15 361.88 54.96 3.69 0.015 0.85 3 2 11 604.72 326.68 3.65 0.037 1.89 2 4 14 497.49 943.46 3.55 0.063 1.45 1 3 11 666.05 1044.92 3.54 0.066 1.87 0 4 14 2901.67 2073.05 3.53 0.094 1.47 20 0 2 178.06 2.32 3.52 0.003 0.86 6 1 2 496.75 309.73 3.51 0.036 2.74 8 3 10 61.73 188.08 3.48 0.028 1.48 2 1 27 204.70 12.02 3.43 0.007 0.85 5 1 24 210.02 48.72 3.40 0.014 0.93 4 1 6 564.34 843.81 3.39 0.060 2.81 1 2 7 8839.30 12395.44 3.36 0.229 2.89 6 0 4 2281.47 1734.92 3.34 0.086 2.58 5 1 9 425.10 243.00 3.33 0.032 2.04 3 3 11 491.82 781.31 3.33 0.057 1.79 1 1 17 4582.46 13073.72 3.23 0.235 1.35 4 4 8 5439.59 4072.04 3.22 0.131 1.92 6 4 0 1401.40 2023.38 3.21 0.092 2.15 1 4 7 105.99 36.11 3.20 0.012 2.28 7 6 5 105.12 28.70 3.08 0.011 1.53 Bond lengths and angles C1 - Distance Angles N1 1.3507 (0.0038) C2 1.3821 (0.0044) 123.15 (0.29) H1 0.9500 118.43 118.43 C1 - N1 C2 C2 - Distance Angles C1 1.3821 (0.0044) C3 1.3934 (0.0045) 118.45 (0.30) H2 0.9500 120.78 120.78 C2 - C1 C3 C3 - Distance Angles C4 1.3824 (0.0043) C2 1.3934 (0.0045) 119.09 (0.29) H3 0.9500 120.45 120.45 C3 - C4 C2 C4 - Distance Angles C3 1.3824 (0.0043) C5 1.3955 (0.0040) 119.49 (0.28) H4 0.9500 120.26 120.26 C4 - C3 C5 C5 - Distance Angles N1 1.3552 (0.0036) C4 1.3955 (0.0040) 121.58 (0.26) C6 1.4932 (0.0039) 115.43 (0.24) 122.98 (0.25) C5 - N1 C4 C6 - Distance Angles N2 1.3380 (0.0036) C7 1.3982 (0.0039) 120.86 (0.27) C5 1.4932 (0.0039) 114.74 (0.24) 124.39 (0.26) C6 - N2 C7 C7 - Distance Angles C8 1.3857 (0.0042) C6 1.3982 (0.0039) 119.26 (0.27) H7 0.9500 120.37 120.37 C7 - C8 C6 C8 - Distance Angles C7 1.3857 (0.0042) C9 1.3887 (0.0041) 119.64 (0.26) H8 0.9500 120.18 120.18 C8 - C7 C9 C9 - Distance Angles C8 1.3887 (0.0041) C10 1.3933 (0.0038) 118.40 (0.27) H9 0.9500 120.80 120.80 C9 - C8 C10 C10 - Distance Angles N2 1.3519 (0.0036) C9 1.3933 (0.0038) 121.57 (0.26) C11 1.4939 (0.0038) 113.38 (0.23) 124.90 (0.26) C10 - N2 C9 C11 - Distance Angles N4 1.3064 (0.0035) N3 1.3370 (0.0036) 124.59 (0.26) C10 1.4939 (0.0038) 115.02 (0.24) 120.22 (0.24) C11 - N4 N3 C12 - Distance Angles N5 1.3138 (0.0035) N6 1.3339 (0.0036) 124.94 (0.26) C13 1.5012 (0.0038) 114.35 (0.25) 120.55 (0.24) C12 - N5 N6 C13 - Distance Angles N7 1.3525 (0.0035) C14 1.3880 (0.0039) 121.96 (0.26) C12 1.5012 (0.0038) 113.19 (0.23) 124.71 (0.26) C13 - N7 C14 C14 - Distance Angles C13 1.3880 (0.0039) C15 1.3896 (0.0042) 117.86 (0.27) H14 0.9500 121.07 121.07 C14 - C13 C15 C15 - Distance Angles C16 1.3806 (0.0043) C14 1.3896 (0.0042) 120.28 (0.27) H15 0.9500 119.86 119.86 C15 - C16 C14 C16 - Distance Angles C15 1.3806 (0.0043) C17 1.3962 (0.0040) 119.01 (0.28) H16 0.9500 120.50 120.50 C16 - C15 C17 C17 - Distance Angles N7 1.3427 (0.0036) C16 1.3962 (0.0040) 120.84 (0.26) C18 1.4915 (0.0038) 114.74 (0.23) 124.42 (0.26) C17 - N7 C16 C18 - Distance Angles N8 1.3650 (0.0036) C19 1.3880 (0.0040) 121.42 (0.26) C17 1.4915 (0.0039) 114.93 (0.24) 123.65 (0.26) C18 - N8 C19 C19 - Distance Angles C18 1.3880 (0.0040) C20 1.3952 (0.0044) 119.64 (0.29) H19 0.9500 120.18 120.18 C19 - C18 C20 C20 - Distance Angles C21 1.3855 (0.0046) C19 1.3952 (0.0044) 118.73 (0.30) H20 0.9500 120.63 120.63 C20 - C21 C19 C21 - Distance Angles C22 1.3805 (0.0046) C20 1.3855 (0.0046) 118.88 (0.29) H21 0.9500 120.56 120.56 C21 - C22 C20 C22 - Distance Angles N8 1.3482 (0.0037) C21 1.3805 (0.0046) 123.24 (0.29) H22 0.9500 118.38 118.38 C22 - N8 C21 N1 - Distance Angles C1 1.3507 (0.0038) C5 1.3552 (0.0036) 118.19 (0.25) Mn1 2.2690 (0.0025) 123.02 (0.19) 118.74 (0.19) N1 - C1 C5 N2 - Distance Angles C6 1.3380 (0.0036) C10 1.3519 (0.0036) 120.26 (0.24) Mn1 2.2637 (0.0023) 119.99 (0.19) 119.75 (0.18) N2 - C6 C10 N3 - Distance Angles C11 1.3370 (0.0036) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.3064 (0.0035) N5_$2 1.4146 (0.0034) 113.98 (0.24) Mn1 2.2380 (0.0024) 121.55 (0.18) 119.11 (0.15) N4 - C11 N5_$2 N5 - Distance Angles C12 1.3138 (0.0035) N4_$2 1.4146 (0.0034) 114.12 (0.24) Mn1 2.2364 (0.0024) 120.77 (0.18) 115.73 (0.15) N5 - C12 N4_$2 N6 - Distance Angles C12 1.3339 (0.0036) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C17 1.3427 (0.0036) C13 1.3525 (0.0035) 119.98 (0.23) Mn1 2.2564 (0.0023) 120.24 (0.18) 119.75 (0.18) N7 - C17 C13 N8 - Distance Angles C22 1.3482 (0.0037) C18 1.3650 (0.0036) 118.07 (0.26) Mn1 2.2660 (0.0025) 122.91 (0.20) 118.88 (0.18) N8 - C22 C18 Mn1 - Distance Angles N5 2.2364 (0.0024) N4 2.2380 (0.0024) 86.78 (0.09) N7 2.2564 (0.0023) 70.36 (0.08) 110.81 (0.08) N2 2.2637 (0.0023) 110.37 (0.08) 70.11 (0.08) 178.92 (0.09) N8 2.2660 (0.0025) 141.46 (0.08) 106.23 (0.08) 71.11 (0.08) 108.16 (0.08) N1 2.2690 (0.0025) 106.31 (0.08) 141.19 (0.08) 108.00 (0.08) 71.09 (0.08) 86.24 (0.09) Mn1 - N5 N4 N7 N2 N8 O1 - Distance Angles Cl1 1.4342 (0.0026) O1 - O2 - Distance Angles Cl1 1.4215 (0.0027) O2 - O3 - Distance Angles Cl1 1.4328 (0.0027) O3 - O4 - Distance Angles Cl1 1.4279 (0.0024) O4 - Cl1 - Distance Angles O2 1.4215 (0.0027) O4 1.4279 (0.0024) 109.78 (0.18) O3 1.4328 (0.0027) 107.53 (0.21) 109.99 (0.17) O1 1.4342 (0.0026) 107.89 (0.17) 111.57 (0.17) 109.97 (0.18) Cl1 - O2 O4 O3 O11 - Distance Angles Cl11 1.4414 (0.0024) O11 - O12 - Distance Angles Cl11 1.4336 (0.0025) O12 - O13 - Distance Angles Cl11 1.4491 (0.0022) O13 - O14 - Distance Angles Cl11 1.4381 (0.0021) O14 - Cl11 - Distance Angles O12 1.4336 (0.0025) O14 1.4381 (0.0021) 109.81 (0.16) O11 1.4414 (0.0024) 109.68 (0.16) 108.61 (0.14) O13 1.4491 (0.0022) 109.59 (0.15) 109.09 (0.14) 110.04 (0.15) Cl11 - O12 O14 O11 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.23 3.039(3) 152.8 N3-H3A...O13_$1 0.88 2.17 3.007(3) 159.0 N3-H3B...O11 0.88 2.33 3.084(3) 144.0 N6-H6A...O1_$2 0.88 2.11 2.977(4) 168.2 N6-H6B...O3_$3 FMAP and GRID set by program FMAP 2 1 21 GRID -1.389 -2 -1 1.389 2 1 R1 = 0.0732 for 5772 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.67 at 0.0015 0.7159 0.1187 [ 0.87 A from MN1 ] Deepest hole -0.55 at 0.2226 0.3546 0.3673 [ 0.31 A from CL11 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4276 / 40566 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0015 0.7159 0.3813 1.00000 0.05 0.67 0.87 MN1 1.61 N1 1.89 N8 2.25 N2 Q2 1 0.0396 0.6802 0.3792 1.00000 0.05 0.60 1.03 N1 1.27 MN1 2.02 C5 2.13 C1 Q3 1 -0.0050 0.7303 0.3063 1.00000 0.05 0.59 0.89 MN1 1.64 N4 1.77 N5 2.39 N2 Q4 1 0.0390 0.7499 0.3093 1.00000 0.05 0.58 1.11 MN1 1.13 N5 2.12 C12 2.14 N4 Q5 1 -0.0424 0.6720 0.3106 1.00000 0.05 0.58 1.21 N4 1.30 MN1 1.62 N2 1.84 C11 Shortest distances between peaks (including symmetry equivalents) 3 4 0.80 1 2 0.85 3 5 1.00 4 5 1.73 1 3 1.75 2 4 1.84 1 4 1.86 1 5 1.87 2 3 1.96 2 5 2.13 3 3 2.61 3 4 2.75 3 5 2.92 4 5 2.95 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 2.95: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 16.00: Structure factors and derivatives 24.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 2.78: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 09:55:24 Total CPU time: 46.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++