+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 09:09:53 on 09-Mar-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in Pbcn CELL 0.71073 17.6476 12.6089 22.9854 90.000 90.000 90.000 ZERR 4.00 0.0031 0.0018 0.0040 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 ZN UNIT 176 144 64 64 16 8 V = 5114.64 F(000) = 2672.0 Mu = 1.24 mm-1 Cell Wt = 5269.71 Rho = 1.711 MERG 2 OMIT -3.00 55.00 OMIT 3 6 9 SHEL 7 0.77 FMAP 2 PLAN 10 EQIV $1 X-1/2, Y-1/2, -Z+1/2 EQIV $2 -X, Y-1, -Z+1/2 EQIV $3 -X+1/2, Y-1/2, Z HTAB N3 O4_$1 HTAB N3 O3_$2 HTAB N6 O14_$3 HTAB N6 O11 SIZE 0.2 0.2 0.1 ACTA BOND $H WGHT 0.03840 6.85520 L.S. 9 TEMP -153.00 FVAR 0.22413 MOLE 1 C1 1 0.106136 0.214718 0.451784 11.00000 0.02337 0.02389 = 0.02179 -0.00130 0.00142 -0.00282 AFIX 43 H1 2 0.111400 0.288769 0.445320 11.00000 -1.20000 AFIX 0 C2 1 0.143771 0.169760 0.498516 11.00000 0.02152 0.03539 = 0.02148 -0.00431 0.00063 -0.00277 AFIX 43 H2 2 0.172491 0.212508 0.524441 11.00000 -1.20000 AFIX 0 C3 1 0.138676 0.060972 0.506707 11.00000 0.02474 0.03476 = 0.02033 0.00328 -0.00218 0.00494 AFIX 43 H3 2 0.165437 0.027587 0.537540 11.00000 -1.20000 AFIX 0 C4 1 0.093876 0.001541 0.469172 11.00000 0.02493 0.02462 = 0.01992 0.00196 0.00014 0.00078 AFIX 43 H4 2 0.089669 -0.073063 0.473958 11.00000 -1.20000 AFIX 0 C5 1 0.055143 0.052880 0.424352 11.00000 0.01856 0.02149 = 0.01695 0.00069 0.00450 0.00144 C6 1 0.002239 -0.003143 0.384396 11.00000 0.01753 0.02199 = 0.01642 0.00050 0.00268 0.00215 C7 1 -0.013667 -0.112251 0.385955 11.00000 0.02041 0.02060 = 0.02570 0.00493 0.00336 0.00235 AFIX 43 H7 2 0.010337 -0.156925 0.413668 11.00000 -1.20000 AFIX 0 C8 1 -0.064796 -0.153434 0.346511 11.00000 0.02174 0.01824 = 0.03033 0.00298 0.00021 -0.00153 AFIX 43 H8 2 -0.076086 -0.227096 0.347025 11.00000 -1.20000 AFIX 0 C9 1 -0.099948 -0.087691 0.305956 11.00000 0.02206 0.01956 = 0.02587 -0.00186 0.00065 -0.00340 AFIX 43 H9 2 -0.135937 -0.114941 0.279100 11.00000 -1.20000 AFIX 0 C10 1 -0.080505 0.019376 0.306147 11.00000 0.01658 0.02149 = 0.01804 0.00027 0.00194 0.00041 C11 1 -0.107134 0.099692 0.263082 11.00000 0.01659 0.02100 = 0.01668 -0.00005 0.00229 0.00062 C12 1 0.100931 0.359016 0.268424 11.00000 0.01448 0.01982 = 0.01678 0.00080 -0.00033 -0.00030 C13 1 0.074935 0.435151 0.314412 11.00000 0.01752 0.02060 = 0.01441 0.00120 -0.00206 0.00005 C14 1 0.097273 0.540448 0.318839 11.00000 0.02426 0.02217 = 0.02140 0.00068 -0.00174 -0.00284 AFIX 43 H14 2 0.135402 0.568776 0.294146 11.00000 -1.20000 AFIX 0 C15 1 0.061786 0.603340 0.360832 11.00000 0.02954 0.01946 = 0.02699 -0.00308 -0.00091 -0.00328 AFIX 43 H15 2 0.075618 0.675772 0.364913 11.00000 -1.20000 AFIX 0 C16 1 0.006478 0.560349 0.396537 11.00000 0.02726 0.02178 = 0.02355 -0.00346 -0.00113 0.00041 AFIX 43 H16 2 -0.018987 0.603132 0.424378 11.00000 -1.20000 AFIX 0 C17 1 -0.011136 0.452500 0.390752 11.00000 0.02081 0.02020 = 0.01468 -0.00034 -0.00442 -0.00026 C18 1 -0.068310 0.394075 0.426692 11.00000 0.01989 0.02349 = 0.01609 0.00049 -0.00253 0.00129 C19 1 -0.107072 0.439817 0.473120 11.00000 0.02587 0.03108 = 0.02054 -0.00302 -0.00061 0.00076 AFIX 43 H19 2 -0.099391 0.512271 0.482800 11.00000 -1.20000 AFIX 0 C20 1 -0.157383 0.377577 0.505213 11.00000 0.02548 0.04016 = 0.01932 -0.00025 0.00315 0.00419 AFIX 43 H20 2 -0.184218 0.406920 0.537224 11.00000 -1.20000 AFIX 0 C21 1 -0.167603 0.272358 0.489689 11.00000 0.02207 0.03647 = 0.02331 0.00713 0.00182 -0.00103 AFIX 43 H21 2 -0.200740 0.227945 0.511307 11.00000 -1.20000 AFIX 0 C22 1 -0.128516 0.233170 0.441985 11.00000 0.02133 0.02570 = 0.02363 0.00305 -0.00300 -0.00064 AFIX 43 H22 2 -0.136949 0.161664 0.430687 11.00000 -1.20000 AFIX 0 N1 3 0.062412 0.158340 0.415065 11.00000 0.01831 0.02281 = 0.01900 -0.00001 0.00090 -0.00117 N2 3 -0.030866 0.059545 0.344776 11.00000 0.01881 0.01752 = 0.01648 0.00027 0.00034 -0.00100 N3 3 -0.147803 0.070543 0.216535 11.00000 0.02658 0.02064 = 0.02174 0.00237 -0.00509 -0.00331 AFIX 93 H3A 2 -0.158892 0.117368 0.189452 11.00000 -1.20000 H3B 2 -0.163427 0.004572 0.213044 11.00000 -1.20000 AFIX 0 N4 3 -0.081569 0.196019 0.271849 11.00000 0.01862 0.01882 = 0.01661 0.00148 -0.00056 0.00058 N5 3 0.081422 0.260430 0.277951 11.00000 0.01940 0.01959 = 0.01561 -0.00165 0.00015 -0.00116 N6 3 0.135399 0.394242 0.220274 11.00000 0.02332 0.01911 = 0.01932 -0.00017 0.00083 -0.00266 AFIX 93 H6A 2 0.146584 0.349765 0.192047 11.00000 -1.20000 H6B 2 0.146870 0.461874 0.216849 11.00000 -1.20000 AFIX 0 N7 3 0.023124 0.392763 0.350348 11.00000 0.01887 0.01875 = 0.01578 0.00150 -0.00190 -0.00052 N8 3 -0.079283 0.291557 0.410992 11.00000 0.01853 0.02267 = 0.01883 0.00170 -0.00121 -0.00109 ZN1 6 -0.004339 0.226639 0.343308 11.00000 0.02054 0.01603 = 0.01634 0.00021 0.00003 -0.00194 MOLE 2 O1 4 0.148969 0.833212 0.377211 11.00000 0.02312 0.03341 = 0.04064 -0.00302 0.00944 -0.00104 O2 4 0.271186 0.885700 0.405672 11.00000 0.03739 0.03753 = 0.05042 -0.00129 -0.01543 -0.00378 O3 4 0.239426 0.875297 0.306136 11.00000 0.03845 0.05269 = 0.03257 0.01895 0.01249 0.01703 O4 4 0.252456 0.718568 0.361667 11.00000 0.04070 0.02999 = 0.03613 0.00277 0.00602 0.01070 CL1 5 0.228176 0.827951 0.362631 11.00000 0.02090 0.02559 = 0.02460 0.00471 0.00415 0.00263 MOLE 3 O11 4 0.160224 0.619366 0.190465 11.00000 0.05766 0.03572 = 0.05089 0.01535 0.02793 0.00593 O12 4 0.269061 0.555445 0.142738 11.00000 0.04030 0.04295 = 0.05443 -0.00240 -0.00458 0.01883 O13 4 0.174730 0.644363 0.090555 11.00000 0.05314 0.03755 = 0.04110 0.00278 -0.02197 0.00198 O14 4 0.250456 0.739867 0.155094 11.00000 0.03637 0.04006 = 0.05079 -0.01125 0.00431 -0.01139 CL11 5 0.214422 0.639473 0.144794 11.00000 0.02234 0.02445 = 0.02561 0.00438 -0.00029 0.00121 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 ZN 1.330 C1 - N1 C2 C2 - C1 C3 C3 - C2 C4 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 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 - C20 C22 C22 - N8 C21 N1 - C1 C5 Zn1 N2 - C6 C10 Zn1 N3 - C11 N4 - C11 N5_$4 Zn1 N5 - C12 N4_$4 Zn1 N6 - C12 N7 - C17 C13 Zn1 N8 - C22 C18 Zn1 Zn1 - N7 N2 N4 N5 N8 N1 O1 - Cl1 O2 - Cl1 O3 - Cl1 O4 - Cl1 Cl1 - O1 O3 O2 O4 O11 - Cl11 O12 - Cl11 O13 - Cl11 O14 - Cl11 Cl11 - O13 O12 O14 O11 Operators for generating equivalent atoms: $1 x-1/2, y-1/2, -z+1/2 $2 -x, y-1, -z+1/2 $3 -x+1/2, y-1/2, z $4 -x, y, -z+1/2 h k l Fo^2 Sigma Why rejected 0 7 0 20.76 4.45 observed but should be systematically absent 1 6 0 6.33 1.58 observed but should be systematically absent 0 5 2 6.52 1.63 observed but should be systematically absent 0 5 0 7.82 1.56 observed but should be systematically absent 0 3 2 10.20 1.46 observed but should be systematically absent 0 3 1 5.89 1.47 observed but should be systematically absent 22 1 0 30.61 7.65 observed but should be systematically absent 0 1 3 6.21 1.55 observed but should be systematically absent 15 0 15 25.19 5.93 observed but should be systematically absent 15 0 15 57.62 9.88 observed but should be systematically absent 15 0 0 89.44 15.16 observed but should be systematically absent 13 0 13 107.02 10.41 observed but should be systematically absent 13 0 13 37.67 8.19 observed but should be systematically absent 13 0 0 292.21 29.23 observed but should be systematically absent 13 0 0 58.51 12.00 observed but should be systematically absent 11 0 11 111.46 10.55 observed but should be systematically absent 11 0 11 40.86 6.29 observed but should be systematically absent 11 0 11 93.08 6.11 observed but should be systematically absent 11 0 11 48.90 9.78 observed but should be systematically absent 9 0 9 24.52 4.60 observed but should be systematically absent 9 0 9 18.66 3.11 observed but should be systematically absent 9 0 9 18.66 1.56 observed but should be systematically absent 9 0 0 72.11 16.77 observed but should be systematically absent 7 0 7 15.57 3.11 observed but should be systematically absent 7 0 7 13.86 1.54 observed but should be systematically absent 7 0 7 16.19 3.24 observed but should be systematically absent 6 0 23 80.92 19.85 observed but should be systematically absent 6 0 23 76.83 18.44 observed but should be systematically absent 5 0 5 13.92 3.09 observed but should be systematically absent 5 0 0 8.59 1.72 observed but should be systematically absent 5 0 0 8.43 1.41 observed but should be systematically absent 4 0 23 61.69 13.88 observed but should be systematically absent 4 0 23 82.94 13.83 observed but should be systematically absent 4 0 21 86.23 16.94 observed but should be systematically absent 4 0 21 134.58 21.41 observed but should be systematically absent 4 0 17 82.13 19.77 observed but should be systematically absent 2 0 29 50.10 10.96 observed but should be systematically absent 2 0 27 213.37 21.82 observed but should be systematically absent 2 0 27 162.05 20.27 observed but should be systematically absent 2 0 23 258.68 23.26 observed but should be systematically absent 2 0 23 297.45 29.30 observed but should be systematically absent 2 0 19 52.24 9.22 observed but should be systematically absent 1 0 25 24.85 6.21 observed but should be systematically absent 1 0 23 41.83 9.30 observed but should be systematically absent 1 0 23 29.35 6.18 observed but should be systematically absent 0 0 27 173.34 18.75 observed but should be systematically absent 0 0 25 90.19 12.45 observed but should be systematically absent 0 0 21 224.69 20.02 observed but should be systematically absent 0 0 13 108.31 13.55 observed but should be systematically absent 0 0 11 99.69 12.09 observed but should be systematically absent ** etc. ** 42641 Reflections read, of which 2457 rejected -22 =< h =< 21, -16 =< k =< 16, -29 =< l =< 29, Max. 2-theta = 54.60 89 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 9 2 165.69 1.40 12 9.31 1 1 3 13.76 0.52 8 2.87 7 2 3 13.81 0.51 13 4.65 3 10 8 323.13 1.48 12 20.94 6 6 11 467.99 1.51 11 35.96 1 1 12 25.02 1.17 8 11.72 6 8 15 59.12 1.21 8 6.43 1 1 16 57.01 2.37 7 23.88 2 2 17 42.68 1.87 9 12.12 5 1 22 29.66 1.99 6 14.17 10 Inconsistent equivalents 5740 Unique reflections, of which 0 suppressed R(int) = 0.0799 R(sigma) = 0.0403 Friedel opposites merged Maximum memory for data reduction = 3271 / 57330 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 = 0.1018 before cycle 1 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 -0.003 OSF Mean shift/esd = 0.004 Maximum = 0.025 for U23 Zn1 Max. shift = 0.000 A for O12 Max. dU = 0.000 for O11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 2 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 -0.003 OSF Mean shift/esd = 0.002 Maximum = 0.009 for U23 Zn1 Max. shift = 0.000 A for O12 Max. dU = 0.000 for O11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 3 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U22 Zn1 Max. shift = 0.000 A for O12 Max. dU = 0.000 for C20 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 4 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N4 Max. dU = 0.000 for O12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 5 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl11 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 6 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl11 Max. shift = 0.000 A for O4 Max. dU = 0.000 for O12 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 7 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl11 Max. shift = 0.000 A for N2 Max. dU = 0.000 for C21 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 8 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl11 Max. shift = 0.000 A for H19 Max. dU = 0.000 for O11 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4238 / 472554 wR2 = 0.1018 before cycle 9 for 5740 data and 370 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22413 0.00032 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y Cl11 Max. shift = 0.000 A for C22 Max. dU = 0.000 for O11 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 H1 0.1114 0.2888 0.4453 43 0.950 0.000 C1 N1 C2 H2 0.1725 0.2125 0.5244 43 0.950 0.000 C2 C1 C3 H3 0.1654 0.0276 0.5375 43 0.950 0.000 C3 C2 C4 H4 0.0897 -0.0731 0.4740 43 0.950 0.000 C4 C3 C5 H7 0.0103 -0.1569 0.4137 43 0.950 0.000 C7 C8 C6 H8 -0.0761 -0.2271 0.3470 43 0.950 0.000 C8 C7 C9 H9 -0.1359 -0.1149 0.2791 43 0.950 0.000 C9 C10 C8 H14 0.1354 0.5688 0.2941 43 0.950 0.000 C14 C13 C15 H15 0.0756 0.6758 0.3649 43 0.950 0.000 C15 C16 C14 H16 -0.0190 0.6031 0.4244 43 0.950 0.000 C16 C15 C17 H19 -0.0994 0.5123 0.4828 43 0.950 0.000 C19 C18 C20 H20 -0.1842 0.4069 0.5372 43 0.950 0.000 C20 C21 C19 H21 -0.2007 0.2279 0.5113 43 0.950 0.000 C21 C20 C22 H22 -0.1369 0.1617 0.4307 43 0.950 0.000 C22 N8 C21 H3A -0.1589 0.1174 0.1895 93 0.880 0.000 N3 C11 N4 H3B -0.1634 0.0046 0.2130 93 0.880 0.000 N3 C11 N4 H6A 0.1466 0.3498 0.1920 93 0.880 0.000 N6 C12 N5 H6B 0.1469 0.4619 0.2168 93 0.880 0.000 N6 C12 N5 s93 in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10614 0.21472 0.45178 1.00000 0.02337 0.02388 0.02179 -0.00130 0.00142 -0.00283 0.02302 0.00451 0.00015 0.00021 0.00012 0.00000 0.00130 0.00126 0.00137 0.00105 0.00110 0.00104 0.00055 H1 0.11140 0.28877 0.44532 1.00000 0.02762 0.00000 0.00000 C2 0.14377 0.16976 0.49852 1.00000 0.02151 0.03540 0.02149 -0.00429 0.00063 -0.00277 0.02613 0.00474 0.00015 0.00022 0.00012 0.00000 0.00130 0.00151 0.00138 0.00114 0.00112 0.00112 0.00058 H2 0.17249 0.21251 0.52444 1.00000 0.03136 0.00000 0.00000 C3 0.13868 0.06097 0.50671 1.00000 0.02474 0.03477 0.02033 0.00329 -0.00218 0.00494 0.02661 0.00489 0.00015 0.00023 0.00012 0.00000 0.00135 0.00149 0.00138 0.00113 0.00114 0.00115 0.00058 H3 0.16544 0.02759 0.53754 1.00000 0.03194 0.00000 0.00000 C4 0.09388 0.00154 0.46917 1.00000 0.02493 0.02461 0.01992 0.00197 0.00013 0.00077 0.02316 0.00461 0.00015 0.00021 0.00011 0.00000 0.00131 0.00125 0.00135 0.00104 0.00109 0.00105 0.00054 H4 0.08967 -0.07306 0.47396 1.00000 0.02779 0.00000 0.00000 C5 0.05514 0.05288 0.42435 1.00000 0.01856 0.02148 0.01694 0.00068 0.00449 0.00144 0.01900 0.00438 0.00014 0.00019 0.00011 0.00000 0.00117 0.00119 0.00123 0.00097 0.00100 0.00097 0.00050 C6 0.00224 -0.00314 0.38439 1.00000 0.01754 0.02198 0.01642 0.00049 0.00268 0.00215 0.01865 0.00443 0.00014 0.00020 0.00011 0.00000 0.00116 0.00117 0.00123 0.00097 0.00100 0.00096 0.00050 C7 -0.01367 -0.11225 0.38596 1.00000 0.02041 0.02061 0.02571 0.00494 0.00336 0.00235 0.02224 0.00467 0.00014 0.00020 0.00012 0.00000 0.00126 0.00121 0.00142 0.00106 0.00108 0.00100 0.00055 H7 0.01034 -0.15692 0.41367 1.00000 0.02669 0.00000 0.00000 C8 -0.06480 -0.15343 0.34651 1.00000 0.02174 0.01823 0.03032 0.00297 0.00020 -0.00153 0.02343 0.00460 0.00015 0.00020 0.00012 0.00000 0.00129 0.00120 0.00150 0.00105 0.00112 0.00100 0.00056 H8 -0.07608 -0.22710 0.34702 1.00000 0.02811 0.00000 0.00000 C9 -0.09995 -0.08769 0.30596 1.00000 0.02205 0.01956 0.02587 -0.00186 0.00064 -0.00340 0.02249 0.00450 0.00015 0.00019 0.00012 0.00000 0.00130 0.00121 0.00143 0.00103 0.00109 0.00101 0.00055 H9 -0.13594 -0.11494 0.27910 1.00000 0.02699 0.00000 0.00000 C10 -0.08050 0.01938 0.30615 1.00000 0.01659 0.02150 0.01803 0.00027 0.00194 0.00041 0.01871 0.00426 0.00014 0.00019 0.00011 0.00000 0.00117 0.00121 0.00125 0.00097 0.00100 0.00094 0.00051 C11 -0.10713 0.09969 0.26308 1.00000 0.01659 0.02100 0.01668 -0.00005 0.00229 0.00061 0.01809 0.00432 0.00014 0.00019 0.00011 0.00000 0.00119 0.00118 0.00127 0.00095 0.00098 0.00096 0.00051 C12 0.10093 0.35901 0.26842 1.00000 0.01449 0.01981 0.01680 0.00079 -0.00033 -0.00031 0.01703 0.00419 0.00014 0.00019 0.00011 0.00000 0.00113 0.00116 0.00120 0.00095 0.00096 0.00094 0.00048 C13 0.07493 0.43515 0.31441 1.00000 0.01751 0.02061 0.01442 0.00120 -0.00206 0.00005 0.01751 0.00417 0.00014 0.00019 0.00011 0.00000 0.00118 0.00117 0.00119 0.00095 0.00097 0.00093 0.00049 C14 0.09727 0.54045 0.31884 1.00000 0.02426 0.02217 0.02142 0.00068 -0.00175 -0.00283 0.02262 0.00440 0.00015 0.00020 0.00012 0.00000 0.00132 0.00123 0.00136 0.00104 0.00109 0.00103 0.00054 H14 0.13540 0.56878 0.29415 1.00000 0.02714 0.00000 0.00000 C15 0.06178 0.60334 0.36083 1.00000 0.02955 0.01946 0.02698 -0.00309 -0.00090 -0.00328 0.02533 0.00461 0.00016 0.00020 0.00012 0.00000 0.00145 0.00122 0.00145 0.00107 0.00118 0.00106 0.00058 H15 0.07561 0.67577 0.36491 1.00000 0.03040 0.00000 0.00000 C16 0.00648 0.56035 0.39654 1.00000 0.02726 0.02177 0.02357 -0.00347 -0.00114 0.00040 0.02420 0.00456 0.00015 0.00021 0.00012 0.00000 0.00136 0.00123 0.00142 0.00107 0.00112 0.00106 0.00056 H16 -0.01898 0.60313 0.42438 1.00000 0.02904 0.00000 0.00000 C17 -0.01114 0.45250 0.39075 1.00000 0.02081 0.02018 0.01468 -0.00033 -0.00443 -0.00026 0.01856 0.00418 0.00014 0.00019 0.00011 0.00000 0.00121 0.00116 0.00121 0.00096 0.00099 0.00096 0.00050 C18 -0.06831 0.39407 0.42669 1.00000 0.01990 0.02348 0.01609 0.00048 -0.00253 0.00129 0.01982 0.00432 0.00014 0.00020 0.00011 0.00000 0.00124 0.00122 0.00124 0.00098 0.00101 0.00099 0.00051 C19 -0.10707 0.43982 0.47312 1.00000 0.02585 0.03109 0.02054 -0.00302 -0.00060 0.00075 0.02583 0.00472 0.00015 0.00023 0.00012 0.00000 0.00137 0.00140 0.00138 0.00111 0.00112 0.00114 0.00058 H19 -0.09939 0.51227 0.48280 1.00000 0.03099 0.00000 0.00000 C20 -0.15738 0.37758 0.50522 1.00000 0.02549 0.04015 0.01932 -0.00025 0.00314 0.00417 0.02832 0.00501 0.00016 0.00023 0.00012 0.00000 0.00141 0.00161 0.00141 0.00118 0.00113 0.00121 0.00061 H20 -0.18422 0.40692 0.53723 1.00000 0.03398 0.00000 0.00000 C21 -0.16760 0.27236 0.48969 1.00000 0.02207 0.03647 0.02331 0.00712 0.00182 -0.00103 0.02729 0.00497 0.00015 0.00023 0.00012 0.00000 0.00134 0.00156 0.00144 0.00117 0.00112 0.00113 0.00060 H21 -0.20074 0.22794 0.51131 1.00000 0.03274 0.00000 0.00000 C22 -0.12852 0.23317 0.44199 1.00000 0.02133 0.02570 0.02364 0.00304 -0.00300 -0.00064 0.02355 0.00465 0.00014 0.00021 0.00012 0.00000 0.00129 0.00134 0.00141 0.00106 0.00109 0.00104 0.00056 H22 -0.13695 0.16166 0.43069 1.00000 0.02826 0.00000 0.00000 N1 0.06241 0.15834 0.41506 1.00000 0.01831 0.02280 0.01901 -0.00001 0.00090 -0.00118 0.02004 0.00359 0.00012 0.00016 0.00009 0.00000 0.00103 0.00108 0.00110 0.00085 0.00087 0.00084 0.00045 N2 -0.03087 0.05955 0.34478 1.00000 0.01880 0.01752 0.01648 0.00027 0.00034 -0.00101 0.01760 0.00352 0.00012 0.00016 0.00009 0.00000 0.00102 0.00096 0.00106 0.00079 0.00085 0.00081 0.00042 N3 -0.14780 0.07054 0.21654 1.00000 0.02656 0.02064 0.02174 0.00236 -0.00509 -0.00331 0.02298 0.00365 0.00012 0.00017 0.00010 0.00000 0.00116 0.00104 0.00120 0.00087 0.00095 0.00091 0.00047 H3A -0.15889 0.11737 0.18945 1.00000 0.02758 0.00000 0.00000 H3B -0.16343 0.00457 0.21304 1.00000 0.02758 0.00000 0.00000 N4 -0.08157 0.19602 0.27185 1.00000 0.01863 0.01881 0.01662 0.00148 -0.00056 0.00058 0.01802 0.00356 0.00011 0.00016 0.00009 0.00000 0.00106 0.00100 0.00104 0.00083 0.00087 0.00081 0.00043 N5 0.08142 0.26043 0.27795 1.00000 0.01940 0.01959 0.01561 -0.00165 0.00016 -0.00116 0.01820 0.00349 0.00012 0.00016 0.00009 0.00000 0.00106 0.00102 0.00109 0.00082 0.00086 0.00081 0.00044 N6 0.13540 0.39424 0.22027 1.00000 0.02331 0.01912 0.01931 -0.00017 0.00083 -0.00266 0.02058 0.00362 0.00012 0.00016 0.00009 0.00000 0.00112 0.00103 0.00114 0.00084 0.00091 0.00086 0.00045 H6A 0.14658 0.34977 0.19205 1.00000 0.02470 0.00000 0.00000 H6B 0.14687 0.46187 0.21685 1.00000 0.02470 0.00000 0.00000 N7 0.02312 0.39276 0.35035 1.00000 0.01887 0.01876 0.01577 0.00151 -0.00190 -0.00051 0.01780 0.00357 0.00012 0.00016 0.00009 0.00000 0.00103 0.00099 0.00107 0.00081 0.00083 0.00082 0.00043 N8 -0.07928 0.29156 0.41099 1.00000 0.01854 0.02267 0.01883 0.00171 -0.00121 -0.00110 0.02001 0.00362 0.00012 0.00017 0.00009 0.00000 0.00103 0.00104 0.00109 0.00085 0.00088 0.00084 0.00045 Zn1 -0.00434 0.22664 0.34331 1.00000 0.02054 0.01603 0.01634 0.00021 0.00003 -0.00194 0.01763 0.00048 0.00002 0.00002 0.00001 0.00000 0.00016 0.00015 0.00016 0.00011 0.00012 0.00011 0.00009 O1 0.14897 0.83321 0.37721 1.00000 0.02311 0.03342 0.04063 -0.00302 0.00944 -0.00104 0.03239 0.00354 0.00011 0.00016 0.00009 0.00000 0.00099 0.00108 0.00126 0.00091 0.00091 0.00084 0.00047 O2 0.27119 0.88570 0.40567 1.00000 0.03739 0.03753 0.05042 -0.00129 -0.01543 -0.00377 0.04178 0.00365 0.00013 0.00017 0.00010 0.00000 0.00122 0.00118 0.00145 0.00103 0.00107 0.00098 0.00055 O3 0.23942 0.87529 0.30614 1.00000 0.03845 0.05267 0.03257 0.01896 0.01248 0.01702 0.04123 0.00442 0.00013 0.00018 0.00009 0.00000 0.00125 0.00135 0.00123 0.00101 0.00099 0.00105 0.00056 O4 0.25246 0.71857 0.36167 1.00000 0.04069 0.02999 0.03612 0.00276 0.00601 0.01072 0.03560 0.00392 0.00013 0.00016 0.00009 0.00000 0.00121 0.00109 0.00119 0.00089 0.00101 0.00092 0.00049 Cl1 0.22818 0.82795 0.36263 1.00000 0.02090 0.02559 0.02460 0.00471 0.00415 0.00263 0.02370 0.00115 0.00004 0.00005 0.00003 0.00000 0.00030 0.00031 0.00033 0.00025 0.00025 0.00024 0.00015 O11 0.16022 0.61937 0.19046 1.00000 0.05767 0.03573 0.05090 0.01535 0.02794 0.00594 0.04810 0.00474 0.00014 0.00018 0.00011 0.00000 0.00156 0.00121 0.00153 0.00107 0.00123 0.00110 0.00064 O12 0.26906 0.55544 0.14274 1.00000 0.04030 0.04295 0.05445 -0.00241 -0.00458 0.01884 0.04590 0.00428 0.00013 0.00019 0.00011 0.00000 0.00129 0.00129 0.00152 0.00111 0.00112 0.00107 0.00059 O13 0.17473 0.64436 0.09055 1.00000 0.05314 0.03754 0.04110 0.00277 -0.02197 0.00198 0.04393 0.00381 0.00014 0.00017 0.00010 0.00000 0.00143 0.00120 0.00134 0.00100 0.00114 0.00106 0.00058 O14 0.25046 0.73987 0.15509 1.00000 0.03637 0.04008 0.05077 -0.01126 0.00430 -0.01141 0.04241 0.00382 0.00013 0.00018 0.00010 0.00000 0.00121 0.00122 0.00146 0.00105 0.00109 0.00099 0.00056 Cl11 0.21442 0.63947 0.14479 1.00000 0.02233 0.02444 0.02561 0.00438 -0.00029 0.00121 0.02413 0.00113 0.00004 0.00005 0.00003 0.00000 0.00032 0.00030 0.00034 0.00025 0.00026 0.00024 0.00015 Final Structure Factor Calculation for s93 in Pbcn Total number of l.s. parameters = 370 Maximum vector length = 511 Memory required = 3868 / 25039 wR2 = 0.1018 before cycle 10 for 5740 data and 0 / 370 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 6.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 4698 Fo > 4sig(Fo) and 0.0552 for all 5740 data wR2 = 0.1018, GooF = S = 1.068, Restrained GooF = 1.068 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 0.0272 0.0212 0.0207 C1 0.0371 0.0210 0.0202 C2 0.0371 0.0249 0.0179 C3 0.0259 0.0243 0.0192 C4 0.0235 0.0203 0.0132 C5 0.0232 0.0186 0.0141 C6 0.0304 0.0188 0.0175 C7 0.0310 0.0222 0.0170 C8 0.0270 0.0235 0.0170 C9 0.0216 0.0193 0.0152 C10 0.0211 0.0189 0.0143 C11 0.0200 0.0166 0.0144 C12 0.0209 0.0184 0.0132 C13 0.0269 0.0210 0.0200 C14 0.0305 0.0281 0.0174 C15 0.0280 0.0255 0.0191 C16 0.0231 0.0202 0.0123 C17 0.0239 0.0208 0.0147 C18 0.0320 0.0258 0.0197 C19 0.0413 0.0259 0.0178 C20 0.0396 0.0234 0.0188 C21 0.0286 0.0230 0.0190 C22 0.0231 0.0195 0.0175 N1 0.0194 0.0172 0.0162 N2 0.0313 0.0192 0.0184 N3 0.0196 0.0187 0.0157 N4 0.0210 0.0186 0.0150 N5 0.0247 0.0192 0.0178 N6 0.0206 0.0183 0.0145 N7 0.0237 0.0189 0.0174 N8 0.0213 0.0164 0.0153 Zn1 0.0456 0.0326 0.0190 O1 0.0607 0.0388 0.0259 O2 0.0759 0.0271 0.0207 O3 0.0504 0.0331 0.0233 O4 0.0319 0.0210 0.0182 Cl1 0.0867 0.0366 0.0211 O11 0.0632 0.0518 0.0226 O12 0.0699 0.0384 0.0235 O13 0.0619 0.0395 0.0258 O14 0.0295 0.0228 0.0201 Cl11 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 0.050 0.066 0.086 0.111 0.145 0.212 1.000 Number in group 614. 564. 571. 573. 559. 566. 574. 579. 567. 573. GooF 1.143 1.160 1.138 1.055 1.082 0.974 0.976 1.000 1.102 1.027 K 2.910 1.446 1.092 1.053 1.021 1.005 0.997 1.008 1.005 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.66 inf Number in group 588. 568. 579. 560. 578. 573. 578. 564. 575. 577. GooF 1.062 1.065 0.999 1.034 0.947 1.011 0.901 0.889 1.087 1.539 K 1.015 1.044 1.029 1.035 1.020 1.002 0.993 0.991 0.986 1.024 R1 0.131 0.108 0.095 0.080 0.058 0.047 0.038 0.031 0.031 0.035 Recommended weighting scheme: WGHT 0.0386 6.8234 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) 9 6 3 798.43 83.50 6.15 0.023 1.41 3 3 3 5378.83 3396.70 6.10 0.150 3.12 19 0 4 923.92 195.60 5.75 0.036 0.92 1 2 22 689.98 0.05 5.51 0.001 1.03 22 1 5 384.23 0.96 5.25 0.003 0.79 2 4 10 295.41 642.55 5.15 0.065 1.82 2 1 23 732.65 50.70 4.59 0.018 0.99 14 3 19 477.92 69.27 4.58 0.021 0.85 4 4 8 4682.36 3552.86 4.47 0.153 1.91 12 0 12 6620.58 4145.06 4.45 0.165 1.17 12 6 18 326.50 24.89 4.38 0.013 0.88 4 2 8 601.47 334.68 4.34 0.047 2.25 0 0 28 934.24 70.82 4.31 0.022 0.82 3 3 7 2829.55 2094.46 4.30 0.118 2.37 1 1 18 2072.46 240.42 4.20 0.040 1.27 1 4 7 209.56 68.52 4.19 0.021 2.26 3 2 11 681.74 390.19 4.08 0.051 1.88 16 1 1 280.70 29.84 4.01 0.014 1.10 6 0 8 14101.70 11372.18 3.91 0.274 2.06 6 4 0 1822.18 2460.73 3.91 0.127 2.15 12 1 1 531.66 157.53 3.91 0.032 1.46 3 1 28 1020.33 510.27 3.88 0.058 0.81 6 1 2 304.27 148.86 3.84 0.031 2.78 3 1 22 736.22 360.14 3.82 0.049 1.03 6 2 4 510.43 287.70 3.78 0.044 2.42 1 1 28 2423.85 1693.38 3.72 0.106 0.82 9 3 3 3116.96 2409.87 3.48 0.126 1.73 7 2 7 233.61 102.96 3.48 0.026 1.91 9 3 9 200.73 62.59 3.47 0.020 1.46 0 2 21 1980.38 1243.13 3.45 0.091 1.08 4 4 7 130.54 37.60 3.44 0.016 2.02 10 14 7 166.69 535.72 3.43 0.059 0.78 1 4 2 72.60 0.18 3.41 0.001 3.00 10 3 2 1375.60 1825.28 3.39 0.110 1.61 9 9 3 108.77 7.73 3.39 0.007 1.13 19 8 7 -70.62 118.13 3.38 0.028 0.78 10 5 5 159.24 47.56 3.37 0.018 1.38 6 0 0 12592.96 10386.85 3.35 0.262 2.94 3 4 2 685.57 446.94 3.33 0.054 2.70 2 2 17 849.71 7.19 3.32 0.007 1.31 1 7 4 304.46 510.12 3.32 0.058 1.71 2 2 3 172.97 60.66 3.27 0.020 4.26 6 3 6 822.23 1161.69 3.25 0.088 2.04 12 3 12 2000.69 1444.48 3.21 0.098 1.12 0 6 0 30392.93 26135.86 3.21 0.415 2.10 1 3 28 812.83 455.74 3.18 0.055 0.80 3 1 20 238.92 3.77 3.17 0.005 1.12 6 4 6 4078.49 4921.95 3.14 0.180 1.88 8 1 2 55.22 4.53 3.11 0.005 2.14 2 3 25 188.13 0.44 3.11 0.002 0.89 Bond lengths and angles C1 - Distance Angles N1 1.3465 (0.0033) C2 1.3842 (0.0038) 123.04 (0.25) H1 0.9500 118.48 118.48 C1 - N1 C2 C2 - Distance Angles C1 1.3842 (0.0038) C3 1.3875 (0.0039) 118.62 (0.25) H2 0.9500 120.69 120.69 C2 - C1 C3 C3 - Distance Angles C2 1.3875 (0.0039) C4 1.3896 (0.0038) 119.06 (0.25) H3 0.9500 120.47 120.47 C3 - C2 C4 C4 - Distance Angles C3 1.3896 (0.0038) C5 1.3955 (0.0036) 119.14 (0.24) H4 0.9500 120.43 120.43 C4 - C3 C5 C5 - Distance Angles N1 1.3529 (0.0031) C4 1.3955 (0.0036) 121.73 (0.23) C6 1.4880 (0.0036) 115.38 (0.22) 122.87 (0.23) C5 - N1 C4 C6 - Distance Angles N2 1.3399 (0.0032) C7 1.4046 (0.0034) 120.53 (0.24) C5 1.4880 (0.0036) 114.40 (0.22) 125.07 (0.23) C6 - N2 C7 C7 - Distance Angles C8 1.3805 (0.0038) C6 1.4046 (0.0034) 118.83 (0.24) H7 0.9500 120.58 120.58 C7 - C8 C6 C8 - Distance Angles C7 1.3805 (0.0038) C9 1.3932 (0.0037) 120.44 (0.23) H8 0.9500 119.78 119.78 C8 - C7 C9 C9 - Distance Angles C10 1.3929 (0.0034) C8 1.3932 (0.0037) 117.70 (0.24) H9 0.9500 121.15 121.15 C9 - C10 C8 C10 - Distance Angles N2 1.3462 (0.0032) C9 1.3929 (0.0034) 121.80 (0.23) C11 1.4921 (0.0034) 112.78 (0.21) 125.32 (0.23) C10 - N2 C9 C11 - Distance Angles N4 1.3113 (0.0032) N3 1.3397 (0.0033) 124.14 (0.23) C10 1.4921 (0.0034) 114.73 (0.22) 120.82 (0.22) C11 - N4 N3 C12 - Distance Angles N5 1.3083 (0.0031) N6 1.3387 (0.0033) 124.97 (0.23) C13 1.4999 (0.0034) 114.18 (0.22) 120.61 (0.21) C12 - N5 N6 C13 - Distance Angles N7 1.3431 (0.0032) C14 1.3887 (0.0034) 121.92 (0.23) C12 1.4999 (0.0034) 112.76 (0.21) 125.22 (0.23) C13 - N7 C14 C14 - Distance Angles C13 1.3887 (0.0034) C15 1.3974 (0.0038) 117.77 (0.24) H14 0.9500 121.12 121.12 C14 - C13 C15 C15 - Distance Angles C16 1.3856 (0.0039) C14 1.3974 (0.0038) 120.19 (0.24) H15 0.9500 119.91 119.91 C15 - C16 C14 C16 - Distance Angles C15 1.3856 (0.0039) C17 1.4013 (0.0035) 118.67 (0.25) H16 0.9500 120.67 120.67 C16 - C15 C17 C17 - Distance Angles N7 1.3399 (0.0033) C16 1.4013 (0.0035) 120.74 (0.23) C18 1.4977 (0.0035) 114.19 (0.21) 125.06 (0.23) C17 - N7 C16 C18 - Distance Angles N8 1.3560 (0.0033) C19 1.3926 (0.0037) 121.91 (0.24) C17 1.4977 (0.0035) 114.73 (0.22) 123.36 (0.23) C18 - N8 C19 C19 - Distance Angles C18 1.3926 (0.0037) C20 1.3959 (0.0039) 118.99 (0.26) H19 0.9500 120.51 120.51 C19 - C18 C20 C20 - Distance Angles C21 1.3857 (0.0041) C19 1.3959 (0.0039) 119.01 (0.26) H20 0.9500 120.50 120.50 C20 - C21 C19 C21 - Distance Angles C20 1.3857 (0.0041) C22 1.3864 (0.0039) 118.70 (0.25) H21 0.9500 120.65 120.65 C21 - C20 C22 C22 - Distance Angles N8 1.3433 (0.0034) C21 1.3864 (0.0039) 123.09 (0.25) H22 0.9500 118.46 118.46 C22 - N8 C21 N1 - Distance Angles C1 1.3465 (0.0033) C5 1.3529 (0.0031) 118.31 (0.22) Zn1 2.2022 (0.0021) 124.72 (0.17) 116.86 (0.17) N1 - C1 C5 N2 - Distance Angles C6 1.3399 (0.0032) C10 1.3462 (0.0032) 120.67 (0.21) Zn1 2.1585 (0.0020) 119.46 (0.17) 119.87 (0.16) N2 - C6 C10 N3 - Distance Angles C11 1.3397 (0.0033) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C11 H3A N4 - Distance Angles C11 1.3113 (0.0032) N5_$4 1.4035 (0.0029) 114.28 (0.21) Zn1 2.1690 (0.0021) 119.83 (0.17) 120.90 (0.15) N4 - C11 N5_$4 N5 - Distance Angles C12 1.3083 (0.0031) N4_$4 1.4035 (0.0029) 114.38 (0.21) Zn1 2.1746 (0.0021) 119.01 (0.17) 116.83 (0.14) N5 - C12 N4_$4 N6 - Distance Angles C12 1.3387 (0.0033) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C17 1.3399 (0.0033) C13 1.3431 (0.0032) 120.64 (0.21) Zn1 2.1560 (0.0021) 119.78 (0.16) 119.57 (0.16) N7 - C17 C13 N8 - Distance Angles C22 1.3433 (0.0033) C18 1.3560 (0.0033) 118.27 (0.23) Zn1 2.1999 (0.0022) 124.06 (0.18) 117.20 (0.16) N8 - C22 C18 Zn1 - Distance Angles N7 2.1560 (0.0021) N2 2.1585 (0.0020) 174.78 (0.08) N4 2.1690 (0.0021) 111.78 (0.08) 72.65 (0.08) N5 2.1746 (0.0021) 72.85 (0.08) 110.67 (0.08) 87.08 (0.08) N8 2.1999 (0.0022) 73.77 (0.08) 102.81 (0.08) 102.94 (0.08) 146.52 (0.08) N1 2.2022 (0.0021) 101.74 (0.08) 73.90 (0.08) 146.48 (0.08) 102.81 (0.08) 86.41 (0.08) Zn1 - N7 N2 N4 N5 N8 O1 - Distance Angles Cl1 1.4390 (0.0020) O1 - O2 - Distance Angles Cl1 1.4440 (0.0022) O2 - O3 - Distance Angles Cl1 1.4429 (0.0021) O3 - O4 - Distance Angles Cl1 1.4444 (0.0020) O4 - Cl1 - Distance Angles O1 1.4390 (0.0020) O3 1.4429 (0.0021) 108.91 (0.13) O2 1.4440 (0.0022) 109.14 (0.13) 109.61 (0.15) O4 1.4444 (0.0020) 109.62 (0.13) 109.90 (0.13) 109.64 (0.13) Cl1 - O1 O3 O2 O11 - Distance Angles Cl11 1.4426 (0.0023) O11 - O12 - Distance Angles Cl11 1.4335 (0.0022) O12 - O13 - Distance Angles Cl11 1.4313 (0.0023) O13 - O14 - Distance Angles Cl11 1.4363 (0.0022) O14 - Cl11 - Distance Angles O13 1.4313 (0.0023) O12 1.4335 (0.0022) 109.41 (0.14) O14 1.4363 (0.0023) 108.80 (0.14) 111.04 (0.15) O11 1.4426 (0.0023) 108.48 (0.16) 109.88 (0.14) 109.18 (0.14) Cl11 - O13 O12 O14 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.34 3.132(3) 150.6 N3-H3A...O4_$1 0.88 2.16 2.991(3) 158.1 N3-H3B...O3_$2 0.88 2.44 3.177(3) 141.8 N6-H6A...O14_$3 0.88 2.09 2.953(3) 166.6 N6-H6B...O11 FMAP and GRID set by program FMAP 2 1 22 GRID -1.316 -2 -1 1.316 2 1 R1 = 0.0536 for 5740 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.54 at 0.0189 0.1411 0.1586 [ 1.05 A from N2 ] Deepest hole -0.50 at 0.0114 0.2049 0.3600 [ 0.55 A from ZN1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4276 / 41296 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0189 0.1411 0.3414 1.00000 0.05 0.54 1.05 N2 1.11 ZN1 2.05 C10 2.06 N4 Q2 1 0.0038 0.3180 0.3480 1.00000 0.05 0.45 1.00 N7 1.17 ZN1 1.98 C17 2.09 C13 Q3 1 0.0213 0.3005 0.3467 1.00000 0.05 0.44 1.04 ZN1 1.17 N7 1.97 N5 2.08 C13 Q4 1 0.0210 0.1617 0.3405 1.00000 0.05 0.43 0.93 ZN1 1.58 N2 1.86 N1 2.18 N5 Q5 1 0.0869 0.3996 0.2896 1.00000 0.05 0.37 0.75 C12 0.76 C13 1.78 N5 1.80 N7 Q6 1 0.0198 0.0254 0.4072 1.00000 0.05 0.37 0.71 C6 0.81 C5 1.75 N2 1.85 N1 Q7 1 0.2032 0.6159 0.2092 1.00000 0.05 0.37 0.87 O11 1.52 CL11 2.06 O12 2.16 O14 Q8 1 0.0064 0.5021 0.3977 1.00000 0.05 0.36 0.72 C17 0.74 C16 1.48 H16 1.78 N7 Q9 1 -0.0382 0.4222 0.4063 1.00000 0.05 0.36 0.71 C17 0.79 C18 1.72 N7 1.80 N8 Q10 1 -0.0641 0.2291 0.3417 1.00000 0.05 0.35 1.06 ZN1 1.69 N4 1.80 N8 2.22 N2 Shortest distances between peaks (including symmetry equivalents) 2 3 0.38 1 4 0.75 8 9 1.29 1 10 1.37 2 10 1.65 4 10 1.72 3 4 1.76 3 10 1.76 2 4 2.00 2 9 2.02 1 3 2.13 3 5 2.15 1 6 2.21 2 5 2.24 1 2 2.27 4 6 2.30 3 9 2.31 2 8 2.59 3 8 2.81 9 10 2.89 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 3.06: 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 0.02: Generate idealized H-atoms 11.52: Structure factors and derivatives 17.45: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.92: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.13: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 09:10:28 Total CPU time: 34.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++