+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0428 started at 15:59:31 on 28-Jun-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0428 in C2 C2/m CELL 0.71073 10.2973 29.8250 9.3067 90.000 90.417 90.000 ZERR 2.00 0.0008 0.0050 0.0011 0.000 0.010 0.000 LATT 7 SYMM - X, Y, - Z SFAC C H N NI PT CL UNIT 112 120 16 2 4 4 V = 2858.17 F(000) = 1340.0 Mu = 5.34 mm-1 Cell Wt = 2729.82 Rho = 1.586 MERG 2 OMIT -3.00 55.00 OMIT 1 7 1 OMIT 1 7 0 OMIT -3 1 1 OMIT -1 1 1 OMIT 0 2 2 OMIT 11 3 0 EXTI 0.00025 FMAP 2 PLAN 5 SIZE 0.04 0.10 0.20 ACTA BOND $H WGHT 0.03520 6.53050 L.S. 6 TEMP -153.00 FVAR 1.85296 0.38363 C1 1 0.321355 0.079882 0.538149 11.00000 0.02454 0.01930 = 0.02679 -0.00083 0.00497 -0.00144 AFIX 43 H1 2 0.357093 0.077998 0.632350 11.00000 -1.20000 AFIX 0 C2 1 0.224442 0.111605 0.512415 11.00000 0.02512 0.01636 = 0.02705 -0.00057 0.00388 -0.00235 C3 1 0.173265 0.113925 0.374413 11.00000 0.03162 0.02305 = 0.03037 0.00177 0.00147 0.00382 AFIX 43 H3 2 0.105254 0.134395 0.352560 11.00000 -1.20000 AFIX 0 C4 1 0.222273 0.086109 0.268778 11.00000 0.05269 0.03469 = 0.02181 -0.00114 0.00050 0.00845 AFIX 43 H4 2 0.190384 0.087968 0.172921 11.00000 -1.20000 AFIX 0 C5 1 0.318024 0.055655 0.304548 11.00000 0.04592 0.02463 = 0.03024 -0.00115 0.01088 0.00706 AFIX 43 H5 2 0.350521 0.036553 0.231466 11.00000 -1.20000 AFIX 0 C6 1 0.174662 0.139943 0.631236 11.00000 0.01729 0.02080 = 0.02210 -0.00044 0.00172 -0.00171 C7 1 0.135038 0.184468 0.606853 11.00000 0.01709 0.02271 = 0.02238 0.00228 -0.00017 0.00026 AFIX 43 H7 2 0.144888 0.197275 0.514107 11.00000 -1.20000 AFIX 0 C8 1 0.081771 0.209922 0.716442 11.00000 0.01762 0.01910 = 0.02195 -0.00128 -0.00082 -0.00102 C9 1 0.065072 0.192790 0.856082 11.00000 0.01536 0.01797 = 0.02075 -0.00082 -0.00099 -0.00032 C10 1 0.110551 0.148886 0.880144 11.00000 0.02154 0.01986 = 0.02176 0.00274 0.00163 -0.00053 AFIX 43 H10 2 0.105304 0.136660 0.974181 11.00000 -1.20000 AFIX 0 C11 1 0.162954 0.122752 0.770942 11.00000 0.01736 0.02046 = 0.03032 0.00169 0.00100 0.00157 AFIX 43 H11 2 0.190998 0.093056 0.791166 11.00000 -1.20000 AFIX 0 C12 1 0.035286 0.257152 0.693084 11.00000 0.02568 0.02188 = 0.01913 0.00027 0.00003 0.00318 AFIX 23 H12A 2 0.084396 0.271103 0.613702 11.00000 -1.20000 H12B 2 -0.057887 0.256948 0.666103 11.00000 -1.20000 AFIX 0 C13 1 -0.022141 0.325694 0.811564 11.00000 0.03840 0.01973 = 0.02711 0.00210 -0.00020 0.00791 AFIX 33 H13A 2 -0.011841 0.344046 0.898246 11.00000 -1.50000 H13B 2 -0.114078 0.318243 0.797744 11.00000 -1.50000 H13C 2 0.009025 0.342468 0.728091 11.00000 -1.50000 AFIX 0 C14 1 0.194498 0.295180 0.843484 11.00000 0.02484 0.02759 = 0.03032 0.00367 0.00190 -0.00562 AFIX 33 H14A 2 0.245398 0.267586 0.853741 11.00000 -1.50000 H14B 2 0.207016 0.313940 0.928920 11.00000 -1.50000 H14C 2 0.223281 0.311580 0.758207 11.00000 -1.50000 AFIX 0 N1 3 0.367230 0.051783 0.437412 11.00000 0.02443 0.01848 = 0.02786 -0.00128 0.00579 0.00014 N2 3 0.054467 0.283689 0.827667 11.00000 0.02184 0.01622 = 0.02019 0.00083 0.00053 0.00115 NI1 4 0.500000 0.000000 0.500000 10.25000 0.02156 0.01276 = 0.03051 0.00000 0.00932 0.00000 PT1 5 0.000000 0.237047 1.000000 10.50000 0.01714 0.01656 = 0.01935 0.00000 0.00113 0.00000 CL1 6 0.590158 0.000000 0.253061 10.50000 0.04820 0.03442 = 0.05631 0.00000 0.01116 0.00000 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2005slh0428 in C2 C2/m C 0.770 H 0.320 N 0.700 NI 1.250 PT 1.370 CL 0.990 C1 - N1 C2 C2 - C3 C1 C6 C3 - C4 C2 C4 - C5 C3 C5 - N1 C4 C6 - C11 C7 C2 C7 - C8 C6 C8 - C7 C9 C12 C9 - C10 C8 Pt1 C10 - C11 C9 C11 - C10 C6 C12 - N2 C8 C13 - N2 C14 - N2 N1 - C5 C1 Ni1 N2 - C13 C14 C12 Pt1 Ni1 - N1_$3 N1_$4 N1 N1_$2 Cl1 Cl1_$2 Pt1 - C9 C9_$1 N2_$1 N2 Cl1 - Ni1 Operators for generating equivalent atoms: $1 -x, y, -z+2 $2 -x+1, -y, -z+1 $3 -x+1, y, -z+1 $4 x, -y, z 14429 Reflections read, of which 39 rejected -10 =< h =< 13, -38 =< k =< 38, -12 =< l =< 12, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 3326 Unique reflections, of which 0 suppressed R(int) = 0.0377 R(sigma) = 0.0332 Friedel opposites merged Maximum memory for data reduction = 2057 / 39366 Special position constraints for Ni1 x = 0.5000 y = 0.0000 z = 0.5000 U23 = 0 U12 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for Pt1 x = 0.0000 z = 1.0000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl1 y = 0.0000 U23 = 0 U12 = 0 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 = 2519 / 204130 wR2 = 0.0675 before cycle 1 for 3326 data and 162 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85302 0.00299 0.021 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 0.019 EXTI Mean shift/esd = 0.013 Maximum = -0.070 for U11 Pt1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2519 / 204130 wR2 = 0.0675 before cycle 2 for 3326 data and 162 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85298 0.00299 -0.014 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 0.006 EXTI Mean shift/esd = 0.004 Maximum = -0.022 for U11 Pt1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2519 / 204130 wR2 = 0.0675 before cycle 3 for 3326 data and 162 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85298 0.00299 -0.001 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2519 / 204130 wR2 = 0.0675 before cycle 4 for 3326 data and 162 / 162 parameters GooF = S = 1.077; Restrained GooF = 1.077 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85298 0.00299 0.001 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H3 Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2519 / 204130 wR2 = 0.0675 before cycle 5 for 3326 data and 162 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85298 0.00299 -0.001 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Pt1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2519 / 204130 wR2 = 0.0675 before cycle 6 for 3326 data and 162 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.85298 0.00299 0.000 OSF 2 0.38363 9.99999 0.000 FVAR 2 3 0.00025 0.00009 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Pt1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C4 Largest correlation matrix elements 0.662 U33 Pt1 / OSF 0.650 U22 Pt1 / OSF 0.660 U11 Pt1 / OSF 0.628 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.3571 0.0780 0.6324 43 0.950 0.000 C1 N1 C2 H3 0.1052 0.1344 0.3526 43 0.950 0.000 C3 C4 C2 H4 0.1904 0.0880 0.1729 43 0.950 0.000 C4 C5 C3 H5 0.3506 0.0366 0.2315 43 0.950 0.000 C5 N1 C4 H7 0.1449 0.1973 0.5141 43 0.950 0.000 C7 C8 C6 H10 0.1053 0.1367 0.9742 43 0.950 0.000 C10 C11 C9 H11 0.1910 0.0931 0.7911 43 0.950 0.000 C11 C10 C6 H12A 0.0844 0.2711 0.6137 23 0.990 0.000 C12 N2 C8 H12B -0.0579 0.2570 0.6661 23 0.990 0.000 C12 N2 C8 H13A -0.0119 0.3440 0.8982 33 0.980 0.000 C13 N2 H13A H13B -0.1141 0.3182 0.7977 33 0.980 0.000 C13 N2 H13A H13C 0.0090 0.3425 0.7281 33 0.980 0.000 C13 N2 H13A H14A 0.2454 0.2676 0.8537 33 0.980 0.000 C14 N2 H14A H14B 0.2070 0.3139 0.9289 33 0.980 0.000 C14 N2 H14A H14C 0.2233 0.3116 0.7582 33 0.980 0.000 C14 N2 H14A 2005slh0428 in C2 C2/m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.32134 0.07989 0.53815 1.00000 0.02448 0.01927 0.02682 -0.00084 0.00501 -0.00146 0.02350 0.00630 0.00034 0.00012 0.00039 0.00000 0.00174 0.00164 0.00180 0.00141 0.00137 0.00140 0.00071 H1 0.35707 0.07800 0.63235 1.00000 0.02820 0.00000 0.00000 C2 0.22444 0.11161 0.51239 1.00000 0.02512 0.01635 0.02697 -0.00056 0.00389 -0.00235 0.02279 0.00594 0.00035 0.00011 0.00037 0.00000 0.00172 0.00153 0.00183 0.00140 0.00138 0.00134 0.00071 C3 0.17325 0.11392 0.37441 1.00000 0.03157 0.02302 0.03038 0.00176 0.00149 0.00385 0.02832 0.00675 0.00038 0.00013 0.00041 0.00000 0.00195 0.00179 0.00195 0.00152 0.00151 0.00151 0.00079 H3 0.10523 0.13439 0.35257 1.00000 0.03398 0.00000 0.00000 C4 0.22226 0.08611 0.26878 1.00000 0.05266 0.03468 0.02179 -0.00116 0.00049 0.00847 0.03637 0.00760 0.00043 0.00015 0.00042 0.00000 0.00259 0.00220 0.00187 0.00163 0.00171 0.00193 0.00094 H4 0.19036 0.08796 0.17293 1.00000 0.04365 0.00000 0.00000 C5 0.31805 0.05566 0.30455 1.00000 0.04586 0.02462 0.03027 -0.00117 0.01084 0.00704 0.03353 0.00744 0.00041 0.00013 0.00042 0.00000 0.00236 0.00190 0.00204 0.00160 0.00172 0.00172 0.00089 H5 0.35057 0.03656 0.23146 1.00000 0.04024 0.00000 0.00000 C6 0.17466 0.13995 0.63123 1.00000 0.01724 0.02078 0.02216 -0.00048 0.00174 -0.00168 0.02005 0.00579 0.00031 0.00011 0.00036 0.00000 0.00157 0.00163 0.00163 0.00133 0.00124 0.00128 0.00067 C7 0.13505 0.18447 0.60685 1.00000 0.01709 0.02270 0.02235 0.00229 -0.00015 0.00025 0.02072 0.00591 0.00031 0.00012 0.00037 0.00000 0.00158 0.00169 0.00165 0.00136 0.00123 0.00130 0.00067 H7 0.14491 0.19727 0.51410 1.00000 0.02486 0.00000 0.00000 C8 0.08176 0.20993 0.71644 1.00000 0.01762 0.01904 0.02197 -0.00125 -0.00083 -0.00101 0.01954 0.00570 0.00031 0.00012 0.00035 0.00000 0.00156 0.00159 0.00160 0.00135 0.00122 0.00130 0.00065 C9 0.06506 0.19279 0.85608 1.00000 0.01536 0.01796 0.02072 -0.00083 -0.00100 -0.00032 0.01802 0.00561 0.00031 0.00011 0.00035 0.00000 0.00152 0.00152 0.00159 0.00127 0.00121 0.00123 0.00064 C10 0.11055 0.14889 0.88014 1.00000 0.02151 0.01984 0.02171 0.00272 0.00162 -0.00051 0.02101 0.00592 0.00032 0.00012 0.00036 0.00000 0.00168 0.00163 0.00165 0.00135 0.00129 0.00134 0.00068 H10 0.10532 0.13666 0.97418 1.00000 0.02522 0.00000 0.00000 C11 0.16295 0.12275 0.77093 1.00000 0.01738 0.02045 0.03031 0.00169 0.00100 0.00157 0.02271 0.00605 0.00032 0.00012 0.00038 0.00000 0.00160 0.00166 0.00185 0.00143 0.00133 0.00132 0.00070 H11 0.19098 0.09306 0.79114 1.00000 0.02725 0.00000 0.00000 C12 0.03529 0.25716 0.69309 1.00000 0.02563 0.02186 0.01913 0.00030 0.00005 0.00322 0.02221 0.00647 0.00038 0.00012 0.00039 0.00000 0.00188 0.00176 0.00169 0.00135 0.00138 0.00139 0.00073 H12A 0.08441 0.27111 0.61372 1.00000 0.02665 0.00000 0.00000 H12B -0.05788 0.25696 0.66610 1.00000 0.02665 0.00000 0.00000 C13 -0.02216 0.32569 0.81156 1.00000 0.03838 0.01969 0.02710 0.00208 -0.00023 0.00793 0.02839 0.00695 0.00039 0.00012 0.00040 0.00000 0.00214 0.00172 0.00186 0.00146 0.00155 0.00156 0.00080 H13A -0.01186 0.34405 0.89824 1.00000 0.04259 0.00000 0.00000 H13B -0.11409 0.31824 0.79774 1.00000 0.04259 0.00000 0.00000 H13C 0.00900 0.34247 0.72808 1.00000 0.04259 0.00000 0.00000 C14 0.19449 0.29518 0.84349 1.00000 0.02484 0.02756 0.03029 0.00368 0.00190 -0.00563 0.02756 0.00650 0.00034 0.00013 0.00040 0.00000 0.00181 0.00189 0.00191 0.00156 0.00144 0.00150 0.00078 H14A 0.24539 0.26759 0.85374 1.00000 0.04133 0.00000 0.00000 H14B 0.20700 0.31394 0.92892 1.00000 0.04133 0.00000 0.00000 H14C 0.22327 0.31158 0.75821 1.00000 0.04133 0.00000 0.00000 N1 0.36722 0.05178 0.43739 1.00000 0.02441 0.01844 0.02787 -0.00127 0.00579 0.00014 0.02355 0.00511 0.00028 0.00010 0.00032 0.00000 0.00152 0.00141 0.00157 0.00120 0.00119 0.00117 0.00062 N2 0.05447 0.28369 0.82766 1.00000 0.02180 0.01619 0.02026 0.00083 0.00054 0.00116 0.01941 0.00489 0.00027 0.00009 0.00029 0.00000 0.00143 0.00136 0.00137 0.00114 0.00108 0.00113 0.00057 Ni1 0.50000 0.00000 0.50000 0.25000 0.02155 0.01275 0.03052 0.00000 0.00932 0.00000 0.02156 0.00000 0.00000 0.00000 0.00000 0.00000 0.00044 0.00039 0.00047 0.00000 0.00035 0.00000 0.00019 Pt1 0.00000 0.23705 1.00000 0.50000 0.01713 0.01656 0.01934 0.00000 0.00113 0.00000 0.01767 0.00017 0.00000 0.00001 0.00000 0.00000 0.00012 0.00011 0.00011 0.00000 0.00007 0.00000 0.00008 Cl1 0.59016 0.00000 0.25306 0.50000 0.04819 0.03443 0.05630 0.00000 0.01117 0.00000 0.04625 0.00257 0.00016 0.00000 0.00019 0.00000 0.00090 0.00078 0.00097 0.00000 0.00072 0.00000 0.00038 Final Structure Factor Calculation for 2005slh0428 in C2 C2/m Total number of l.s. parameters = 162 Maximum vector length = 511 Memory required = 2357 / 25039 wR2 = 0.0675 before cycle 7 for 3326 data and 0 / 162 parameters GooF = S = 1.076; Restrained GooF = 1.076 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0352 * P )^2 + 6.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0269 for 3101 Fo > 4sig(Fo) and 0.0295 for all 3326 data wR2 = 0.0675, GooF = S = 1.076, Restrained GooF = 1.076 for all data Occupancy sum of asymmetric unit = 17.25 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0308 0.0209 0.0188 C1 0.0301 0.0225 0.0157 C2 0.0340 0.0296 0.0214 C3 0.0560 0.0315 0.0216 C4 0.0523 0.0283 0.0199 C5 0.0231 0.0208 0.0163 C6 0.0248 0.0203 0.0170 C7 0.0225 0.0194 0.0167 C8 0.0211 0.0179 0.0151 C9 0.0240 0.0216 0.0175 C10 0.0307 0.0207 0.0167 C11 0.0275 0.0201 0.0190 C12 0.0413 0.0275 0.0164 C13 0.0335 0.0300 0.0192 C14 0.0320 0.0206 0.0180 N1 0.0222 0.0202 0.0158 N2 0.0361 0.0158 0.0127 Ni1 0.0197 0.0167 0.0166 Pt1 0.0637 0.0406 0.0344 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.040 0.076 0.108 0.137 0.161 0.186 0.215 0.258 0.324 1.000 Number in group 338. 333. 327. 337. 340. 326. 332. 326. 333. 334. GooF 0.890 1.196 1.207 1.142 1.120 1.086 0.983 1.025 0.969 1.104 K 1.195 0.950 0.963 0.974 0.991 1.004 1.013 1.016 1.015 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 339. 337. 327. 343. 324. 325. 332. 333. 331. 335. GooF 1.047 0.935 0.923 0.988 0.990 1.008 0.931 0.861 1.107 1.716 K 0.960 0.995 0.999 1.026 1.025 1.018 1.014 1.013 1.005 0.994 R1 0.065 0.043 0.039 0.034 0.030 0.028 0.023 0.018 0.018 0.027 Recommended weighting scheme: WGHT 0.0351 6.6331 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 1 2 758.21 1280.74 5.21 0.070 4.19 -1 1 2 1329.35 800.47 5.01 0.055 4.21 5 5 0 901.25 483.52 4.95 0.043 1.95 1 5 0 1010.11 1494.01 4.24 0.075 5.16 3 3 0 7412.68 5892.77 4.23 0.150 3.24 1 3 4 6222.22 7763.05 4.21 0.172 2.21 0 6 0 34586.18 41492.85 3.85 0.397 4.97 1 9 0 24911.10 20651.02 3.84 0.280 3.15 2 2 10 10356.48 8043.49 3.79 0.175 0.91 -1 7 5 1915.99 2546.34 3.78 0.098 1.68 0 10 6 7344.80 8884.81 3.68 0.184 1.38 3 3 3 3731.51 4649.43 3.67 0.133 2.23 -2 0 9 20430.82 16699.30 3.66 0.252 1.02 -2 4 1 16768.01 19824.49 3.66 0.274 3.86 1 11 7 1665.33 2678.20 3.61 0.101 1.18 0 6 10 9802.38 7778.39 3.56 0.172 0.91 -1 1 6 360.10 160.93 3.54 0.025 1.53 3 1 5 287.61 504.75 3.33 0.044 1.63 -3 7 3 8029.44 6778.31 3.32 0.160 2.03 0 2 10 15940.65 13392.12 3.23 0.226 0.93 0 18 4 2116.19 2723.04 3.22 0.102 1.35 0 0 2 19005.77 15285.21 3.22 0.241 4.65 0 26 1 1438.77 2059.48 3.20 0.088 1.14 0 14 4 2236.13 1695.16 3.17 0.080 1.57 -1 1 5 1566.71 1173.26 3.16 0.067 1.83 -1 3 1 11571.65 9999.30 3.09 0.195 5.68 -3 5 4 2845.85 3485.03 3.06 0.115 1.84 2 4 3 52806.35 60145.71 3.06 0.478 2.50 1 5 2 5299.24 6340.54 3.04 0.155 3.45 -3 3 9 796.11 423.83 3.02 0.040 0.99 2 6 0 5450.02 6437.67 3.01 0.156 3.58 -12 4 5 1656.60 3136.19 2.98 0.109 0.78 1 5 4 6798.57 5767.59 2.94 0.148 2.12 -5 1 2 951.67 1262.71 2.92 0.069 1.88 1 5 5 5852.17 6893.70 2.90 0.162 1.75 -5 9 4 5579.96 6646.17 2.88 0.159 1.40 3 9 2 5638.42 6597.16 2.82 0.158 2.12 2 0 4 40982.56 46589.74 2.81 0.421 2.11 6 18 2 218.13 29.89 2.80 0.011 1.15 10 16 6 744.12 1343.29 2.80 0.071 0.78 -3 9 4 3829.41 4535.19 2.78 0.131 1.67 -2 14 1 24822.75 21987.52 2.77 0.289 1.93 3 7 3 3649.71 4320.00 2.77 0.128 2.02 2 2 5 33814.13 38082.18 2.77 0.380 1.73 -2 12 3 2713.01 2209.18 2.77 0.092 1.82 1 3 2 3412.04 2866.31 2.76 0.104 3.89 -3 1 4 1089.95 811.58 2.73 0.056 1.93 0 2 3 57926.49 64930.36 2.73 0.497 3.04 0 0 8 41368.03 36059.80 2.70 0.370 1.16 6 12 0 14899.32 13111.38 2.68 0.223 1.41 Bond lengths and angles C1 - Distance Angles N1 1.3459 (0.0045) C2 1.3944 (0.0048) 123.85 (0.33) H1 0.9500 118.07 118.07 C1 - N1 C2 C2 - Distance Angles C3 1.3863 (0.0052) C1 1.3944 (0.0048) 117.38 (0.32) C6 1.4862 (0.0047) 122.01 (0.32) 120.54 (0.31) C2 - C3 C1 C3 - Distance Angles C4 1.3845 (0.0054) C2 1.3863 (0.0052) 119.32 (0.36) H3 0.9500 120.34 120.34 C3 - C4 C2 C4 - Distance Angles C5 1.3797 (0.0057) C3 1.3845 (0.0054) 119.13 (0.37) H4 0.9500 120.44 120.44 C4 - C5 C3 C5 - Distance Angles N1 1.3376 (0.0049) C4 1.3797 (0.0057) 123.03 (0.35) H5 0.9500 118.49 118.49 C5 - N1 C4 C6 - Distance Angles C11 1.4036 (0.0048) C7 1.4070 (0.0047) 117.86 (0.31) C2 1.4862 (0.0047) 120.93 (0.31) 121.19 (0.30) C6 - C11 C7 C7 - Distance Angles C8 1.3878 (0.0047) C6 1.4070 (0.0047) 120.90 (0.31) H7 0.9500 119.55 119.55 C7 - C8 C6 C8 - Distance Angles C7 1.3878 (0.0047) C9 1.4083 (0.0046) 122.09 (0.31) C12 1.5031 (0.0048) 122.26 (0.30) 115.64 (0.29) C8 - C7 C9 C9 - Distance Angles C10 1.4080 (0.0047) C8 1.4083 (0.0046) 116.20 (0.30) Pt1 1.9996 (0.0033) 128.32 (0.25) 114.98 (0.24) C9 - C10 C8 C10 - Distance Angles C11 1.3927 (0.0048) C9 1.4080 (0.0047) 122.31 (0.32) H10 0.9500 118.84 118.84 C10 - C11 C9 C11 - Distance Angles C10 1.3927 (0.0048) C6 1.4036 (0.0048) 120.53 (0.32) H11 0.9500 119.74 119.74 C11 - C10 C6 C12 - Distance Angles N2 1.4933 (0.0045) C8 1.5031 (0.0048) 109.59 (0.28) H12A 0.9900 109.75 109.75 H12B 0.9900 109.75 109.75 108.22 C12 - N2 C8 H12A C13 - Distance Angles N2 1.4876 (0.0043) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - N2 H13A H13B C14 - Distance Angles N2 1.4883 (0.0044) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - N2 H14A H14B N1 - Distance Angles C5 1.3376 (0.0049) C1 1.3459 (0.0045) 117.24 (0.31) Ni1 2.1407 (0.0029) 123.41 (0.24) 119.10 (0.24) N1 - C5 C1 N2 - Distance Angles C13 1.4876 (0.0043) C14 1.4883 (0.0044) 109.19 (0.28) C12 1.4933 (0.0045) 107.15 (0.27) 109.09 (0.27) Pt1 2.1989 (0.0028) 117.93 (0.21) 109.00 (0.21) 104.10 (0.20) N2 - C13 C14 C12 Ni1 - Distance Angles N1_$3 2.1407 (0.0029) N1_$4 2.1407 (0.0029) 180.00 (0.11) N1 2.1407 (0.0029) 87.65 (0.16) 92.35 (0.16) N1_$2 2.1407 (0.0029) 92.35 (0.16) 87.65 (0.16) 180.00 (0.11) Cl1 2.4849 (0.0017) 90.55 (0.08) 89.45 (0.08) 89.45 (0.08) 90.55 (0.08) Cl1_$2 2.4849 (0.0017) 89.45 (0.08) 90.55 (0.08) 90.55 (0.08) 89.45 (0.08) 180.00 Ni1 - N1_$3 N1_$4 N1 N1_$2 Cl1 Pt1 - Distance Angles C9 1.9996 (0.0033) C9_$1 1.9996 (0.0033) 97.38 (0.19) N2_$1 2.1989 (0.0028) 174.09 (0.11) 80.83 (0.13) N2 2.1989 (0.0028) 80.83 (0.13) 174.09 (0.11) 101.51 (0.15) Pt1 - C9 C9_$1 N2_$1 Cl1 - Distance Angles Ni1 2.4849 (0.0017) Cl1 - FMAP and GRID set by program FMAP 2 1 14 GRID -2.273 -1 -2 2.273 1 2 R1 = 0.0291 for 3326 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.65 at 0.0000 0.2898 0.0000 [ 1.57 A from PT1 ] Deepest hole -1.50 at 0.0947 0.5000 0.2954 [ 0.40 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 3036 / 29109 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0000 0.2898 1.0000 0.50000 0.05 1.65 1.57 PT1 1.71 N2 1.88 H13A 2.07 C13 Q2 1 0.5957 0.0000 0.3594 0.50000 0.05 1.17 0.99 CL1 1.64 NI1 2.38 H1 2.47 N1 Q3 1 0.0273 0.2388 1.0864 1.00000 0.05 0.89 0.85 PT1 1.75 C9 1.78 N2 2.22 C12 Q4 1 0.5935 0.0000 0.1276 0.50000 0.05 0.63 1.17 CL1 2.90 H5 3.26 H1 3.57 H5 Q5 1 0.0000 0.2044 1.0000 0.50000 0.05 0.61 0.97 PT1 1.54 C9 2.30 C10 2.31 H10 Shortest distances between peaks (including symmetry equivalents) 3 5 1.33 3 3 1.70 1 3 1.74 2 4 2.16 1 5 2.55 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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. 1.24: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.84: Structure factors and derivatives 1.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0428 finished at 15:59:36 Total CPU time: 5.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++