ࡱ> M -bjbj== rWW&lTl+FFFFFFFF*******$, ."+EFFFFF"+*FFg+***FFF**F**b***F: p&.v^ **}+0+*S/*S/**    Table 1. Crystal data and structure refinement for jpb25. Identification code jpb25 Empirical formula C34 H54 Cr N2 O Si Formula weight 586.88 Temperature 218(2) K Wavelength 0.71073 Crystal system Monoclinic Space group P2(1)/c Unit cell dimensions a = 18.0097(18) a= 90. b = 11.2061(11) b= 117.162(2). c = 19.151(2) g = 90. Volume 3438.7(6) 3 Z 4 Density (calculated) 1.134 Mg/m3 Absorption coefficient 0.394 mm-1 F(000) 1272 Crystal size 0.20 x 0.20 x 0.15 mm3 Theta range for data collection 2.13 to 25.00. Index ranges -20<=h<=21, -12<=k<=13, -22<=l<=22 Reflections collected 20485 Independent reflections 6059 [R(int) = 0.0570] Completeness to theta = 25.00 100.0 % Absorption correction None Max. and min. transmission 0.9433 and 0.9254 Refinement method Full-matrix least-squares on F2 Data / restraints / parameters 6059 / 0 / 347 Goodness-of-fit on F2 1.006 Final R indices [I>2sigma(I)] R1 = 0.0536, wR2 = 0.1321 R indices (all data) R1 = 0.0774, wR2 = 0.1455 Largest diff. peak and hole 0.447 and -0.383 e.-3 Table 2. Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (2x 103) for jpb25. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ O(1) 2779(1) 10109(2) 4650(1) 38(1) Si(1) 2818(1) 9599(1) 3829(1) 43(1) Cr(1) 2195(1) 8494(1) 4809(1) 28(1) N(1) 1895(2) 6754(2) 4897(1) 30(1) N(2) 2093(1) 8894(2) 5817(1) 29(1) C(1) 1436(3) 5019(3) 5406(2) 52(1) C(2) 1618(2) 6335(3) 5389(2) 35(1) C(3) 1513(2) 7027(3) 5939(2) 36(1) C(4) 1765(2) 8189(3) 6169(2) 30(1) C(5) 1689(2) 8616(3) 6874(2) 42(1) C(6) 2452(2) 9995(3) 6210(2) 31(1) C(7) 1955(2) 11018(3) 6075(2) 36(1) C(8) 2338(2) 12065(3) 6450(2) 44(1) C(9) 3186(2) 12114(3) 6942(2) 51(1) C(10) 3661(2) 11105(3) 7076(2) 50(1) C(11) 3306(2) 10025(3) 6721(2) 40(1) C(12) 1027(2) 10988(3) 5520(2) 41(1) C(13) 509(2) 11702(4) 5824(3) 65(1) C(14) 848(2) 11421(4) 4703(2) 62(1) C(15) 3842(2) 8908(3) 6911(2) 54(1) C(16) 4563(3) 9043(4) 6713(3) 78(1) C(17) 4169(3) 8555(4) 7769(3) 85(2) C(18) 2052(2) 5900(3) 4421(2) 35(1) C(19) 2882(2) 5591(3) 4633(2) 43(1) C(20) 3041(3) 4794(3) 4160(2) 55(1) C(21) 2394(3) 4310(3) 3503(2) 57(1) C(22) 1586(3) 4617(3) 3305(2) 48(1) C(23) 1387(2) 5420(3) 3747(2) 38(1) C(24) 3593(2) 6129(3) 5360(2) 54(1) C(25) 4437(3) 6126(5) 5350(3) 84(2) C(26) 3676(3) 5543(5) 6111(3) 78(1) C(27) 489(2) 5763(3) 3490(2) 44(1) C(28) -85(3) 4674(4) 3316(3) 74(1) C(29) 154(2) 6558(4) 2766(2) 63(1) C(30) 2166(2) 8332(3) 3680(2) 51(1) C(31) 2451(3) 10825(4) 3093(3) 77(1) C(32) 3925(3) 9233(5) 4091(3) 85(2) C(33) 2935(2) 11343(3) 4904(2) 53(1) C(34) 3806(3) 11741(4) 5138(3) 73(1) ________________________________________________________________________________ Table 3. Bond lengths [] and angles [] for jpb25. _________________________________________________________________________________________ O(1)-C(33) 1.451(4) O(1)-Si(1) 1.704(2) O(1)-Cr(1) 2.182(2) Si(1)-C(30) 1.780(4) Si(1)-C(31) 1.860(4) Si(1)-C(32) 1.866(4) Si(1)-Cr(1) 2.8695(11) Cr(1)-N(1) 2.052(2) Cr(1)-N(2) 2.071(2) Cr(1)-C(30) 2.147(3) N(1)-C(2) 1.334(4) N(1)-C(18) 1.436(4) N(2)-C(4) 1.337(4) N(2)-C(6) 1.436(4) C(1)-C(2) 1.515(4) C(2)-C(3) 1.391(4) C(3)-C(4) 1.383(4) C(4)-C(5) 1.496(4) C(6)-C(11) 1.398(4) C(6)-C(7) 1.403(4) C(7)-C(8) 1.384(4) C(7)-C(12) 1.517(4) C(8)-C(9) 1.382(5) C(9)-C(10) 1.369(5) C(10)-C(11) 1.392(4) C(11)-C(15) 1.520(5) C(12)-C(14) 1.524(5) C(12)-C(13) 1.533(5) C(15)-C(16) 1.517(6) C(15)-C(17) 1.524(6) C(18)-C(19) 1.402(4) C(18)-C(23) 1.407(4) C(19)-C(20) 1.392(5) C(19)-C(24) 1.521(5) C(20)-C(21) 1.377(6) C(21)-C(22) 1.369(5) C(22)-C(23) 1.390(5) C(23)-C(27) 1.509(5) C(24)-C(26) 1.525(6) C(24)-C(25) 1.530(5) C(27)-C(29) 1.523(5) C(27)-C(28) 1.534(5) C(33)-C(34) 1.489(5) C(33)-O(1)-Si(1) 123.0(2) C(33)-O(1)-Cr(1) 140.9(2) Si(1)-O(1)-Cr(1) 94.37(9) O(1)-Si(1)-C(30) 96.54(14) O(1)-Si(1)-C(31) 107.59(18) C(30)-Si(1)-C(31) 119.1(2) O(1)-Si(1)-C(32) 108.32(18) C(30)-Si(1)-C(32) 114.4(2) C(31)-Si(1)-C(32) 109.4(2) O(1)-Si(1)-Cr(1) 49.32(7) C(30)-Si(1)-Cr(1) 48.33(11) C(31)-Si(1)-Cr(1) 134.79(17) C(32)-Si(1)-Cr(1) 114.70(18) N(1)-Cr(1)-N(2) 89.42(10) N(1)-Cr(1)-C(30) 96.69(12) N(2)-Cr(1)-C(30) 170.41(13) N(1)-Cr(1)-O(1) 164.05(9) N(2)-Cr(1)-O(1) 101.77(9) C(30)-Cr(1)-O(1) 73.84(11) N(1)-Cr(1)-Si(1) 131.35(7) N(2)-Cr(1)-Si(1) 138.07(7) C(30)-Cr(1)-Si(1) 38.27(9) O(1)-Cr(1)-Si(1) 36.31(6) C(2)-N(1)-C(18) 117.3(2) C(2)-N(1)-Cr(1) 126.1(2) C(18)-N(1)-Cr(1) 116.41(19) C(4)-N(2)-C(6) 116.1(3) C(4)-N(2)-Cr(1) 126.1(2) C(6)-N(2)-Cr(1) 117.68(19) N(1)-C(2)-C(3) 124.2(3) N(1)-C(2)-C(1) 120.8(3) C(3)-C(2)-C(1) 114.9(3) C(4)-C(3)-C(2) 128.8(3) N(2)-C(4)-C(3) 123.6(3) N(2)-C(4)-C(5) 120.6(3) C(3)-C(4)-C(5) 115.8(3) C(11)-C(6)-C(7) 121.0(3) C(11)-C(6)-N(2) 118.5(3) C(7)-C(6)-N(2) 120.5(3) C(8)-C(7)-C(6) 118.2(3) C(8)-C(7)-C(12) 120.7(3) C(6)-C(7)-C(12) 121.1(3) C(9)-C(8)-C(7) 121.4(3) C(10)-C(9)-C(8) 119.8(3) C(9)-C(10)-C(11) 121.2(3) C(10)-C(11)-C(6) 118.4(3) C(10)-C(11)-C(15) 120.0(3) C(6)-C(11)-C(15) 121.5(3) C(7)-C(12)-C(14) 111.2(3) C(7)-C(12)-C(13) 112.9(3) C(14)-C(12)-C(13) 110.1(3) C(16)-C(15)-C(11) 112.3(3) C(16)-C(15)-C(17) 110.0(3) C(11)-C(15)-C(17) 111.2(3) C(19)-C(18)-C(23) 121.3(3) C(19)-C(18)-N(1) 118.3(3) C(23)-C(18)-N(1) 120.4(3) C(20)-C(19)-C(18) 118.6(3) C(20)-C(19)-C(24) 120.8(3) C(18)-C(19)-C(24) 120.5(3) C(21)-C(20)-C(19) 120.5(4) C(22)-C(21)-C(20) 120.2(3) C(21)-C(22)-C(23) 122.1(4) C(22)-C(23)-C(18) 117.3(3) C(22)-C(23)-C(27) 120.2(3) C(18)-C(23)-C(27) 122.6(3) C(26)-C(24)-C(19) 111.8(3) C(26)-C(24)-C(25) 109.9(3) C(19)-C(24)-C(25) 114.4(3) C(23)-C(27)-C(29) 111.5(3) C(23)-C(27)-C(28) 112.6(3) C(29)-C(27)-C(28) 108.7(3) Si(1)-C(30)-Cr(1) 93.41(15) O(1)-C(33)-C(34) 113.8(3) ________________________________________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Anisotropic displacement parameters (2x 103) for jpb25. The anisotropic displacement factor exponent takes the form: -2p2[ h2 a*2U11 + ... + 2 h k a* b* U12 ] ______________________________________________________________________________ U11 U22 U33 U23 U13 U12 ______________________________________________________________________________ O(1) 47(1) 32(1) 41(1) -3(1) 26(1) -8(1) Si(1) 53(1) 42(1) 42(1) -1(1) 29(1) -9(1) Cr(1) 34(1) 24(1) 30(1) 0(1) 17(1) -2(1) N(1) 38(1) 25(1) 30(1) 0(1) 17(1) 3(1) N(2) 33(1) 27(1) 28(1) 0(1) 14(1) 1(1) C(1) 87(3) 29(2) 52(2) 4(2) 41(2) -7(2) C(2) 43(2) 27(2) 37(2) 3(1) 21(2) -1(1) C(3) 45(2) 33(2) 38(2) 4(1) 27(2) -3(1) C(4) 33(2) 32(2) 29(2) 0(1) 17(1) 3(1) C(5) 53(2) 42(2) 39(2) 0(2) 28(2) 2(2) C(6) 38(2) 28(2) 30(2) -3(1) 17(1) -2(1) C(7) 46(2) 29(2) 36(2) -1(1) 22(2) 1(1) C(8) 58(2) 30(2) 47(2) -5(2) 25(2) 2(2) C(9) 57(2) 36(2) 52(2) -16(2) 19(2) -12(2) C(10) 41(2) 47(2) 49(2) -11(2) 10(2) -7(2) C(11) 39(2) 37(2) 37(2) -5(2) 11(2) -1(1) C(12) 41(2) 36(2) 47(2) -1(2) 20(2) 6(1) C(13) 54(2) 64(3) 75(3) -9(2) 29(2) 18(2) C(14) 49(2) 76(3) 51(2) 11(2) 14(2) 6(2) C(15) 35(2) 45(2) 61(3) -4(2) 4(2) 7(2) C(16) 61(3) 78(3) 90(4) 0(3) 30(2) 23(2) C(17) 69(3) 81(3) 90(4) 30(3) 23(3) 19(2) C(18) 55(2) 20(2) 38(2) 4(1) 28(2) 3(1) C(20) 74(3) 47(2) 55(2) 8(2) 39(2) 26(2) C(21) 96(3) 39(2) 53(3) 1(2) 49(2) 17(2) C(22) 75(3) 35(2) 40(2) -4(2) 31(2) -3(2) C(23) 54(2) 26(2) 39(2) 0(1) 27(2) -5(1) C(24) 45(2) 53(2) 59(3) -3(2) 20(2) 16(2) C(25) 52(3) 101(4) 98(4) -7(3) 34(3) 15(2) C(26) 70(3) 98(4) 54(3) 5(3) 18(2) 21(3) C(27) 50(2) 42(2) 43(2) -8(2) 25(2) -13(2) C(28) 69(3) 67(3) 84(3) 1(2) 33(3) -30(2) C(29) 46(2) 69(3) 69(3) 18(2) 23(2) -1(2) C(30) 77(3) 45(2) 38(2) -3(2) 33(2) -17(2) C(31) 106(4) 67(3) 55(3) 11(2) 33(3) -25(3) C(32) 73(3) 90(4) 113(4) -16(3) 60(3) -3(3) C(33) 72(3) 34(2) 65(3) -7(2) 42(2) -11(2) C(34) 74(3) 54(3) 92(4) -11(2) 39(3) -26(2) ______________________________________________________________________________ Table 5. Hydrogen coordinates ( x 104) and isotropic displacement parameters (2x 10 3) for jpb25. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ H(1A) 1525 4604 5006 79 H(1B) 861 4916 5306 79 H(1C) 1806 4693 5918 79 H(3A) 1231 6655 6190 43 H(5A) 1879 9436 6986 63 H(5B) 2029 8118 7321 63 H(5C) 1110 8569 6772 63 H(8A) 2014 12757 6367 53 H(9A) 3435 12837 7185 61 H(10A) 4237 11143 7413 60 H(12A) 845 10146 5470 49 H(13A) -78 11644 5451 97 H(13B) 680 12532 5886 97 H(13C) 596 11382 6326 97 H(14A) 1169 10952 4511 93 H(14B) 1002 12255 4728 93 H(14C) 257 11330 4350 93 H(15A) 3484 8249 6586 65 H(16A) 4349 9265 6166 117 H(16B) 4861 8292 6805 117 H(16C) 4939 9658 7042 117 H(17A) 3704 8466 7890 127 H(17B) 4543 9169 8101 127 H(17C) 4468 7804 7863 127 H(20A) 3594 4585 4290 66 H(21A) 2507 3767 3189 68 H(22A) 1153 4273 2857 58 H(24A) 3446 6975 5381 64 H(25A) 4855 6488 5829 125 H(25B) 4395 6578 4901 125 H(25C) 4598 5311 5314 125 H(26A) 3140 5555 6116 117 H(26B) 4082 5977 6562 117 H(26C) 3859 4723 6133 117 H(27A) 465 6218 3922 53 H(28A) 113 4171 3779 111 H(28B) -84 4224 2884 111 H(28C) -649 4939 3176 111 H(29A) 507 7257 2871 94 H(29B) -410 6806 2637 94 H(29C) 151 6120 2328 94 H(30A) 2417 7588 3619 61 H(30B) 1606 8433 3243 61 H(31A) 2845 10934 2883 116 H(31B) 2408 11558 3341 116 H(31C) 1908 10621 2670 116 H(32A) 4085 9639 3734 128 H(32B) 3981 8378 4052 128 H(32C) 4283 9492 4624 128 H(33A) 2815 11450 5350 64 H(33B) 2551 11854 4476 64 H(34A) 3867 12571 5298 109 H(34B) 3927 11654 4697 109 H(34C) 4191 11255 5572 109 ________________________________________________________________________________ 5jl$vMּI?;5ba$ԐL<'ǭmh5ЖMq<'nq?7[pAGy B9s:m;,uӔDAblzfkMլd%8 AɳI=Iۭg`\U=*DR}fm[ҟ@GڌŗvC* PPo9+EBy*mMTVɩf.75^tAlޚy BL 1e7+ZjiJ _@Ii8.m'"TD],AB }vYTqF VlTWWv͝x+×o٩YvY,gL/Q<2ࣰHX9k/lJOܠ6F4 ]%I==ZW3mJa[}@ٝ oXYf}Wx@U|j Ri៶Sib}nީDS%Ao˫|>3b]e{e=<C,䏋%\_^ Fb0 ٪lc|>h6l:Q9P6#0&/lKըh)WNQ+c.(>h ScJAɄxxo&!OJ|*& k&R+nILlWl=ޭbDNslÀƒ7hP>ۚt%4`WsO2\ XFUyJm*w WCRS*7d @]" EwgyTs@F*ɛijen46TQ}26V X >|s*@nii|206AO K'gF)cdE5x\̕1}ՙ%EWqluibNv⪥f x gXĎa;$ymCD=+bBA l릥=M|ƋA[g a.c >]T_= Ef>Hew)M˂3ƶUJ9_=u:+kcm@"AS|JQ!T:,!D#uIК.wZ}gVCy\jbVMճvbD!hKZ?׺%Ŀst†E E CϹ$τ+a$s]l1h_nvA(Ãd.r#UVGM*rŹ/F: )mBF׹N)S-c4֒ྺ8ZacTٶk}Rѵ+5tqrE_ՅKI2dM5.5m?n`̈́θT:FxBƭzR ØۉU:O%͓l}&gђ5EJN2&}%#86s]po&S[-5u~Sn im2c.j†"f ϕ-+n8PtbBP/`OYrNn蒚plT{[lg I֞P};<)ҁo(i*?a2wrEplD65+ _b\IN(8ccmK}ȷ0-*ut[~il!g1 flPh8 t>G?!Q& i{?ZA¡\Z%F }1f!T #y/5(7,H-%  4QϱY}eFeox6nc E6m77 7Qf9MD2h,\'Q-?-7'ԳELEf/~{3iiS8Hten)g4;ɝŒc,DmC{qʔV:A)'Z$d|‘ ?N]b _e Z(Ö]J>x778ܡ%b{>FRV{ZJxQ 2.AQLb(Z>/qśMmL?ߟ4^]}D5l  ,7ƺK4>-j6K(LJ| %"ip#bO#@g9B]ZŒKʇM!R3r:(vIk#&[D cE wV] m!7q>=B8ھR/ 7 4,u*&,ż ǩ>¯$6Dv8MGicnؤ*4Pae5! 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-*-; -* ; -*-:  -*-: -*-:   -*-: -*-:  -* ;  -*-;  -* ;  -* ; -* ; -*-; -*-8   -* 8  -* 8 -*-8  -* 8 -* 8  -*-9 -* 9  -* 9 -*-9  -* 9  -* 9  -* >  -* > -*-> -* >   -*-> -* >  -* ?  -* ?  -*-?  -* ?  -*-?  -* ?   -* < -*-< -* <  -* <  -* < -*-<  -* < -* =  -* =  -* = -* = -* =   -*-=  -* 2 -* 2 -* 2  -* 2 -* 2  -* 2  -*-2   -* 3 -* 3  -*-3 -* 3 -* 3 -*<: -*<: -*<:  -*<:  -*<:   -*<;   -*<; -*<;  -*<; -*<;   -*<8  -*<8 -*<8  -*<8 -*<8 -*<9   -*<9  -*<9  3 0.63 7.37 6 7 14 -3 -4.73 4.91 6 -7 14 3 -0.92 6.73 5 -6 14 3 -2.28 6.50 6 -6 14 3 1.83 6.52 5 6 14 -3 4.75 4.60 6 -5 14 3 -1.85 6.27 6 -5 14 3 -3.30 5.97 5 5 14 -3 8.96 4.61 6 4 14 -3 -0.11 3.86 6 -4 14 3 -1.23 6.19 6 -4 14 3 -3.75 5.41 5 3 14 -3 10.05 4.40 6 -3 14 3 5.97 6.21 6 -3 14 3 -2.09 5.69 5 -2 14 3 -3.40 5.75 6 2 14 -3 3.52 4.83 6 -2 14 3 3.00 5.82 5 -1 14 3 10.62 4.77 6 -1 14 3 5.94 4.68 5 1 14 -3 9.64 6.57 6 0 14 -3 -0.94 5.70 6 0 14 3 -1.54 3.98 5 0 14 3 -1.29 3.22 6 1 14 3 1.63 3.44 6 1 14 3 11.72 4.69 5 -1 14 -3 2.50 6.00 6 -2 14 -3 2.79 6.90 6 2 14 3 5.16 4.00 5 2 14 3 7.66 3.93 6 3 14 3 12.75 5.10 6 -3 14 -3 7.19 7.24 6 3 14 3 8.32 4.99 5 4 14 3 4.03 5.08 5 4 14 3 3.02 4.84 6 -4 14 -3 1.89 7.29 6 5 14 3 0.57 4.82 5 -5 14 -3 5.62 7.62 6 5 14 3 0.64 4.86 6 22 0 -4 11.64 4.69 5 21 0 -4 1.30 3.46 5 20 0 -4 5.48 3.58 6 19 0 -4 9.34 3.56 6 18 0 -4 3.62 2.45 6 17 0 -4 -3.72 2.00 6 16 0 -4 65.09 7.05 6 15 0 -4 55.78 6.10 6 14 0 -4 37.47 4.67 6 13 0 -4 42.66 4.91 6 -12 0 4 -0.38 2.11 2 12 0 -4 -0.03 2.13 6 -11 0 4 220.83 19.49 2 11 0 -4 252.04 18.76 6 10 0 -4 215.95 16.32 6 -10 0 4 203.99 16.27 5 -10 0 4 194.57 16.98 2 -9 0 4 1081.87 80.65 2 -9 0 4 1049.87 79.22 5 9 0 -4 1046.81 78.01 6 8 0 -4 17.88 2.89 6 -8 0 4 19.15 2.84 5 -8 0 4 17.58 3.08 2 7 0 -4 138.93 10.96 6 -7 0 4 145.51 11.02 5 -7 0 4 123.11 11.15 2 -6 0 4 22.98 2.53 2 6 0 -4 13.99 2.45 6 -6 0 4 12.29 2.34 5 -5 0 4 40.69 3.73 2 5 0 -4 37.15 3.93 6 -5 0 4 40.43 4.03 5 4 0 -4 686.64 49.64 6 -4 0 4 690.07 50.54 5 -4 0 4 647.28 50.81 2 -3 0 4 726.26 57.29 2 -3 0 4 765.54 57.04 5 3 0 -4 797.88 56.01 6 -2 0 4 2684.42 196.82 5 2 0 -4 2627.65 193.16 6 -1 0 4 683.15 51.50 5 1 0 -4 695.28 50.54 6 0 0 -4 9.66 1.67 6 1 0 4 32.42 3.33 5 -1 0 -4 34.00 3.33 6 -2 0 -4 570.80 40.99 6 -2 0 -4 540.09 42.39 1 2 0 4 562.54 41.82 5 -3 0 -4 370.64 27.53 6 3 0 4 379.97 28.20 5 -3 0 -4 366.18 28.72 1 -4 0 -4 103.20 8.82 1 4 0 4 100.24 8.30 5 5 0 4 117.97 9.68 5 -5 0 -4 119.45 10.27 1 6 0 4 39.25 3.78 5 -6 0 -4 23.97 4.02 1 -7 0 -4 94.98 9.42 1 7 0 4 112.94 8.94 5 -8 0 -4 56.61 6.13 1 8 0 4 49.74 5.35 5 -9 0 -4 24.34 4.31 1 -9 0 -4 25.03 4.08 3 9 0 4 33.27 3.93 5 10 0 4 63.09 6.21 5 -10 0 -4 64.04 6.52 3 -10 0 -4 61.06 6.96 1 11 0 4 42.80 5.29 5 -11 0 -4 54.52 6.26 1 -11 0 -4 55.97 6.08 3 -12 0 -4 17.23 4.17 1 12 0 4 34.80 4.10 5 -12 0 -4 21.07 4.11 3 -13 0 -4 1.17 2.80 3 -13 0 -4 4.46 2.75 1 13 0 4 3.00 2.42 5 -14 0 -4 47.45 6.35 1 14 0 4 47.02 5.82 5 15 0 4 3.17 2.67 5 -15 0 -4 -2.64 2.56 1 16 0 4 1.43 3.14 5 -16 0 -4 -2.70 3.33 1 -17 0 -4 15.84 4.87 1 17 0 4 6.91 3.90 5 18 0 4 7.40 4.49 5 -18 0 -4 8.54 4.49 1 -19 0 -4 28.86 7.09 1 22 1 -4 7.64 4.31 5 22 -1 -4 2.36 3.93 5 21 -1 -4 4.78 3.80 5 21 1 -4 0.97 3.62 6 20 -1 -4 -1.34 3.39 5 20 1 -4 8.45 3.55 6 19 1 -4 2.16 2.98 6 19 -1 -4 5.42 3.23 6 18 1 -4 12.79 3.48 6 18 -1 -4 15.14 3.94 6 17 -1 -4 -0.23 2.31 6 17 1 -4 1.00 2.43 6 -16 -1 4 3.59 2.89 2 16 1 -4 5.99 2.56 6 16 -1 -4 6.52 2.83 6 15 1 -4 32.61 4.83 6 15 -1 -4 26.23 4.69 6 -15 -1 4 39.08 5.93 2 14 1 -4 -0.41 1.85 6 -14 -1 4 0.39 2.22 2 14 -1 -4 0.79 1.87 6 -13 -1 4 5.97 2.88 2 13 -1 -4 4.98 2.35 6 13 1 -4 6.81 2.20 6 -12 -1 4 67.70 7.33 2 12 1 -4 73.14 6.76 6 12 -1 -4 60.19 6.62 6 11 -1 -4 0.59 2.08 6 11 1 -4 -1.25 1.71 6 -11 -1 4 0.42 2.06 2 -11 1 4 -0.46 2.05 5 -10 1 4 561.90 42.89 5 -10 -1 4 554.85 43.83 2 10 1 -4 584.41 42.22 6 10 -1 -4 561.55 42.44 6 -10 -1 4 560.28 42.58 5 9 -1 -4 11.66 2.82 6 -9 -1 4 21.64 3.43 2 9 1 -4 11.10 2.65 6 -9 -1 4 17.70 2.71 5 -9 1 4 12.91 2.62 5 8 -1 -4 192.34 16.36 6 8 1 -4 221.52 16.27 6 -8 -1 4 211.24 16.32 5 -8 -1 4 205.20 16.88 2 -8 1 4 215.13 16.60 5 -7 1 4 12.93 2.34 5 7 -1 -4 9.20 2.20 6 -7 -1 4 14.31 2.25 5 7 1 -4 13.21 2.33 6 -7 -1 4 5.41 1.94 2 -6 1 4 102.67 8.28 5 -6 -1 4 96.91 8.16 5 6 -1 -4 95.90 8.23 6 6 1 -4 98.32 8.08 6 5 1 -4 974.90 72.35 6 -5 1 4 975.53 73.76 5 5 -1 -4 994.12 72.48 6 -5 -1 4 1004.64 73.20 4 -5 -1 4 987.59 73.63 5 -4 -1 4 113.88 9.68 5 4 1 -4 142.82 9.65 6 4 -1 -4 118.68 9.62 6 -4 1 4 105.57 9.74 5 -3 1 4 1198.74 90.68 5 3 1 -4 1231.76 89.03 6 3 -1 -4 1231.11 89.03 6 -3 -1 4 1211.65 90.66 5 -2 1 4 4.98 1.55 5 2 -1 -4 8.73 1.22 4 -2 -1 4 7.60 1.75 5 2 1 -4 8.06 1.69 6 2 -1 -4 7.69 1.69 6 -1 1 4 128.76 10.52 5 1 1 -4 133.86 10.44 6 -1 -1 4 145.37 10.66 5 1 -1 -4 128.09 10.35 4 1 -1 -4 132.27 10.32 6 0 -1 4 20.09 2.54 5 0 1 -4 12.94 2.23 6 0 -1 -4 12.99 1.98 6 -1 -1 -4 2.26 1.26 6 -1 -1 -4 4.89 1.39 2 1 -1 4 4.90 1.56 5 -1 1 -4 1.96 1.47 6 -1 -1 -4 0.31 1.27 1 2 1 4 188.83 14.68 5 -2 -1 -4 192.88 15.28 1 2 -1 4 179.27 14.97 5 -2 1 -4 181.92 15.07 1 -2 -1 -4 215.27 15.26 2 -2 1 -4 191.68 14.65 6 -3 -1 -4 52.49 5.36 2 3 -1 4 56.34 5.19 5 -3 -1 -4 58.09 5.44 1 -3 1 -4 59.35 5.04 6 -3 1 -4 56.28 5.27 1 3 1 4 56.46 4.83 5 -4 -1 -4 618.35 48.37 1 4 1 4 625.70 47.31 5 -4 1 -4 652.17 46.68 6 -4 -1 -4 641.91 48.54 2 4 -1 4 632.05 47.69 5 4 1 4 656.79 46.47 6 -4 1 -4 603.91 48.17 1 5 -1 4 45.91 4.22 5 -5 1 -4 38.46 3.89 6 -5 -1 -4 33.19 4.20 1 5 1 4 37.09 3.72 6 5 1 4 35.90 3.61 5 -5 -1 -4 28.16 4.07 2 6 1 4 549.82 40.02 5 6 -1 4 537.11 40.49 5 -6 1 -4 557.37 41.14 1 6 1 4 517.82 39.28 6 -6 -1 -4 522.71 41.21 1 -6 1 -4 494.41 39.39 6 -6 -1 -4 546.41 41.49 2 -7 1 -4 66.67 6.00 1 -7 -1 -4 51.92 5.75 2 7 -1 4 47.49 5.26 5 7 1 4 44.59 4.98 5 -7 -1 -4 52.75 5.70 1 7 1 4 50.15 4.82 5 7 1 4 48.56 5.06 6 -8 1 -4 152.88 12.33 3 -8 -1 -4 155.59 13.12 1 8 -1 4 130.59 12.27 5 8 1 4 156.42 11.98 5 -8 1 -4 148.02 12.87 1 -8 -1 -4 145.30 13.15 2 9 -1 4 6.36 2.43 5 -9 -1 -4 3.59 2.32 3 -9 -1 -4 1.94 2.40 2 -9 1 -4 4.51 2.67 1 -9 -1 -4 -0.19 1.69 1 9 1 4 2.86 2.05 5 -9 1 -4 7.63 2.41 3 -10 -1 -4 39.34 5.41 3 10 -1 4 51.29 5.42 5 10 1 4 56.75 5.21 5 -10 -1 -4 44.25 5.83 1 -10 -1 -4 46.25 6.10 2 -10 1 -4 47.12 5.38 3 -10 1 -4 49.21 5.86 1 -11 -1 -4 6.60 2.79 1 -11 -1 -4 7.63 2.70 3 11 -1 4 13.34 3.02 5 -11 -1 -4 10.72 3.21 2 -11 1 -4 12.22 3.17 3 11 1 4 17.22 2.80 5 -11 1 -4 5.15 2.85 1 -12 -1 -4 0.99 2.43 1 -12 -1 -4 4.32 2.64 3 12 -1 4 5.40 2.45 5 12 1 4 0.36 1.96 5 -12 1 -4 2.51 2.48 1 13 1 4 9.18 2.80 5 -13 -1 -4 11.86 3.69 1 -13 1 -4 8.98 3.39 1 13 -1 4 13.44 3.44 5 -13 -1 -4 15.06 3.43 3 -14 -1 -4 1.14 2.72 1 -14 -1 -4 6.89 2.95 3 -14 1 -4 4.45 3.00 1 14 -1 4 -0.99 2.47 5 14 1 4 8.26 2.62 5 -15 1 -4 4.12 3.16 1 -15 -1 -4 5.44 3.45 1 15 1 4 4.53 2.83 5 15 -1 4 7.04 3.25 5 16 1 4 2.95 2.99 5 -16 1 -4 2.45 3.30 1 -16 -1 -4 -2.51 2.78 1 16 -1 4 2.62 3.13 5 -17 -1 -4 -0.79 3.21 1 17 -1 4 -3.28 3.73 5 -17 1 -4 4.87 4.17 1 -18 -1 -4 5.72 3.90 1 18 -1 4 6.35 4.02 5 -18 1 -4 4.39 4.46 1 -19 1 -4 -1.33 5.24 1 -19 -1 -4 -0.92 4.73 1 19 -1 4 2.38 4.60 5 22 -2 -4 5.49 4.43 5 21 -2 -4 -1.01 3.39 5 21 2 -4 0.95 3.71 6 20 -2 -4 -1.54 3.47 5 20 2 -4 0.04 3.09 6 19 -2 -4 -4.26 2.87 5 19 2 -4 3.50 2.93 6 18 2 -4 7.89 3.10 6 -18 -2 4 12.11 4.26 2 -17 -2 4 3.33 3.09 2 17 2 -4 0.95 2.63 6 17 -2 -4 4.36 2.62 6 -16 -2 4 11.63 3.69 2 16 -2 -4 1.70 2.51 6 16 2 -4 3.78 2.54 6 15 -2 -4 5.49 2.77 6 15 2 -4 9.86 2.81 6 -15 -2 4 7.77 3.01 2 14 2 -4 4.06 2.01 6 -14 -2 4 0.84 2.12 2 14 -2 -4 1.30 2.16 6 13 -2 -4 -4.35 1.62 6 13 2 -4 7.15 2.32 6 -13 -2 4 1.02 2.09 2 12 -2 -4 3.07 2.19 6 -12 -2 4 -2.01 1.95 2 12 2 -4 3.00 2.36 6 -11 2 4 30.62 4.28 5 -11 -2 4 34.90 4.48 2 11 2 -4 24.11 3.85 6 11 -2 -4 30.42 4.06 6 -10 -2 4 12.35 2.98 2 10 -2 -4 11.63 2.86 6 10 2 -4 10.91 2.53 6 -10 2 4 18.89 3.20 5 9 -2 -4 6.05 2.33 6 -9 -2 4 7.32 2.17 2 9 2 -4 4.52 1.98 6 -9 2 4 2.33 1.99 5 -8 -2 4 272.33 20.94 5 -8 2 4 263.59 21.40 5 -8 -2 4 284.28 21.12 4 8 -2 -4 258.06 21.08 6 8 2 -4 286.22 20.88 6 -7 2 4 24.41 3.15 5 -7 -2 4 22.52 2.70 4 7 -2 -4 19.59 3.21 6 7 2 -4 24.44 3.00 6 -7 -2 4 24.06 2.97 5 -6 -2 4 82.81 5.97 5 6 -2 -4 58.73 6.00 6 -6 2 4 71.68 6.13 5 6 2 -4 61.84 5.75 6 -6 -2 4 55.02 5.54 4 -5 2 4 119.51 10.62 5 5 2 -4 134.32 10.39 6 -5 -2 4 137.66 10.27 4 5 -2 -4 133.25 10.59 6 -5 -2 4 128.84 10.46 5 -4 2 4 399.18 31.17 5 4 -2 -4 408.30 30.67 6 -4 -2 4 424.54 31.09 5 4 2 -4 408.73 30.54 6 3 -2 -4 297.20 22.55 6 -3 2 4 298.59 22.96 5 -3 -2 4 305.90 22.91 5 3 2 -4 294.88 22.49 6 2 -2 -4 944.82 71.70 6 2 2 -4 964.00 71.77 6 -2 -2 4 1053.11 73.16 5 -2 2 4 955.40 73.05 5 1 -2 -4 21.64 2.61 6 -1 2 4 22.90 2.70 5 1 -2 -4 25.02 2.59 4 1 2 -4 22.17 2.71 6 -1 -2 4 20.23 2.90 5 0 -2 4 1230.51 87.47 5 0 2 -4 1146.80 85.76 6 0 -2 -4 1116.72 87.19 4 0 -2 -4 1211.33 85.49 6 0 2 4 1155.44 87.15 5 1 2 4 23.67 2.85 5 -1 -2 -4 34.11 3.38 4 -1 2 -4 24.75 3.16 6 1 -2 4 30.47 3.45 5 -1 -2 -4 30.11 3.32 1 -2 2 -4 62.39 5.68 6 2 2 4 68.23 5.35 5 2 2 4 55.14 5.21 6 -2 -2 -4 67.34 6.01 1 2 -2 4 66.51 5.92 5 3 -2 4 94.66 7.60 5 -3 2 -4 85.99 7.28 6 -3 2 -4 89.81 7.34 1 -3 -2 -4 82.32 7.63 1 3 2 4 90.12 6.85 5 3 2 4 82.01 6.69 6 -3 -2 -4 75.30 7.49 2 -4 -2 -4 59.80 5.96 1 4 -2 4 60.23 5.85 5 4 2 4 57.33 4.95 6 -4 2 -4 65.10 5.72 1 -4 -2 -4 70.84 6.06 2 4 2 4 53.88 5.07 5 -4 2 -4 61.08 5.67 6 -5 -2 -4 3.27 1.92 2 5 2 4 5.65 1.27 6 5 2 4 6.15 1.34 5 5 -2 4 8.64 2.33 5 -5 2 -4 7.04 1.88 1 -5 -2 -4 2.49 1.64 1 -5 2 -4 8.25 2.19 6 -6 2 -4 13.72 2.69 1 -6 -2 -4 11.37 2.70 1 -6 2 -4 11.24 2.50 6 6 2 4 11.27 1.73 6 -6 -2 -4 11.67 2.90 2 6 2 4 12.19 1.77 5 6 -2 4 10.93 2.73 5 7 2 4 22.34 2.43 5 -7 2 -4 24.83 3.34 6 7 -2 4 19.62 3.40 5 -7 2 -4 14.86 3.19 1 -7 -2 -4 17.40 3.49 1 -7 2 -4 19.35 2.83 3 -7 -2 -4 12.36 3.26 2 7 2 4 17.77 2.32 6 -8 2 -4 37.70 4.67 1 -8 -2 -4 35.36 4.61 2 -8 -2 -4 37.58 4.75 1 8 2 4 27.19 3.48 5 -8 2 -4 35.48 3.80 3 8 -2 4 30.97 4.55 5 -9 2 -4 5.57 2.15 3 9 -2 4 3.78 2.14 5 -9 -2 -4 6.11 2.54 1 9 2 4 5.12 1.93 5 -9 -2 -4 5.39 2.61 2 -9 -2 -4 4.10 2.43 3 -9 2 -4 6.94 2.73 1 -10 -2 -4 38.71 5.29 1 10 2 4 40.59 4.52 5 -10 2 -4 40.37 5.53 1 -10 -2 -4 45.43 5.69 2 10 -2 4 39.18 5.17 5 -10 -2 -4 47.68 5.45 3 -11 -2 -4 11.14 3.00 3 11 2 4 10.64 2.61 5 -11 -2 -4 12.19 3.62 2 11 -2 4 11.44 3.29 5 -11 -2 -4 7.78 3.26 1 -11 2 -4 11.97 3.26 1 -12 -2 -4 27.67 4.81 3 -12 -2 -4 27.47 5.32 2 12 -2 4 27.06 4.68 5 12 2 4 23.77 3.57 5 -12 2 -4 40.30 5.17 1 -12 -2 -4 28.28 5.19 1 13 2 4 1.47 2.23 5 -13 -2 -4 0.14 2.61 1 -13 -2 -4 3.14 2.96 2 13 -2 4 -2.25 2.25 5 -13 -2 -4 2.08 2.54 3 -13 2 -4 2.16 2.58 1 14 -2 4 7.43 3.35 5 -14 -2 -4 9.78 3.76 1 -14 -2 -4 15.45 4.49 2 14 2 4 11.47 2.91 5 -14 2 -4 16.48 4.15 1 -14 -2 -4 17.47 4.12 3 -15 -2 -4 -2.09 2.35 3 15 -2 4 8.98 3.33 5 -15 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + jpb25 started at 12:35:36 on 17-Sep-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL jpb25 in P2(1)/c CELL 0.71073 18.0097 11.2061 19.1506 90.000 117.162 90.000 ZERR 4.00 0.0018 0.0011 0.0020 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O SI CR UNIT 136 216 8 4 4 4 V = 3438.72 F(000) = 1272.0 Mu = 0.39 mm-1 Cell Wt = 2347.53 Rho = 1.134 TEMP -55 ACTA SIZE 0.20 0.20 0.15 OMIT -3 50 L.S. 5 BOND FMAP 2 PLAN 5 WGHT 0.059900 2.472700 FVAR 0.09599 O1 4 0.27785 1.01087 0.46502 11.00000 0.02937 0.01666 = 0.02414 -0.00276 0.01790 -0.00739 SI1 5 0.28176 0.95990 0.38292 11.00000 0.05352 0.04268 = 0.04259 -0.00063 0.02977 -0.00913 CR1 6 0.21945 0.84944 0.48089 11.00000 0.03461 0.02456 = 0.02987 0.00017 0.01720 -0.00148 N1 3 0.18957 0.67520 0.48967 11.00000 0.03836 0.02526 = 0.03010 -0.00005 0.01728 0.00264 N2 3 0.20924 0.88950 0.58175 11.00000 0.03364 0.02707 = 0.02886 0.00024 0.01506 0.00103 C1 1 0.14371 0.50188 0.54073 11.00000 0.08805 0.02886 = 0.05269 0.00341 0.04137 -0.00702 AFIX 33 H1A 2 0.15254 0.46041 0.50068 11.00000 -1.50000 H1B 2 0.08624 0.49159 0.53080 11.00000 -1.50000 H1C 2 0.18073 0.46936 0.59189 11.00000 -1.50000 AFIX 0 C2 1 0.16182 0.63338 0.53890 11.00000 0.04384 0.02740 = 0.03701 0.00375 0.02158 -0.00136 C3 1 0.15129 0.70275 0.59394 11.00000 0.04548 0.03311 = 0.03871 0.00384 0.02702 -0.00382 AFIX 43 H3A 2 0.12320 0.66550 0.61906 11.00000 -1.20000 AFIX 0 C4 1 0.17644 0.81901 0.61683 11.00000 0.03305 0.03306 = 0.02932 0.00014 0.01681 0.00308 C5 1 0.16891 0.86156 0.68749 11.00000 0.05341 0.04273 = 0.03983 -0.00005 0.02870 0.00166 AFIX 33 H5A 2 0.18787 0.94359 0.69869 11.00000 -1.50000 H5B 2 0.20291 0.81176 0.73220 11.00000 -1.50000 H5C 2 0.11106 0.85687 0.67732 11.00000 -1.50000 AFIX 0 C6 1 0.24510 0.99944 0.62116 11.00000 0.03893 0.02850 = 0.03025 -0.00340 0.01773 -0.00174 C7 1 0.19544 1.10166 0.60748 11.00000 0.04657 0.02847 = 0.03628 -0.00061 0.02206 0.00150 C8 1 0.23388 1.20658 0.64499 11.00000 0.05845 0.03021 = 0.04724 -0.00460 0.02487 0.00149 AFIX 43 H8A 2 0.20159 1.27595 0.63672 11.00000 -1.20000 AFIX 0 C9 1 0.31855 1.21123 0.69420 11.00000 0.05675 0.03651 = 0.05341 -0.01658 0.01803 -0.01203 AFIX 43 H9A 2 0.34356 1.28350 0.71845 11.00000 -1.20000 AFIX 0 C10 1 0.36598 1.11052 0.70761 11.00000 0.04137 0.04764 = 0.04930 -0.01098 0.00970 -0.00731 AFIX 43 H10A 2 0.42357 1.11432 0.74144 11.00000 -1.20000 AFIX 0 C11 1 0.33065 1.00247 0.67213 11.00000 0.03960 0.03719 = 0.03644 -0.00455 0.01061 -0.00075 C12 1 0.10277 1.09881 0.55189 11.00000 0.04143 0.03640 = 0.04701 -0.00074 0.02007 0.00596 AFIX 13 H12A 2 0.08441 1.01460 0.54688 11.00000 -1.20000 AFIX 0 C13 1 0.05089 1.17024 0.58229 11.00000 0.05447 0.06406 = 0.07625 -0.00937 0.02945 0.01841 AFIX 33 H13A 2 -0.00775 1.16441 0.54503 11.00000 -1.50000 H13B 2 0.06801 1.25324 0.58855 11.00000 -1.50000 H13C 2 0.05959 1.13826 0.63253 11.00000 -1.50000 AFIX 0 C14 1 0.08480 1.14224 0.47037 11.00000 0.04988 0.07641 = 0.05078 0.01077 0.01429 0.00619 AFIX 33 H14A 2 0.11693 1.09548 0.45109 11.00000 -1.50000 H14B 2 0.10026 1.22565 0.47299 11.00000 -1.50000 H14C 2 0.02578 1.13326 0.43509 11.00000 -1.50000 AFIX 0 C15 1 0.38422 0.89059 0.69108 11.00000 0.03597 0.04609 = 0.06174 -0.00299 0.00408 0.00714 AFIX 13 H15A 2 0.34846 0.82472 0.65866 11.00000 -1.20000 AFIX 0 C16 1 0.45632 0.90416 0.67136 11.00000 0.06058 0.07838 = 0.09040 -0.00081 0.03087 0.02273 AFIX 33 H16A 2 0.43501 0.92640 0.61663 11.00000 -1.50000 H16B 2 0.48616 0.82909 0.68062 11.00000 -1.50000 H16C 2 0.49393 0.96568 0.70423 11.00000 -1.50000 AFIX 0 C17 1 0.41685 0.85555 0.77700 11.00000 0.06959 0.08164 = 0.08967 0.03007 0.02314 0.01949 AFIX 33 H17A 2 0.37033 0.84667 0.78901 11.00000 -1.50000 H17B 2 0.45416 0.91712 0.81013 11.00000 -1.50000 H17C 2 0.44683 0.78057 0.78653 11.00000 -1.50000 AFIX 0 C18 1 0.20520 0.59016 0.44218 11.00000 0.05471 0.02025 = 0.03843 0.00371 0.02838 0.00333 C19 1 0.28810 0.55921 0.46319 11.00000 0.04333 C20 1 0.30411 0.47934 0.41599 11.00000 0.07529 0.04788 = 0.05559 0.00831 0.03921 0.02683 AFIX 43 H20A 2 0.35944 0.45833 0.42900 11.00000 -1.20000 AFIX 0 C21 1 0.23927 0.43094 0.35030 11.00000 0.09547 0.03944 = 0.05239 0.00054 0.04769 0.01623 AFIX 43 H21A 2 0.25048 0.37653 0.31895 11.00000 -1.20000 AFIX 0 C22 1 0.15879 0.46183 0.33064 11.00000 0.07615 0.03477 = 0.04076 -0.00338 0.03199 -0.00312 AFIX 43 H22A 2 0.11546 0.42765 0.28568 11.00000 -1.20000 AFIX 0 C23 1 0.13871 0.54193 0.37469 11.00000 0.05532 0.02616 = 0.03943 0.00083 0.02731 -0.00449 C24 1 0.35930 0.61296 0.53615 11.00000 0.04551 0.05297 = 0.05943 -0.00233 0.01968 0.01553 AFIX 13 H24A 2 0.34464 0.69757 0.53826 11.00000 -1.20000 AFIX 0 C25 1 0.44365 0.61273 0.53489 11.00000 0.05216 0.10207 = 0.09858 -0.00691 0.03447 0.01566 AFIX 33 H25A 2 0.48550 0.64886 0.58273 11.00000 -1.50000 H25B 2 0.43924 0.65793 0.48996 11.00000 -1.50000 H25C 2 0.45966 0.53123 0.53118 11.00000 -1.50000 AFIX 0 C26 1 0.36785 0.55451 0.61124 11.00000 0.06975 0.09787 = 0.05494 0.00490 0.01843 0.01971 AFIX 33 H26A 2 0.31430 0.55566 0.61186 11.00000 -1.50000 H26B 2 0.40849 0.59803 0.65627 11.00000 -1.50000 H26C 2 0.38622 0.47261 0.61343 11.00000 -1.50000 AFIX 0 C27 1 0.04883 0.57614 0.34896 11.00000 0.05019 0.04264 = 0.04418 -0.00751 0.02523 -0.01281 AFIX 13 H27A 2 0.04641 0.62180 0.39213 11.00000 -1.20000 AFIX 0 C28 1 -0.00867 0.46763 0.33163 11.00000 0.06995 0.06706 = 0.08362 0.00095 0.03335 -0.03031 AFIX 33 H28A 2 0.01113 0.41729 0.37786 11.00000 -1.50000 H28B 2 -0.00859 0.42261 0.28840 11.00000 -1.50000 H28C 2 -0.06496 0.49428 0.31767 11.00000 -1.50000 AFIX 0 C29 1 0.01529 0.65567 0.27653 11.00000 0.04682 0.07029 = 0.06889 0.01848 0.02285 -0.00068 AFIX 33 H29A 2 0.05060 0.72554 0.28706 11.00000 -1.50000 H29B 2 -0.04113 0.68041 0.26362 11.00000 -1.50000 H29C 2 0.01503 0.61174 0.23278 11.00000 -1.50000 AFIX 0 C30 1 0.21664 0.83315 0.36781 11.00000 0.07791 0.04498 = 0.03751 -0.00315 0.03275 -0.01693 AFIX 23 H30A 2 0.24181 0.75882 0.36177 11.00000 -1.20000 H30B 2 0.16061 0.84329 0.32412 11.00000 -1.20000 AFIX 0 C31 1 0.24487 1.08313 0.30924 11.00000 0.10458 0.06783 = 0.05516 0.01198 0.03197 -0.02421 AFIX 33 H31A 2 0.28423 1.09422 0.28820 11.00000 -1.50000 H31B 2 0.24066 1.15631 0.33425 11.00000 -1.50000 H31C 2 0.19054 1.06290 0.26696 11.00000 -1.50000 AFIX 0 C32 1 0.39253 0.92313 0.40934 11.00000 0.07170 0.09095 = 0.11156 -0.01689 0.05775 -0.00361 AFIX 33 H32A 2 0.40870 0.96365 0.37362 11.00000 -1.50000 H32B 2 0.39815 0.83762 0.40549 11.00000 -1.50000 H32C 2 0.42829 0.94903 0.46265 11.00000 -1.50000 AFIX 0 C33 1 0.29367 1.13426 0.49053 11.00000 0.07040 0.03696 = 0.06465 -0.00427 0.04130 -0.00937 AFIX 23 H33A 2 0.28168 1.14486 0.53518 11.00000 -1.20000 H33B 2 0.25519 1.18546 0.44785 11.00000 -1.20000 AFIX 0 C34 1 0.38071 1.17420 0.51396 11.00000 0.07397 0.05290 = 0.09362 -0.01037 0.03868 -0.02607 AFIX 33 H34A 2 0.38669 1.25722 0.52997 11.00000 -1.50000 H34B 2 0.39287 1.16566 0.46982 11.00000 -1.50000 H34C 2 0.41927 1.12575 0.55736 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for jpb25 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CR 1.240 O1 - C33 Si1 Cr1 Si1 - O1 C30 C31 C32 Cr1 Cr1 - N1 N2 C30 O1 Si1 N1 - C2 C18 Cr1 N2 - C4 C6 Cr1 C1 - C2 C2 - N1 C3 C1 C3 - C4 C2 C4 - N2 C3 C5 C5 - C4 C6 - C11 C7 N2 C7 - C8 C6 C12 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C10 C6 C15 C12 - C7 C14 C13 C13 - C12 C14 - C12 C15 - C16 C11 C17 C16 - C15 C17 - C15 C18 - C19 C23 N1 C19 - C20 C18 C24 C20 - C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C22 C18 C27 C24 - C26 C19 C25 C25 - C24 C26 - C24 C27 - C23 C29 C28 C28 - C27 C29 - C27 C30 - Si1 Cr1 C31 - Si1 C32 - Si1 C33 - O1 C34 C34 - C33 h k l Fo^2 Sigma Why rejected 0 0 1 0.19 0.04 observed but should be systematically absent 1 0 1 0.23 0.04 observed but should be systematically absent 2 0 5 1.35 0.20 observed but should be systematically absent 25935 Reflections read, of which 5450 rejected -20 =< h =< 21, -12 =< k =< 13, -22 =< l =< 22, Max. 2-theta = 50.00 3 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 4 0 1.16 0.09 4 0.65 -6 12 2 11.45 0.58 3 4.51 -7 6 3 3.25 0.20 4 1.08 -6 0 10 12.33 0.71 2 3.90 4 Inconsistent equivalents 6059 Unique reflections, of which 0 suppressed R(int) = 0.0570 R(sigma) = 0.0701 Friedel opposites merged Maximum memory for data reduction = 3990 / 61237 Default effective X-H distances for T = -55.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.99 0.98 0.97 0.94 0.87 0.90 1.11 0.83 0.94 0.87 0.94 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 = 5123 / 440745 wR2 = 0.1631 before cycle 1 for 6059 data and 347 / 347 parameters GooF = S = 1.138; Restrained GooF = 1.138 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0599 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09549 0.00021 -2.445 OSF 5 0.04047 0.00109 10.169 U11 O1 6 0.02674 0.00103 9.780 U22 O1 7 0.03511 0.00113 9.680 U33 O1 9 0.02302 0.00092 5.576 U13 O1 Mean shift/esd = 0.312 Maximum = 10.169 for U11 O1 Max. shift = 0.006 A for C31 Max. dU = 0.011 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5123 / 440745 wR2 = 0.1473 before cycle 2 for 6059 data and 347 / 347 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0599 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09557 0.00019 0.459 OSF 5 0.04649 0.00117 5.146 U11 O1 6 0.03146 0.00110 4.290 U22 O1 7 0.04054 0.00122 4.458 U33 O1 Mean shift/esd = 0.108 Maximum = 5.146 for U11 O1 Max. shift = 0.002 A for H31A Max. dU = 0.005 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5123 / 440745 wR2 = 0.1455 before cycle 3 for 6059 data and 347 / 347 parameters GooF = S = 1.006; Restrained GooF = 1.006 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0599 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09557 0.00018 -0.006 OSF Mean shift/esd = 0.021 Maximum = 0.407 for U11 O1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5123 / 440745 wR2 = 0.1455 before cycle 4 for 6059 data and 347 / 347 parameters GooF = S = 1.006; Restrained GooF = 1.006 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0599 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09557 0.00018 0.003 OSF Mean shift/esd = 0.004 Maximum = -0.029 for x C28 Max. shift = 0.000 A for H28C Max. dU = 0.000 for C15 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5123 / 440745 wR2 = 0.1455 before cycle 5 for 6059 data and 347 / 347 parameters GooF = S = 1.006; Restrained GooF = 1.006 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0599 * P )^2 + 2.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09557 0.00018 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.002 for z C31 Max. shift = 0.000 A for H31A Max. dU = 0.000 for C21 Largest correlation matrix elements 0.647 U13 C21 / U33 C21 0.586 U13 C33 / U33 C33 0.569 U13 C1 / U11 C1 0.644 U13 C32 / U33 C32 0.582 U13 Si1 / U11 Si1 0.568 U13 C5 / U11 C5 0.625 U13 C32 / U11 C32 0.581 U13 C20 / U11 C20 0.567 U13 C23 / U33 C23 0.617 U13 C21 / U11 C21 0.581 U13 Cr1 / U33 Cr1 0.566 U13 O1 / U33 O1 0.603 U13 C20 / U33 C20 0.581 U13 C18 / U33 C18 0.561 U13 C3 / U11 C3 0.596 U13 Si1 / U33 Si1 0.579 U13 C3 / U33 C3 0.559 U13 C18 / U11 C18 0.592 U13 C1 / U33 C1 0.578 U13 C30 / U33 C30 0.556 U13 Cr1 / U11 Cr1 0.590 U13 C33 / U11 C33 0.577 U13 C5 / U33 C5 0.555 U13 C30 / U11 C30 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.1525 0.4604 0.5006 33 0.970 0.000 C1 C2 H1A H1B 0.0861 0.4916 0.5306 33 0.970 0.000 C1 C 12 9 -6 4.21 0.54 -12 9 6 3.43 0.66 11 9 -6 4.98 0.62 11 -9 -6 4.38 0.76 -11 9 6 6.10 0.75 10 9 -6 4.97 0.60 -10 9 6 5.15 0.76 10 -9 -6 3.96 0.71 9 9 -6 13.22 1.21 -9 9 6 13.29 1.30 9 -9 -6 13.67 1.29 -8 9 6 2.63 0.51 8 9 -6 1.75 0.39 -7 9 6 15.49 1.46 7 9 -6 15.56 1.37 6 9 -6 1.43 0.37 -6 9 6 0.86 0.35 -5 9 6 9.29 0.94 5 9 -6 8.02 0.89 4 9 -6 0.86 0.37 -4 9 6 0.44 0.33 -3 9 6 5.23 0.63 2 9 -6 3.27 0.57 -2 9 6 2.71 0.49 -1 9 6 2.49 0.49 1 9 -6 3.74 0.61 0 -9 6 2.69 0.54 0 9 -6 2.76 0.56 0 9 6 2.22 0.44 -1 9 -6 5.50 0.73 1 -9 6 5.30 0.73 1 9 6 5.72 0.65 2 -9 6 -0.46 0.32 -2 9 -6 -0.50 0.29 2 9 6 0.34 0.24 -3 9 -6 3.36 0.63 3 9 6 3.73 0.52 3 -9 6 3.08 0.62 -4 -9 -6 10.33 1.03 4 9 6 9.51 0.93 -4 9 -6 10.59 1.08 4 -9 6 9.51 1.12 5 -9 6 2.95 0.63 -5 9 -6 2.75 0.63 -5 -9 -6 4.09 0.61 5 9 6 3.12 0.47 -6 9 -6 9.22 1.08 6 9 6 9.45 0.93 -6 -9 -6 12.36 1.09 6 -9 6 9.61 1.16 7 -9 6 2.56 0.65 -7 -9 -6 2.32 0.49 -7 -9 -6 2.02 0.51 -8 -9 -6 4.50 0.67 8 -9 6 4.10 0.76 -8 -9 -6 2.68 0.59 -8 -9 -6 2.13 0.57 -9 -9 -6 3.93 0.69 -9 -9 -6 3.86 0.69 -9 -9 -6 2.93 0.62 9 -9 6 4.35 0.87 -10 -9 -6 1.87 0.56 -10 -9 -6 1.04 0.51 -10 -9 -6 1.40 0.47 10 -9 6 2.17 0.71 -11 -9 -6 2.71 0.70 -11 -9 -6 2.62 0.70 -11 -9 -6 3.13 0.70 -11 -9 -6 3.09 0.69 11 -9 6 2.97 0.85 -12 -9 -6 0.17 0.51 -12 -9 -6 0.62 0.49 -12 -9 -6 0.24 0.51 -12 -9 -6 0.51 0.53 12 -9 6 0.55 0.72 -13 -9 -6 -0.36 0.46 13 -9 6 0.42 0.79 -13 -9 -6 0.31 0.58 17 -10 -6 -0.47 0.72 16 -10 -6 0.89 0.67 15 10 -6 1.00 0.43 15 -10 -6 2.07 0.74 14 -10 -6 0.39 0.57 14 10 -6 0.29 0.38 13 -10 -6 2.85 0.69 -13 10 6 3.57 0.75 13 10 -6 2.64 0.52 12 10 -6 -0.24 0.28 12 -10 -6 -0.06 0.41 -12 10 6 1.11 0.49 11 10 -6 3.04 0.56 -11 10 6 4.03 0.72 10 10 -6 0.74 0.35 -10 10 6 0.60 0.43 9 10 -6 1.69 0.42 -9 10 6 1.96 0.53 -8 10 6 5.55 0.75 8 10 -6 5.86 0.69 -7 10 6 1.43 0.44 7 10 -6 1.93 0.41 6 10 -6 5.30 0.66 -6 10 6 4.16 0.70 -5 10 6 7.96 0.89 5 10 -6 6.61 0.81 4 10 -6 1.19 0.42 -4 10 6 0.89 0.41 -3 10 6 21.31 1.86 3 10 -6 21.30 1.86 -2 10 6 4.86 0.64 2 10 -6 4.60 0.73 -1 10 6 3.97 0.59 1 10 -6 2.82 0.61 0 10 -6 8.12 0.90 0 10 6 6.86 0.80 -1 10 -6 2.99 0.63 1 10 6 2.75 0.51 2 10 6 8.67 0.88 -2 10 -6 8.18 0.97 -3 10 -6 3.35 0.67 3 -10 6 3.26 0.66 3 10 6 1.95 0.45 4 -10 6 1.00 0.49 4 10 6 0.92 0.33 -4 10 -6 0.31 0.45 -5 10 -6 3.79 0.71 5 10 6 3.63 0.52 5 -10 6 2.54 0.68 -6 -10 -6 2.08 0.55 6 -10 6 2.87 0.69 6 10 6 1.94 0.40 -6 10 -6 1.37 0.58 -7 -10 -6 3.35 0.66 -7 -10 -6 4.06 0.69 7 -10 6 3.52 0.78 8 -10 6 5.97 1.02 -8 -10 -6 4.84 0.81 -8 -10 -6 4.84 0.81 -9 -10 -6 0.83 0.42 9 -10 6 1.05 0.72 -9 -10 -6 1.10 0.53 -10 -10 -6 4.08 0.79 10 -10 6 4.17 1.01 -10 -10 -6 4.69 0.79 -10 -10 -6 5.58 0.89 11 -10 6 0.25 0.75 -11 -10 -6 -0.72 0.47 -11 -10 -6 -0.08 0.47 -11 -10 -6 -0.22 0.34 -11 -10 -6 -0.04 0.49 -12 -10 -6 0.83 0.63 -12 -10 -6 1.94 0.68 16 -11 -6 0.46 0.79 15 11 -6 2.10 0.57 15 -11 -6 1.53 0.77 14 11 -6 1.04 0.44 -13 11 6 1.94 0.69 13 11 -6 0.81 0.44 12 11 -6 5.60 0.77 -12 11 6 4.04 0.86 11 11 -6 0.88 0.37 -11 11 6 0.00 0.49 10 11 -6 4.23 0.65 -10 11 6 2.67 0.67 -9 11 6 -0.71 0.36 9 11 -6 -0.30 0.29 8 11 -6 0.23 0.33 -8 11 6 0.43 0.42 -7 11 6 -0.41 0.35 7 11 -6 0.07 0.32 -6 11 6 0.07 0.38 6 11 -6 0.58 0.35 -5 11 6 4.05 0.71 5 11 -6 5.12 0.75 4 11 -6 0.02 0.39 -4 11 6 1.03 0.44 -3 11 6 6.39 0.80 3 11 -6 6.26 0.90 -2 11 6 0.85 0.38 2 11 -6 0.82 0.45 -1 11 6 4.10 0.65 1 11 -6 4.07 0.73 0 11 -6 7.16 0.90 0 11 6 5.81 0.77 1 11 6 4.64 0.73 -1 11 -6 6.58 0.84 2 11 6 10.50 1.11 -2 11 -6 12.67 1.29 -3 11 -6 2.00 0.57 3 11 6 0.83 0.39 -4 11 -6 7.94 1.01 4 11 6 6.37 0.79 -5 11 -6 0.82 0.53 -5 -11 -6 -0.21 0.31 5 -11 6 0.93 0.57 5 11 6 0.73 0.36 -6 -11 -6 2.74 0.60 -6 11 -6 2.77 0.77 6 11 6 2.81 0.53 6 -11 6 2.89 0.77 7 -11 6 0.27 0.65 -7 -11 -6 0.38 0.36 8 -11 6 1.13 0.71 -8 -11 -6 1.31 0.46 -9 -11 -6 0.42 0.35 9 -11 6 0.22 0.70 -10 -11 -6 0.78 0.47 10 -11 6 0.15 0.74 14 12 -6 0.40 0.48 13 12 -6 -0.28 0.35 -13 12 6 -0.13 0.62 12 12 -6 2.88 0.57 -12 12 6 1.71 0.74 11 12 -6 0.80 0.45 -11 12 6 1.03 0.63 -10 12 6 0.93 0.65 10 12 -6 0.31 0.44 -9 12 6 -0.35 0.47 9 12 -6 0.05 0.38 -8 12 6 0.33 0.51 8 12 -6 0.23 0.35 7 12 -6 0.55 0.41 -7 12 6 1.54 0.59 -6 12 6 -0.17 0.39 6 12 -6 0.01 0.34 -5 12 6 0.02 0.45 5 12 -6 0.45 0.40 4 12 -6 -0.07 0.48 -4 12 6 0.33 0.47 -3 12 6 0.45 0.40 3 12 -6 1.56 0.59 -2 12 6 -0.52 0.31 2 12 -6 -0.06 0.47 -1 12 6 4.18 0.76 1 12 -6 6.61 0.99 0 12 -6 0.45 0.48 0 12 6 0.24 0.36 1 12 6 4.10 0.68 -1 12 -6 4.35 0.86 2 12 6 0.86 0.42 -2 12 -6 1.09 0.62 -3 12 -6 2.76 0.79 3 12 6 2.15 0.56 -3 -12 -6 3.13 0.61 -4 -12 -6 0.38 0.41 4 12 6 0.20 0.36 -4 12 -6 0.29 0.61 5 12 6 -0.22 0.38 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6.22 4.23 6 21 -4 -7 0.44 3.42 5 -20 -4 7 0.84 4.03 2 20 4 -7 0.18 3.31 6 20 -4 -7 -3.24 3.25 5 19 4 -7 -4.51 2.60 6 -19 -4 7 -0.76 3.04 2 19 -4 -7 2.86 4.75 6 18 4 -7 6.94 3.11 6 18 -4 -7 8.81 5.15 6 -18 -4 7 9.60 3.91 2 17 -4 -7 3.87 3.52 6 -17 -4 7 3.76 2.93 2 17 4 -7 2.28 2.63 6 16 4 -7 20.51 3.90 6 16 -4 -7 20.50 4.87 6 -16 -4 7 13.51 4.04 2 15 4 -7 8.09 2.90 6 15 -4 -7 5.25 3.53 6 -15 -4 7 8.38 3.41 2 14 4 -7 9.48 3.22 6 -14 -4 7 11.72 3.45 2 14 -4 -7 14.06 4.19 6 -13 -4 7 15.40 3.52 2 -13 -4 7 12.52 3.12 4 13 4 -7 11.62 3.06 6 13 -4 -7 16.25 4.04 6 -13 4 7 14.89 4.08 5 12 -4 -7 377.00 32.86 6 -12 -4 7 479.40 32.82 4 -12 4 7 422.83 33.43 5 12 4 -7 412.30 32.42 6 -11 4 7 7.51 3.55 5 11 -4 -7 17.18 3.78 6 -11 -4 7 17.44 3.09 4 11 4 -7 12.18 2.84 6 10 -4 -7 392.42 31.07 6 10 4 -7 401.15 30.68 6 -10 4 7 407.33 31.61 5 -9 4 7 23.17 4.18 5 9 4 -7 18.39 3.70 6 9 -4 -7 27.84 4.42 6 8 -4 -7 16.49 3.26 6 -8 -4 7 15.51 3.14 5 -8 4 7 11.36 3.08 5 8 4 -7 16.24 3.20 6 -7 -4 7 23.81 3.61 5 7 -4 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-3.55 4.00 5 15 -7 -9 111.85 11.93 5 15 7 -9 109.04 10.64 6 -14 7 9 15.56 4.72 5 14 7 -9 10.72 3.41 6 13 7 -9 154.14 14.27 6 -13 7 9 173.10 15.46 5 -12 7 9 28.05 5.98 5 12 7 -9 33.45 5.42 6 12 -7 -9 34.81 5.89 6 11 -7 -9 39.95 6.45 6 -11 7 9 46.07 6.71 5 11 7 -9 40.61 5.38 6 10 -7 -9 57.09 7.16 6 -10 7 9 52.42 7.65 5 10 7 -9 59.22 6.66 6 9 7 -9 9.34 3.32 6 9 -7 -9 8.94 3.46 6 -9 7 9 5.65 3.37 5 8 7 -9 93.60 8.73 6 -8 7 9 80.54 8.83 5 8 -7 -9 75.97 8.60 6 -7 7 9 1.89 2.96 5 7 7 -9 5.80 3.09 6 6 7 -9 99.63 9.86 6 -6 7 9 98.80 10.03 5 -5 7 9 13.42 3.94 5 5 7 -9 18.88 4.39 6 -5 -7 9 19.24 4.25 5 -4 -7 9 48.10 6.61 5 4 7 -9 44.28 6.74 6 -4 7 9 58.92 6.41 5 -3 7 9 4.70 2.72 5 -3 -7 9 11.58 3.94 5 3 7 -9 10.40 3.63 6 -2 -7 9 151.53 13.82 5 2 7 -9 149.97 13.38 6 -2 7 9 146.49 13.15 5 -1 7 9 317.58 24.67 5 -1 -7 9 240.61 24.81 5 1 7 -9 359.68 25.15 6 0 7 9 4.91 2.67 5 0 7 -9 5.28 3.44 6 0 -7 9 5.28 3.85 5 1 7 9 380.34 29.61 5 -1 7 -9 351.30 29.74 6 1 -7 9 418.40 30.98 5 -1 -7 -9 354.58 30.13 4 -2 7 -9 11.82 4.18 6 2 -7 9 12.03 4.55 5 2 7 9 5.48 2.62 5 -2 -7 -9 3.84 2.86 4 -3 -7 -9 162.75 14.02 4 3 -7 9 157.63 14.66 5 3 7 9 149.55 12.94 5 -3 7 -9 140.06 13.75 6 4 -7 9 12.75 4.47 5 -4 -7 -9 14.13 4.08 4 -4 7 -9 17.15 4.90 6 4 7 9 17.91 3.42 5 -5 -7 -9 35.56 5.84 4 5 7 9 34.81 4.24 5 5 -7 9 30.33 6.21 5 -6 -7 -9 4.81 3.54 1 -6 -7 -9 11.62 3.67 4 6 7 9 10.13 2.73 5 6 -7 9 5.81 4.50 5 -7 -7 -9 20.64 5.21 1 -7 -7 -9 19.17 4.58 2 -7 -7 -9 22.61 4.98 4 7 -7 9 8.72 5.13 5 8 -7 9 4.13 4.80 5 -8 -7 -9 3.91 3.38 1 -8 -7 -9 -0.37 3.00 4 -8 -7 -9 -2.26 2.73 2 9 -7 9 1.81 4.87 5 -9 -7 -9 5.47 3.52 4 -9 -7 -9 0.93 3.26 2 -9 -7 -9 8.47 4.64 1 -10 -7 -9 -1.34 2.93 4 -10 -7 -9 2.63 4.01 2 10 -7 9 -1.04 5.25 5 -10 -7 -9 1.97 4.49 1 11 -7 9 -0.66 5.60 5 -11 -7 -9 -2.88 3.52 4 -11 -7 -9 2.38 4.57 2 -11 -7 -9 -0.02 4.40 1 -11 -7 -9 -0.42 3.56 3 12 -7 9 15.98 7.47 5 -12 -7 -9 34.71 7.12 2 -12 -7 -9 15.34 6.37 4 -12 -7 -9 18.17 6.02 3 -12 -7 -9 18.98 6.91 1 -13 -7 -9 -0.84 5.35 2 -20 -8 9 8.54 6.01 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11 32.98 4.87 5 0 -7 -11 6.65 3.03 4 0 7 -11 15.34 4.44 6 0 7 11 10.75 3.13 5 0 -7 11 4.70 3.77 5 -1 -7 -11 76.47 8.25 4 -1 7 -11 76.49 8.86 6 1 7 11 88.71 8.10 5 1 -7 11 68.52 8.96 5 -2 7 -11 0.77 3.40 6 2 -7 11 1.62 3.30 5 2 7 11 -1.57 2.47 5 -2 -7 -11 7.27 3.09 4 -3 -7 -11 76.52 8.73 4 3 -7 11 88.52 10.09 5 3 7 11 75.59 7.96 5 -4 -7 -11 27.25 5.03 2 -4 -7 -11 24.76 5.17 4 4 -7 11 30.81 6.31 5 4 7 11 16.93 3.95 5 -5 -7 -11 11.39 3.95 2 -5 -7 -11 15.32 4.41 4 5 -7 11 17.73 5.33 5 5 7 11 17.71 3.39 5 6 -7 11 21.66 6.28 5 -6 -7 -11 20.62 4.84 4 -6 -7 -11 25.15 5.13 2 -7 -7 -11 2.86 3.46 4 7 -7 11 -3.23 4.96 5 -7 -7 -11 8.04 3.76 2 -8 -7 -11 11.54 4.98 4 8 -7 11 18.03 6.90 5 -8 -7 -11 17.49 5.06 2 -9 -7 -11 11.02 4.54 4 -9 -7 -11 5.32 4.63 2 9 -7 11 -3.61 5.77 5 -10 -7 -11 10.34 5.21 2 10 -7 11 6.77 6.80 5 -10 -7 -11 3.13 3.73 4 -11 -7 -11 0.57 4.58 3 -11 -7 -11 0.36 5.59 2 -20 -8 11 6.41 5.50 2 20 8 -11 17.84 6.25 6 19 -8 -11 0.31 6.85 5 -19 -8 11 4.85 4.95 2 19 8 -11 4.88 4.45 6 18 -8 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