ࡱ> M -bjbj== lWW%lT dG+ZZZZZZZZ*******$A, a.*EZZZZZ*2*ZZ+2*2*2*Z>ZZ*2*Z*2*d2***ZN 0 **+0G+*.2*.*2*  Table 1. Crystal data and structure refinement for jpb26. Identification code jpb26 Empirical formula C31 H51 Cr N2 O2 Si2 Formula weight 591.92 Temperature 147(2) K Wavelength 0.71073 Crystal system Monoclinic Space group P2(1)/c Unit cell dimensions a = 11.1209(9) a= 90. b = 10.6695(9) b= 90.398(2). c = 28.046(2) g = 90. Volume 3327.7(5) 3 Z 4 Density (calculated) 1.181 Mg/m3 Absorption coefficient 0.444 mm-1 F(000) 1276 Crystal size 0.45 x 0.20 x 0.05 mm3 Theta range for data collection 1.83 to 23.00. Index ranges -12<=h<=12, -10<=k<=11, -28<=l<=30 Reflections collected 13964 Independent reflections 4628 [R(int) = 0.0625] Completeness to theta = 23.00 100.0 % Absorption correction None Max. and min. transmission 0.9781 and 0.8253 Refinement method Full-matrix least-squares on F2 Data / restraints / parameters 4628 / 0 / 343 Goodness-of-fit on F2 1.015 Final R indices [I>2sigma(I)] R1 = 0.0650, wR2 = 0.1494 R indices (all data) R1 = 0.1023, wR2 = 0.1636 Largest diff. peak and hole 0.555 and -0.421 e.-3 Table 2. Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (2x 103) for jpb26. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Cr(1) 8065(1) 6816(1) 1135(1) 19(1) Si(1) 10624(1) 7007(1) 1206(1) 24(1) Si(2) 6666(1) 8144(2) 2092(1) 31(1) O(1) 9595(3) 6104(3) 1499(1) 26(1) O(2) 7192(4) 7264(4) 2532(1) 43(1) N(1) 7169(4) 5106(4) 1156(1) 18(1) N(2) 6812(4) 7438(4) 669(1) 20(1) C(1) 6060(5) 4881(5) 988(2) 23(1) C(2) 5368(5) 5780(5) 754(2) 26(1) C(3) 5730(5) 6946(5) 585(2) 28(1) C(4) 5495(5) 3590(5) 1024(2) 34(2) C(5) 4830(5) 7639(6) 273(2) 37(2) C(6) 7133(5) 8526(5) 381(2) 23(1) C(7) 6911(5) 9751(5) 534(2) 25(1) C(8) 7389(5) 10727(5) 267(2) 30(1) C(9) 7994(5) 10519(6) -151(2) 36(2) C(10) 8119(5) 9308(5) -316(2) 29(1) C(11) 7694(5) 8300(5) -57(2) 26(1) C(12) 6143(6) 10065(5) 958(2) 38(2) C(13) 7813(5) 6990(5) -251(2) 33(1) C(14) 7803(4) 4000(5) 1313(2) 23(1) C(15) 8571(5) 3406(5) 988(2) 26(1) C(16) 9180(5) 2324(6) 1128(2) 39(2) C(17) 9031(5) 1850(6) 1579(2) 44(2) C(18) 8288(5) 2443(6) 1899(2) 36(2) C(19) 7678(5) 3526(5) 1772(2) 24(1) C(20) 8724(5) 3908(6) 494(2) 37(2) C(21) 6835(5) 4126(5) 2125(2) 34(2) C(22) 9541(4) 7727(5) 809(2) 25(1) C(23) 11420(5) 8041(6) 1639(2) 41(2) C(24) 11737(5) 5939(6) 929(2) 50(2) C(25) 9688(6) 5773(6) 2015(2) 48(2) C(26) 10580(6) 4788(7) 2079(3) 68(2) C(27) 7897(5) 8186(5) 1651(2) 29(1) C(28) 6295(6) 9742(6) 2325(2) 47(2) C(29) 5224(5) 7460(6) 1878(2) 37(2) C(30) 6582(7) 7113(8) 2965(2) 68(2) C(31) 7281(8) 6630(10) 3344(3) 98(3) ________________________________________________________________________________ Table 3. Bond lengths [] and angles [] for jpb26. _____________________________________________________ Cr(1)-N(2) 2.017(4) Cr(1)-C(27) 2.066(5) Cr(1)-N(1) 2.080(4) Cr(1)-O(1) 2.119(4) Cr(1)-C(22) 2.120(5) Cr(1)-Si(1) 2.8588(17) Si(1)-O(1) 1.711(4) Si(1)-C(22) 1.806(5) Si(1)-C(24) 1.856(6) Si(1)-C(23) 1.860(6) Si(2)-O(2) 1.654(4) Si(2)-C(27) 1.853(5) Si(2)-C(29) 1.858(6) Si(2)-C(28) 1.873(6) O(1)-C(25) 1.491(7) O(2)-C(30) 1.404(7) N(1)-C(1) 1.339(6) N(1)-C(14) 1.441(6) N(2)-C(3) 1.333(7) N(2)-C(6) 1.459(6) C(1)-C(2) 1.391(7) C(1)-C(4) 1.518(7) C(2)-C(3) 1.391(7) C(3)-C(5) 1.517(7) C(6)-C(7) 1.398(7) C(6)-C(11) 1.403(7) C(7)-C(8) 1.390(7) C(7)-C(12) 1.508(7) C(8)-C(9) 1.374(7) C(9)-C(10) 1.379(8) C(10)-C(11) 1.383(7) C(11)-C(13) 1.506(7) C(14)-C(19) 1.393(7) C(14)-C(15) 1.405(7) C(15)-C(16) 1.394(8) C(15)-C(20) 1.495(7) C(16)-C(17) 1.373(8) C(17)-C(18) 1.378(8) C(18)-C(19) 1.385(8) C(19)-C(21) 1.511(7) C(25)-C(26) 1.456(9) C(30)-C(31) 1.411(9) N(2)-Cr(1)-C(27) 98.9(2) N(2)-Cr(1)-N(1) 88.79(17) C(27)-Cr(1)-N(1) 123.66(19) N(2)-Cr(1)-O(1) 168.36(15) C(27)-Cr(1)-O(1) 89.54(18) N(1)-Cr(1)-O(1) 93.15(15) N(2)-Cr(1)-C(22) 95.93(18) C(27)-Cr(1)-C(22) 92.9(2) N(1)-Cr(1)-C(22) 141.97(18) O(1)-Cr(1)-C(22) 75.56(16) N(2)-Cr(1)-Si(1) 134.82(12) C(27)-Cr(1)-Si(1) 89.75(15) N(1)-Cr(1)-Si(1) 122.51(12) O(1)-Cr(1)-Si(1) 36.52(9) C(22)-Cr(1)-Si(1) 39.10(14) O(1)-Si(1)-C(22) 95.2(2) O(1)-Si(1)-C(24) 107.8(3) C(22)-Si(1)-C(24) 116.5(3) O(1)-Si(1)-C(23) 109.7(2) C(22)-Si(1)-C(23) 117.5(3) C(24)-Si(1)-C(23) 108.8(3) O(1)-Si(1)-Cr(1) 47.51(12) C(22)-Si(1)-Cr(1) 47.78(15) C(24)-Si(1)-Cr(1) 126.4(2) C(23)-Si(1)-Cr(1) 123.8(2) O(2)-Si(2)-C(27) 104.7(2) O(2)-Si(2)-C(29) 108.5(3) C(27)-Si(2)-C(29) 115.7(2) O(2)-Si(2)-C(28) 109.5(3) C(27)-Si(2)-C(28) 112.1(3) C(29)-Si(2)-C(28) 106.2(3) C(25)-O(1)-Si(1) 123.9(3) C(25)-O(1)-Cr(1) 127.0(3) Si(1)-O(1)-Cr(1) 95.97(16) C(30)-O(2)-Si(2) 122.7(4) C(1)-N(1)-C(14) 114.1(4) C(1)-N(1)-Cr(1) 125.9(3) C(14)-N(1)-Cr(1) 119.6(3) C(3)-N(2)-C(6) 116.1(4) C(3)-N(2)-Cr(1) 127.1(4) C(6)-N(2)-Cr(1) 116.7(3) N(1)-C(1)-C(2) 123.3(5) N(1)-C(1)-C(4) 121.3(5) C(2)-C(1)-C(4) 115.4(5) C(3)-C(2)-C(1) 128.0(5) N(2)-C(3)-C(2) 123.8(5) N(2)-C(3)-C(5) 120.0(5) C(2)-C(3)-C(5) 116.1(5) C(7)-C(6)-C(11) 120.7(5) C(7)-C(6)-N(2) 122.0(4) C(11)-C(6)-N(2) 117.3(5) C(8)-C(7)-C(6) 117.8(5) C(8)-C(7)-C(12) 118.6(5) C(6)-C(7)-C(12) 123.5(5) C(9)-C(8)-C(7) 122.0(5) C(8)-C(9)-C(10) 119.3(5) C(9)-C(10)-C(11) 121.1(5) C(10)-C(11)-C(6) 118.8(5) C(10)-C(11)-C(13) 120.0(5) C(6)-C(11)-C(13) 121.2(5) C(19)-C(14)-C(15) 120.1(5) C(19)-C(14)-N(1) 121.8(5) C(15)-C(14)-N(1) 118.1(5) C(16)-C(15)-C(14) 119.2(5) C(16)-C(15)-C(20) 120.0(5) C(14)-C(15)-C(20) 120.9(5) C(17)-C(16)-C(15) 120.2(6) C(16)-C(17)-C(18) 120.5(6) C(17)-C(18)-C(19) 120.8(6) C(18)-C(19)-C(14) 119.2(5) C(18)-C(19)-C(21) 119.4(5) C(14)-C(19)-C(21) 121.3(5) Si(1)-C(22)-Cr(1) 93.1(2) C(26)-C(25)-O(1) 109.5(6) Si(2)-C(27)-Cr(1) 121.4(3) O(2)-C(30)-C(31) 115.3(6) _____________________________________________________________ Table 4. Anisotropic displacement parameters (2x 103) for jpb26. The anisotropic displacement factor exponent takes the form: -2p2[ h2 a*2U11 + ... + 2 h k a* b* U12 ] ______________________________________________________________________________ U11 U22 U33 U23 U13 U12 ______________________________________________________________________________ Cr(1) 21(1) 19(1) 18(1) 3(1) 2(1) 0(1) Si(1) 21(1) 26(1) 26(1) 0(1) 2(1) -1(1) Si(2) 33(1) 35(1) 26(1) -6(1) 10(1) 3(1) O(1) 27(2) 31(2) 20(2) 7(2) -4(2) -5(2) O(2) 46(3) 52(3) 31(2) -1(2) 9(2) 5(2) N(1) 19(2) 18(2) 18(2) 3(2) 4(2) -1(2) N(2) 23(2) 17(2) 21(2) 4(2) 1(2) 2(2) C(1) 25(3) 24(3) 21(3) -6(2) 10(2) 1(3) C(2) 19(3) 27(3) 32(3) 1(3) 0(3) -1(3) C(3) 27(3) 31(3) 26(3) -2(3) 0(2) 9(3) C(4) 28(3) 30(3) 43(4) 2(3) -3(3) -2(3) C(5) 32(3) 41(4) 38(4) 11(3) -4(3) 8(3) C(6) 26(3) 22(3) 21(3) 10(2) -1(2) 5(2) C(7) 28(3) 26(3) 22(3) 5(3) -1(2) 4(3) C(8) 35(3) 22(3) 32(4) 8(3) 2(3) 7(3) C(9) 34(4) 36(4) 39(4) 21(3) 6(3) 1(3) C(10) 30(3) 34(4) 24(3) 5(3) 5(3) 8(3) C(11) 27(3) 32(3) 18(3) 6(3) -2(2) 6(3) C(12) 51(4) 25(3) 39(4) 3(3) 11(3) 14(3) C(13) 45(4) 33(3) 20(3) 1(3) 4(3) 4(3) C(14) 20(3) 17(3) 32(3) 1(3) -1(2) -3(2) C(15) 27(3) 22(3) 30(3) -1(3) 5(3) 0(3) C(16) 33(4) 29(4) 55(4) -1(3) 0(3) 9(3) C(17) 38(4) 26(3) 68(5) 9(4) -10(3) 7(3) C(18) 39(4) 35(4) 34(4) 12(3) -5(3) -5(3) C(19) 23(3) 21(3) 29(3) 6(3) -1(3) -5(2) C(20) 38(4) 35(4) 36(4) -8(3) 10(3) 6(3) C(21) 36(4) 41(4) 24(3) 5(3) 6(3) -6(3) C(22) 24(3) 29(3) 21(3) 5(2) 5(2) 0(3) C(23) 37(4) 41(4) 44(4) -2(3) 1(3) -20(3) C(24) 39(4) 58(5) 52(4) -6(4) 5(3) 12(3) C(25) 44(4) 47(4) 52(4) 10(4) -7(3) -14(3) C(26) 56(5) 62(5) 87(6) 25(5) -16(4) -5(4) C(27) 23(3) 38(3) 26(3) -7(3) 7(2) 4(3) C(28) 48(4) 46(4) 47(4) -15(3) 25(3) -3(3) C(29) 42(4) 36(4) 31(3) -3(3) 12(3) 5(3) C(30) 62(5) 109(7) 34(4) 12(4) 11(4) -6(5) C(31) 95(7) 144(9) 57(6) 34(6) 7(5) 39(7) ______________________________________________________________________________ Table 5. Hydrogen coordinates ( x 104) and isotropic displacement parameters (2x 10 3) for jpb26. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ H(2A) 4546 5573 703 31 H(4A) 6047 3025 1193 51 H(4B) 5337 3263 703 51 H(4C) 4738 3648 1199 51 H(5A) 5173 8443 174 56 H(5B) 4092 7788 454 56 H(5C) 4643 7134 -9 56 H(8A) 7294 11563 377 36 H(9A) 8323 11201 -324 43 H(10A) 8504 9165 -612 35 H(12A) 6112 10976 999 57 H(12B) 6490 9680 1245 57 H(12C) 5328 9742 907 57 H(13A) 8226 7018 -558 49 H(13B) 7012 6624 -295 49 H(13C) 8278 6477 -26 49 H(16A) 9700 1913 911 47 H(17A) 9444 1108 1671 53 H(18A) 8193 2105 2209 43 H(20A) 9290 3377 319 55 H(20B) 9039 4765 511 55 H(20C) 7945 3912 328 55 H(21A) 6869 3666 2427 50 H(21B) 6012 4105 1998 50 H(21C) 7076 4998 2180 50 H(22A) 9650 7484 472 29 H(22B) 9511 8651 840 29 H(23A) 12290 7952 1599 61 H(23B) 11202 7801 1964 61 H(23C) 11187 8914 1582 61 H(24A) 12552 6219 1010 74 H(24B) 11630 5949 581 74 H(24C) 11615 5086 1048 74 H(25A) 9925 6522 2201 57 H(25B) 8897 5482 2131 57 H(26A) 10641 4570 2417 103 H(26B) 11362 5084 1966 103 H(26C) 10337 4046 1896 103 H(27A) 8662 8201 1833 35 H(27B) 7836 8999 1482 35 H(28A) 7030 10146 2443 71 H(28B) 5717 9667 2586 71 H(28C) 5943 10248 2068 71 H(29A) 5369 6618 1751 55 H(29B) 4884 7992 1626 55 H(29C) 4658 7410 2143 55 H(30A) 5890 6546 2910 82 H(30B) 6257 7937 3062 82 H(31A) 6782 6558 3630 148 H(31B) 7957 7195 3409 148 H(31C) 7588 5801 3257 148 ________________________________________________________________________________ P$Q~> +]zVM?¤~gy*(g>yH/$"=cHppF8NH^bFn@zѽ4o}G5osI]Ř!yQsK7rHm5ٻ\3Tl?w9'pdhmTkG]"2`Qᬕ+ !/%Ty#7OPkd_`?(^r6I= ִUҗ1siE往^J~RN6a{r#ZnhU¯YXYY+!Ķ/Re뛋'%E 8HK8_PbחWMg@CQpS쒼PeYd 3Xw\б!= 7=fONooiT_"@tATөꥯiLsITԑOq7@Z>M횎v'<eT݄l}F(^niѼ./.)ݝI1tkqR1UD3 (?^zj-}nwsj000luYԕ (2a &ɭfX4뱵M3"3h#1g=p VB) %RVmHAAV4Np|yS O߻'I]OƑe>C|%YW57I`'2d>5.F5g갏Q՘Rr5)ЋuL`ˡش@xFD4Ɂ|L;Zy@G^ Ж 4FU? dzي54bUuYQ0vXT {5)ŤGl`APQO؉"ҲS>^T2xsA ^(!63P]]{qGy(x@ $#=x@vA09k|?Yh,NPc$Rl{PWd8g N=() No6Q>w0ޱ*ʳɰ#M?IὝsSᨰwi=ٛZ!yi%e5YN;Y''ucNЎd[pR197>ӟ~t1NpλRub[*>;S=؁T{ 9ًٜ9KX&jUq(k>dSnZyEvBYU|zo0VQ'&pdN&>,zԕn Wj]ؙr#KwS*`GzVxߖKObbG9<5[ONC1)1iY0nqRuX !dU_3$/IXvS҅Y4o+<*FK0[7gg56"|b l-&?Rl Ν+¶@0 QιV\gJZvY*ʽ adm F{Iuޯ*P3FLWF Vmr6Ծyޱ%#hxjTfjcW1ЋgX.5'ؓI/UGC˾ R~obK΋@i2} ez*|h ,dG,YA_݂F_T'K.Y|{wgnmo6ܟſ [—$0-[FC7HtOeAC8f%M8bNwȣ_ߐcl8zdM|2m1\[yݯz " 5}F _ʜfF5[r v.Q`ME_"R \FsT-Bt}҅X|{Z㳋 YG<~Ho[)-ݞ6{?_W|y̔o(?]{=;Ů<S_Jx}o]cULMv0WQLr3WzKb)=%E}hpNT1"5'GpXm~Vaiw\^c}Va C/Bgy[)Xf8I]OƑe>|YkG;D ,N*= G_nޑe BjbY7s 7t)bid{bE+5ꔺ%#L%J2e{;\ 'P ]X\A94XN?[h q4 -- b+ }5 D6YbE|fE6F]^a%Fon1LdDo?1J.w/o s+{xlaX 1 "1u&BIPeRT} )C9&T7-n%'T[lqun[FuGVPl:k{l[DP3Izq_d{B %?f%_ۨ'8|vwj=F[cwyr` ]fO~T,nIrKnn(LX%E U B ȵP{ҿLBKm$jJQ vHPbV{j#O# J3Oi)2cGW`wQ.(2 QV1׆{}\gK;<2#yI޲_ǖ>;Ʊ(ۅ:]9w_΢9Y"238=Ks¸4pʪ&CA軯oe `h!&ӿwwh3{ֲ+hd Ln{\v0T18ˌ󲂸+ ʸ);:x=$2k1n2by|/8 $v xK }s_`,ք{- 8D\&1Sgl> =33Zޞe.+<'ͿS4 OSplT HFEYqvZÜ8Nx2+w8d_Q>F tEȜ"xE#B{! emQaU}C:5;QO zͧМbI}HxM'Rlx8M{QXQ#-м +K'CM%9ߚ!tAwAG:>%n:Q.~# ݇Hs(w>xATWC" 2Q-؆Ѹ3MROhTES'4“U v3%bubFIT>lԈsiFIh#ߏ|aߖ-lN|}Wi6F( z}2%YX?_S<ɠ>/z: D{/ɖN2̫aH~C`^_ٵIs;.d`V;?ZgWݕh7 SxYͣd7m*.!tR'M~Z?xS{_h O{=SH;S^L~fgƼ/ȉm1./4/T@A.&&Z,Wa)Ro0o1v:O'4DrOv`W1u4eMdo(tkl׾dneFcmzMG H2Rw5p#S,\f`-J1dµJ2Y v{Mk_gsA5v|^ m`9TKR FѶN03FѦ>=uw`׋^V҇%X&PX kz'~h:ؿ U=w.\@+׺{Fh '!Ia$v|҉Op Y}@]Sj" 8cw ;3:(@7`=w qOPw7;HA$annz9p^7/~f/z5+'p>H#tŹ rzSG_Y5Ah[t* ֝$GM'XexB{YOu(GYЎxz )}mA=h5=.q'!yIx?Kt薳i=yNBh2WCŕo:.lKY 𪚮]΀<>W5\qBHK/<#InټQ4Z]V=s_djk](b{}+ 2+>,h T-r7L }}/zd@NH[{2-g+ |\bb>\ E+5ˏq+B|bh }#}3kwtr f[џV8h+6 FuU`2GkP74'YXE!+=G+?]O0C?#Uwa<҄յ0ƛѧ3^ E+Sx73)|&;ifOu. %ͬ oc`GK\I82LyH^/R'0\lzy@mտ`v]?mh<{=פss=ڭgxj2=< -s.ۦW%d<$WuO?bwz4b5'(#U60)˗gAHs# >&g\^`+xf=+_ӧW'U=o73#U5xB2@,{R?Du$hYb6 zUjsHӹLuvq=x{Eprf_gxqA0~g!vZKU:YomW&JyRGmA= [9An&K<ʈ43^$ӛ4dџMAl؅SS"|ӷЌ]JZ4ҩ]۪L͂J*B+m"ڿTD˴N+1gWm­r>bBqTӒF: |A*I_[sq%nVZdW\J$]I>,xvoo'V&;4- #WPp}'w * &\Mo*}* HW J㞆 JG}0rJ^a:wGݲ )G=Em EK?GƗy$&je]w%l(*GÝ;F)ÓPpTE^jhėwí?p54%\?[sA9|Fov UL=Q1vGt(]Q~M5WR#ϓ5 Ե¿ѮMym[D[m4> 2[kǀ> -|m.Ƣz=hZ,i \}ݺDMi/XV&w0f<'- CB~ ;.u' 2!yػONGcF?D2hj6jYTe|#HoZwd{!Li3X VU,g2o[-V+[/_*CbUVo+RɢֶD[*EIʉ4b Xe4Y"ֺ4p~ \ꀡ95= l]\˕!\g1~U\cml`f>Y@ؚb c,BņG OԆqԳhht_41uKƑiYd6ii෕=yQNgYʽF;+@GX"nVՌ3ĀFLj=*̃|HK֕{/A97|R9w㯠f}(Eu@I:58Gep~m1jk&# 7aW`NYC<\#Y_1Saňp, }Q߰CY}!֛C:xYъe7yVi38)2DPpD3o/}(3,=12}x;Mo*$ivw߸'yRlBWK'<5#I² Mic .z,~?m 0B$~d+bZMUtAI m#kQAȣ1*|fJ6uIcl‹ nr"pء7n2guv2UP2!f.ڰr&ѝIlAc3k̀1H GhfD!Sc$:^dNkuorl6 \ȎyH&se`jпL)shg&cQ-Ys mk bzRI BI3FĆ 3N[ 6;0'w)?|P5Q<qgxcT|QV'g3{2X8ѼQw2&I˺ kLH`cq7vqRJ̒Uc`,bNը?5ԝZ(bgsn6M;$!J,YzSG{{q昔sj[PAQgꝚg =QÍQv OdiT8),99|pa N yL‡^Kg&[aFmoY hhb}ƽΊG;v$/삆t-PaC9ڙ.q,՞ ]#f.Sj:itZVRxTcv ?+DDh/ }2,ŻsҮ.ؚH^;ҠE%ZTDJݪ|V]gH"m5T䫱^Z*GApjnmRp*z2PQ2Fi@2A(N"d?Uݽ]'O;F\J`QvW|yENGу,pF2sFcA1Q{JLƣc߳E e}br&ީ:!fNm!mTૂ謵/8m?93 32Hmqo[xG[uE`=IvUR%PMNFLj'6/|kq^ sBy:FAPSW_Yy>ĺTNm}[Jr@9跇,֛o |M1Ymkf+EлJ  0˃Ͳ]3tW?h07mD}ּ;TRljGZ ^kOhҼ}kciOǴ|y@պm#XByeTa_k:JKҧ٬O@6jh7 qL Fa]A킆 [vG`AY#WUb/G7%({0ab.=Pbunac~ 9R,g*@ƂKM.'2e8yI=lab&3wT+zp'r|+!|+&m &/<m1К)M{feմ^%2]% WMT4cyCOPvuRQHDg >-og;2҆`A1 l;3@l(HL6Wyf9h}?{SOԪ)N6|@ż$d? 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Crystal data and structure refinement for jpb26.\par Identification code \tab jpb26\par Empirical formula \tab C31 H51 Cr N2 O2 Si2\par Formula weight \tab 591.92\par Temperature \tab 147(2) K\par Wavelength \tab 0.71073 \'c5\par Crystal system \tab Monoclinic\par Space group \tab P2(1)/c\par Unit cell dimensions\tab a = 11.1209(9) \'c5\tab}{\f2\fs20 a}{\fs20 = 90\'b0.\par \tab b = 10.6695(9) \'c5\tab}{\f2\fs20 b}{\fs20 = 90.398(2)\'b0.\par \tab c = 28.046(2) \'c5\tab}{\f2\fs20 g}{\fs20 = 90\'b0.\par Volume\tab 3327.7(5) \'c5}{\fs14\up6 3}{\fs20\par Z\tab 4\par Density (calculated)\tab 1.181 Mg/m}{\fs14\up6 3}{\fs20 \par Absorption coefficient\tab 0.444 mm{\fs14\up6 -1}\par F(000)\tab 1276\par Crystal size\tab 0.45 x 0.20 x 0.05 mm}{\fs14\up6 3}{\fs20\par Theta range for data collection\tab 1.83 to 23.00\'b0.\par Index ranges\tab -12<=h<=12, -10<=k<=11, -28<=l<=30\par Reflections collected\tab 13964\par Independent reflections\tab 4628 [R(int) = 0.0625]\par Completeness to theta = 23.00{\'b0}\tab 100.0 % \par Absorption correction\tab None\par Max. and min. transmission\tab 0.9781 and 0.8253\par Refinement method\tab Full-matrix least-squares on F}{\fs14\up6 2}{\fs20\par Data / restraints / parameters\tab 4628 / 0 / 343\par Goodness-of-fit on F}{\fs14\up6 2}{\fs20\tab 1.015\par Final R indices [I>2sigma(I)]\tab R1 = 0.0650, wR2 = 0.1494\par R indices (all data)\tab R1 = 0.1023, wR2 = 0.1636\par Largest diff. peak and hole\tab 0.555 and -0.421 e.\'c5}{\fs14\up6 -3}{\par\page} \pard \sl360\tqc\tx2880\tqc\tx4320\tqc\tx5760\tqc\tx7200\tx11900 {\fs20 Table 2. Atomic coordinates ( x 10}{\fs14\up6 4}{\fs20 ) and equivalent isotropic displacement parameters (\'c5}{\fs14\up6 2}{\fs20 x 10}{\fs14\up6 3}{\fs20)\par for jpb26. U(eq) is defined as one third of the trace of the orthogonalized U{\fs14\up6 ij} tensor.\par ________________________________________________________________________________ \par \tab x\tab y\tab z\tab U(eq)\par ________________________________________________________________________________ } \pard \sl360\tqdec\tx2880\tqdec\tx4320\tqdec\tx5760 \tqdec\tx7200\tx11900 {\fs20\par Cr(1)\tab 8065(1)\tab 6816(1)\tab 1135(1)\tab 19(1)\par Si(1)\tab 10624(1)\tab 7007(1)\tab 1206(1)\tab 24(1)\par Si(2)\tab 6666(1)\tab 8144(2)\tab 2092(1)\tab 31(1)\par O(1)\tab 9595(3)\tab 6104(3)\tab 1499(1)\tab 26(1)\par O(2)\tab 7192(4)\tab 7264(4)\tab 2532(1)\tab 43(1)\par N(1)\tab 7169(4)\tab 5106(4)\tab 1156(1)\tab 18(1)\par N(2)\tab 6812(4)\tab 7438(4)\tab 669(1)\tab 20(1)\par C(1)\tab 6060(5)\tab 4881(5)\tab 988(2)\tab 23(1)\par C(2)\tab 5368(5)\tab 5780(5)\tab 754(2)\tab 26(1)\par C(3)\tab 5730(5)\tab 6946(5)\tab 585(2)\tab 28(1)\par C(4)\tab 5495(5)\tab 3590(5)\tab 1024(2)\tab 34(2)\par C(5)\tab 4830(5)\tab 7639(6)\tab 273(2)\tab 37(2)\par C(6)\tab 7133(5)\tab 8526(5)\tab 381(2)\tab 23(1)\par C(7)\tab 6911(5)\tab 9751(5)\tab 534(2)\tab 25(1)\par C(8)\tab 7389(5)\tab 10727(5)\tab 267(2)\tab 30(1)\par C(9)\tab 7994(5)\tab 10519(6)\tab -151(2)\tab 36(2)\par C(10)\tab 8119(5)\tab 9308(5)\tab -316(2)\tab 29(1)\par C(11)\tab 7694(5)\tab 8300(5)\tab -57(2)\tab 26(1)\par C(12)\tab 6143(6)\tab 10065(5)\tab 958(2)\tab 38(2)\par C(13)\tab 7813(5)\tab 6990(5)\tab -251(2)\tab 33(1)\par C(14)\tab 7803(4)\tab 4000(5)\tab 1313(2)\tab 23(1)\par C(15)\tab 8571(5)\tab 3406(5)\tab 988(2)\tab 26(1)\par C(16)\tab 9180(5)\tab 2324(6)\tab 1128(2)\tab 39(2)\par C(17)\tab 9031(5)\tab 1850(6)\tab 1579(2)\tab 44(2)\par C(18)\tab 8288(5)\tab 2443(6)\tab 1899(2)\tab 36(2)\par C(19)\tab 7678(5)\tab 3526(5)\tab 1772(2)\tab 24(1)\par C(20)\tab 8724(5)\tab 3908(6)\tab 494(2)\tab 37(2)\par C(21)\tab 6835(5)\tab 4126(5)\tab 2125(2)\tab 34(2)\par C(22)\tab 9541(4)\tab 7727(5)\tab 809(2)\tab 25(1)\par C(23)\tab 11420(5)\tab 8041(6)\tab 1639(2)\tab 41(2)\par C(24)\tab 11737(5)\tab 5939(6)\tab 929(2)\tab 50(2)\par C(25)\tab 9688(6)\tab 5773(6)\tab 2015(2)\tab 48(2)\par C(26)\tab 10580(6)\tab 4788(7)\tab 2079(3)\tab 68(2)\par C(27)\tab 7897(5)\tab 8186(5)\tab 1651(2)\tab 29(1)\par C(28)\tab 6295(6)\tab 9742(6)\tab 2325(2)\tab 47(2)\par C(29)\tab 5224(5)\tab 7460(6)\tab 1878(2)\tab 37(2)\par C(30)\tab 6582(7)\tab 7113(8)\tab 2965(2)\tab 68(2)\par C(31)\tab 7281(8)\tab 6630(10)\tab 3344(3)\tab 98(3)\par ________________________________________________________________________________ \page} \pard \sl360\tqdec\tx2880\tx11900 {\fs20 Table 3. Bond lengths [\'c5] and angles [\'b0] for jpb26.\par _____________________________________________________ \par Cr(1)-N(2) \tab 2.017(4)\par Cr(1)-C(27) \tab 2.066(5)\par Cr(1)-N(1) \tab 2.080(4)\par Cr(1)-O(1) \tab 2.119(4)\par Cr(1)-C(22) \tab 2.120(5)\par Cr(1)-Si(1) \tab 2.8588(17)\par Si(1)-O(1) \tab 1.711(4)\par Si(1)-C(22) \tab 1.806(5)\par Si(1)-C(24) \tab 1.856(6)\par Si(1)-C(23) \tab 1.860(6)\par Si(2)-O(2) \tab 1.654(4)\par Si(2)-C(27) \tab 1.853(5)\par Si(2)-C(29) \tab 1.858(6)\par Si(2)-C(28) \tab 1.873(6)\par O(1)-C(25) \tab 1.491(7)\par O(2)-C(30) \tab 1.404(7)\par N(1)-C(1) \tab 1.339(6)\par N(1)-C(14) \tab 1.441(6)\par N(2)-C(3) \tab 1.333(7)\par N(2)-C(6) \tab 1.459(6)\par C(1)-C(2) \tab 1.391(7)\par C(1)-C(4) \tab 1.518(7)\par C(2)-C(3) \tab 1.391(7)\par C(3)-C(5) \tab 1.517(7)\par C(6)-C(7) \tab 1.398(7)\par C(6)-C(11) \tab 1.403(7)\par C(7)-C(8) \tab 1.390(7)\par C(7)-C(12) \tab 1.508(7)\par C(8)-C(9) \tab 1.374(7)\par C(9)-C(10) \tab 1.379(8)\par C(10)-C(11) \tab 1.383(7)\par C(11)-C(13) \tab 1.506(7)\par C(14)-C(19) \tab 1.393(7)\par C(14)-C(15) \tab 1.405(7)\par C(15)-C(16) \tab 1.394(8)\par C(15)-C(20) \tab 1.495(7)\par C(16)-C(17) \tab 1.373(8)\par C(17)-C(18) \tab 1.378(8)\par C(18)-C(19) \tab 1.385(8)\par C(19)-C(21) \tab 1.511(7)\par C(25)-C(26) \tab 1.456(9)\par C(30)-C(31) \tab 1.411(9)\par \par N(2)-Cr(1)-C(27)\tab 98.9(2)\par N(2)-Cr(1)-N(1)\tab 88.79(17)\par C(27)-Cr(1)-N(1)\tab 123.66(19)\par N(2)-Cr(1)-O(1)\tab 168.36(15)\par C(27)-Cr(1)-O(1)\tab 89.54(18)\par N(1)-Cr(1)-O(1)\tab 93.15(15)\par N(2)-Cr(1)-C(22)\tab 95.93(18)\par C(27)-Cr(1)-C(22)\tab 92.9(2)\par N(1)-Cr(1)-C(22)\tab 141.97(18)\par O(1)-Cr(1)-C(22)\tab 75.56(16)\par N(2)-Cr(1)-Si(1)\tab 134.82(12)\par C(27)-Cr(1)-Si(1)\tab 89.75(15)\par N(1)-Cr(1)-Si(1)\tab 122.51(12)\par O(1)-Cr(1)-Si(1)\tab 36.52(9)\par C(22)-Cr(1)-Si(1)\tab 39.10(14)\par O(1)-Si(1)-C(22)\tab 95.2(2)\par O(1)-Si(1)-C(24)\tab 107.8(3)\par C(22)-Si(1)-C(24)\tab 116.5(3)\par O(1)-Si(1)-C(23)\tab 109.7(2)\par C(22)-Si(1)-C(23)\tab 117.5(3)\par C(24)-Si(1)-C(23)\tab 108.8(3)\par O(1)-Si(1)-Cr(1)\tab 47.51(12)\par C(22)-Si(1)-Cr(1)\tab 47.78(15)\par C(24)-Si(1)-Cr(1)\tab 126.4(2)\par C(23)-Si(1)-Cr(1)\tab 123.8(2)\par O(2)-Si(2)-C(27)\tab 104.7(2)\par O(2)-Si(2)-C(29)\tab 108.5(3)\par C(27)-Si(2)-C(29)\tab 115.7(2)\par O(2)-Si(2)-C(28)\tab 109.5(3)\par C(27)-Si(2)-C(28)\tab 112.1(3)\par C(29)-Si(2)-C(28)\tab 106.2(3)\par C(25)-O(1)-Si(1)\tab 123.9(3)\par C(25)-O(1)-Cr(1)\tab 127.0(3)\par Si(1)-O(1)-Cr(1)\tab 95.97(16)\par C(30)-O(2)-Si(2)\tab 122.7(4)\par C(1)-N(1)-C(14)\tab 114.1(4)\par C(1)-N(1)-Cr(1)\tab 125.9(3)\par C(14)-N(1)-Cr(1)\tab 119.6(3)\par C(3)-N(2)-C(6)\tab 116.1(4)\par C(3)-N(2)-Cr(1)\tab 127.1(4)\par C(6)-N(2)-Cr(1)\tab 116.7(3)\par N(1)-C(1)-C(2)\tab 123.3(5)\par N(1)-C(1)-C(4)\tab 121.3(5)\par C(2)-C(1)-C(4)\tab 115.4(5)\par C(3)-C(2)-C(1)\tab 128.0(5)\par N(2)-C(3)-C(2)\tab 123.8(5)\par N(2)-C(3)-C(5)\tab 120.0(5)\par C(2)-C(3)-C(5)\tab 116.1(5)\par C(7)-C(6)-C(11)\tab 120.7(5)\par C(7)-C(6)-N(2)\tab 122.0(4)\par C(11)-C(6)-N(2)\tab 117.3(5)\par C(8)-C(7)-C(6)\tab 117.8(5)\par C(8)-C(7)-C(12)\tab 118.6(5)\par C(6)-C(7)-C(12)\tab 123.5(5)\par C(9)-C(8)-C(7)\tab 122.0(5)\par C(8)-C(9)-C(10)\tab 119.3(5)\par C(9)-C(10)-C(11)\tab 121.1(5)\par C(10)-C(11)-C(6)\tab 118.8(5)\par C(10)-C(11)-C(13)\tab 120.0(5)\par C(6)-C(11)-C(13)\tab 121.2(5)\par C(19)-C(14)-C(15)\tab 120.1(5)\par C(19)-C(14)-N(1)\tab 121.8(5)\par C(15)-C(14)-N(1)\tab 118.1(5)\par C(16)-C(15)-C(14)\tab 119.2(5)\par C(16)-C(15)-C(20)\tab 120.0(5)\par C(14)-C(15)-C(20)\tab 120.9(5)\par C(17)-C(16)-C(15)\tab 120.2(6)\par C(16)-C(17)-C(18)\tab 120.5(6)\par C(17)-C(18)-C(19)\tab 120.8(6)\par C(18)-C(19)-C(14)\tab 119.2(5)\par C(18)-C(19)-C(21)\tab 119.4(5)\par C(14)-C(19)-C(21)\tab 121.3(5)\par Si(1)-C(22)-Cr(1)\tab 93.1(2)\par C(26)-C(25)-O(1)\tab 109.5(6)\par Si(2)-C(27)-Cr(1)\tab 121.4(3)\par O(2)-C(30)-C(31)\tab 115.3(6)\par _____________________________________________________________ \par Symmetry transformations used to generate equivalent atoms: \par \par \page} \pard\sl360\tqc\tx1200\tqc\tx2400\tqc\tx3600 \tqc\tx4800\tqc\tx6000\tqc\tx7200\tx8400 {\fs20 Table 4. Anisotropic displacement parameters (\'c5}{\fs14\up6 2}{\fs20 x 10}{\fs14\up6 3}{\fs20) for jpb26. The anisotropic\par displacement factor exponent takes the form: -2}{\f2\fs20 p}{\fs14\up6 2}{\fs20 [ h}{\fs14\up6 2} {\fs20 a*}{\fs14\up6 2}{\fs20 U{\fs14\up6 11} + ... + 2 h k a* b* U{\fs14\up6 12} ]\par ______________________________________________________________________________ \par \tab U{\fs14\up6 11}\tab U{\fs14\up6 22} \tab U{\fs14\up6 33}\tab U{\fs14\up6 23}\tab U{\fs14\up6 13}\tab U{\fs14\up6 12}\par ______________________________________________________________________________ \par\fs20 Cr(1)\tab 21(1) \tab 19(1)\tab 18(1) \tab 3(1)\tab 2(1) \tab 0(1)\par Si(1)\tab 21(1) \tab 26(1)\tab 26(1) \tab 0(1)\tab 2(1) \tab -1(1)\par Si(2)\tab 33(1) \tab 35(1)\tab 26(1) \tab -6(1)\tab 10(1) \tab 3(1)\par O(1)\tab 27(2) \tab 31(2)\tab 20(2) \tab 7(2)\tab -4(2) \tab -5(2)\par O(2)\tab 46(3) \tab 52(3)\tab 31(2) \tab -1(2)\tab 9(2) \tab 5(2)\par N(1)\tab 19(2) \tab 18(2)\tab 18(2) \tab 3(2)\tab 4(2) \tab -1(2)\par N(2)\tab 23(2) \tab 17(2)\tab 21(2) \tab 4(2)\tab 1(2) \tab 2(2)\par C(1)\tab 25(3) \tab 24(3)\tab 21(3) \tab -6(2)\tab 10(2) \tab 1(3)\par C(2)\tab 19(3) \tab 27(3)\tab 32(3) \tab 1(3)\tab 0(3) \tab -1(3)\par C(3)\tab 27(3) \tab 31(3)\tab 26(3) \tab -2(3)\tab 0(2) \tab 9(3)\par C(4)\tab 28(3) \tab 30(3)\tab 43(4) \tab 2(3)\tab -3(3) \tab -2(3)\par C(5)\tab 32(3) \tab 41(4)\tab 38(4) \tab 11(3)\tab -4(3) \tab 8(3)\par C(6)\tab 26(3) \tab 22(3)\tab 21(3) \tab 10(2)\tab -1(2) \tab 5(2)\par C(7)\tab 28(3) \tab 26(3)\tab 22(3) \tab 5(3)\tab -1(2) \tab 4(3)\par C(8)\tab 35(3) \tab 22(3)\tab 32(4) \tab 8(3)\tab 2(3) \tab 7(3)\par C(9)\tab 34(4) \tab 36(4)\tab 39(4) \tab 21(3)\tab 6(3) \tab 1(3)\par C(10)\tab 30(3) \tab 34(4)\tab 24(3) \tab 5(3)\tab 5(3) \tab 8(3)\par C(11)\tab 27(3) \tab 32(3)\tab 18(3) \tab 6(3)\tab -2(2) \tab 6(3)\par C(12)\tab 51(4) \tab 25(3)\tab 39(4) \tab 3(3)\tab 11(3) \tab 14(3)\par C(13)\tab 45(4) \tab 33(3)\tab 20(3) \tab 1(3)\tab 4(3) \tab 4(3)\par C(14)\tab 20(3) \tab 17(3)\tab 32(3) \tab 1(3)\tab -1(2) \tab -3(2)\par C(15)\tab 27(3) \tab 22(3)\tab 30(3) \tab -1(3)\tab 5(3) \tab 0(3)\par C(16)\tab 33(4) \tab 29(4)\tab 55(4) \tab -1(3)\tab 0(3) \tab 9(3)\par C(17)\tab 38(4) \tab 26(3)\tab 68(5) \tab 9(4)\tab -10(3) \tab 7(3)\par C(18)\tab 39(4) \tab 35(4)\tab 34(4) \tab 12(3)\tab -5(3) \tab -5(3)\par C(19)\tab 23(3) \tab 21(3)\tab 29(3) \tab 6(3)\tab -1(3) \tab -5(2)\par C(20)\tab 38(4) \tab 35(4)\tab 36(4) \tab -8(3)\tab 10(3) \tab 6(3)\par C(21)\tab 36(4) \tab 41(4)\tab 24(3) \tab 5(3)\tab 6(3) \tab -6(3)\par C(22)\tab 24(3) \tab 29(3)\tab 21(3) \tab 5(2)\tab 5(2) \tab 0(3)\par C(23)\tab 37(4) \tab 41(4)\tab 44(4) \tab -2(3)\tab 1(3) \tab -20(3)\par C(24)\tab 39(4) \tab 58(5)\tab 52(4) \tab -6(4)\tab 5(3) \tab 12(3)\par C(25)\tab 44(4) \tab 47(4)\tab 52(4) \tab 10(4)\tab -7(3) \tab -14(3)\par C(26)\tab 56(5) \tab 62(5)\tab 87(6) \tab 25(5)\tab -16(4) \tab -5(4)\par C(27)\tab 23(3) \tab 38(3)\tab 26(3) \tab -7(3)\tab 7(2) \tab 4(3)\par C(28)\tab 48(4) \tab 46(4)\tab 47(4) \tab -15(3)\tab 25(3) \tab -3(3)\par C(29)\tab 42(4) \tab 36(4)\tab 31(3) \tab -3(3)\tab 12(3) \tab 5(3)\par C(30)\tab 62(5) \tab 109(7)\tab 34(4) \tab 12(4)\tab 11(4) \tab -6(5)\par C(31)\tab 95(7) \tab 144(9)\tab 57(6) \tab 34(6)\tab 7(5) \tab 39(7)\par ______________________________________________________________________________ \page} \pard \sl360\tqc\tx2880\tqc\tx4320\tqc \tx5760\tqc\tx7200\tx11900 {\fs20 Table 5. Hydrogen coordinates ( x 10}{\fs14\up6 4}{\fs20 ) and isotropic displacement parameters (\'c5}{\fs14\up6 2}{\fs20 x 10} {\fs14\up6 3}{\fs20)\par for jpb26.\par ________________________________________________________________________________ \par \tab x \tab y \tab z \tab U(eq)\par ________________________________________________________________________________ \par} \pard \sl360\tqdec\tx2880\tqdec\tx4320\tqdec\tx5760 \tqdec\tx7200\tx11900 {\fs20\par H(2A)\tab 4546\tab 5573\tab 703\tab 31\par H(4A)\tab 6047\tab 3025\tab 1193\tab 51\par H(4B)\tab 5337\tab 3263\tab 703\tab 51\par H(4C)\tab 4738\tab 3648\tab 1199\tab 51\par H(5A)\tab 5173\tab 8443\tab 174\tab 56\par H(5B)\tab 4092\tab 7788\tab 454\tab 56\par H(5C)\tab 4643\tab 7134\tab -9\tab 56\par H(8A)\tab 7294\tab 11563\tab 377\tab 36\par H(9A)\tab 8323\tab 11201\tab -324\tab 43\par H(10A)\tab 8504\tab 9165\tab -612\tab 35\par H(12A)\tab 6112\tab 10976\tab 999\tab 57\par H(12B)\tab 6490\tab 9680\tab 1245\tab 57\par H(12C)\tab 5328\tab 9742\tab 907\tab 57\par H(13A)\tab 8226\tab 7018\tab -558\tab 49\par H(13B)\tab 7012\tab 6624\tab -295\tab 49\par H(13C)\tab 8278\tab 6477\tab -26\tab 49\par H(16A)\tab 9700\tab 1913\tab 911\tab 47\par H(17A)\tab 9444\tab 1108\tab 1671\tab 53\par H(18A)\tab 8193\tab 2105\tab 2209\tab 43\par H(20A)\tab 9290\tab 3377\tab 319\tab 55\par H(20B)\tab 9039\tab 4765\tab 511\tab 55\par H(20C)\tab 7945\tab 3912\tab 328\tab 55\par H(21A)\tab 6869\tab 3666\tab 2427\tab 50\par H(21B)\tab 6012\tab 4105\tab 1998\tab 50\par H(21C)\tab 7076\tab 4998\tab 2180\tab 50\par H(22A)\tab 9650\tab 7484\tab 472\tab 29\par H(22B)\tab 9511\tab 8651\tab 840\tab 29\par H(23A)\tab 12290\tab 7952\tab 1599\tab 61\par H(23B)\tab 11202\tab 7801\tab 1964\tab 61\par H(23C)\tab 11187\tab 8914\tab 1582\tab 61\par H(24A)\tab 12552\tab 6219\tab 1010\tab 74\par H(24B)\tab 11630\tab 5949\tab 581\tab 74\par H(24C)\tab 11615\tab 5086\tab 1048\tab 74\par H(25A)\tab 9925\tab 6522\tab 2201\tab 57\par H(25B)\tab 8897\tab 5482\tab 2131\tab 57\par H(26A)\tab 10641\tab 4570\tab 2417\tab 103\par H(26B)\tab 11362\tab 5084\tab 1966\tab 103\par H(26C)\tab 10337\tab 4046\tab 1896\tab 103\par H(27A)\tab 8662\tab 8201\tab 1833\tab 35\par H(27B)\tab 7836\tab 8999\tab 1482\tab 35\par H(28A)\tab 7030\tab 10146\tab 2443\tab 71\par H(28B)\tab 5717\tab 9667\tab 2586\tab 71\par H(28C)\tab 5943\tab 10248\tab 2068\tab 71\par H(29A)\tab 5369\tab 6618\tab 1751\tab 55\par H(29B)\tab 4884\tab 7992\tab 1626\tab 55\par H(29C)\tab 4658\tab 7410\tab 2143\tab 55\par H(30A)\tab 5890\tab 6546\tab 2910\tab 82\par H(30B)\tab 6257\tab 7937\tab 3062\tab 82\par H(31A)\tab 6782\tab 6558\tab 3630\tab 148\par H(31B)\tab 7957\tab 7195\tab 3409\tab 148\par H(31C)\tab 7588\tab 5801\tab 3257\tab 148\par ________________________________________________________________________________ \page} } ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + jpb26 started at 00:31:23 on 19-Sep-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL jpb26 in P2(1)/c CELL 0.71073 11.1209 10.6695 28.0462 90.000 90.398 90.000 ZERR 4.00 0.0009 0.0009 0.0023 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O SI CR UNIT 124 204 8 8 8 4 V = 3327.73 F(000) = 1276.0 Mu = 0.44 mm-1 Cell Wt = 2367.67 Rho = 1.181 TEMP -126 L.S. 4 BOND FMAP 2 PLAN 5 ACTA SIZE 0.45 0.20 0.05 OMIT -3 46 OMIT 0 0 2 WGHT 0.085200 FVAR 0.11116 CR1 6 0.80650 0.68157 0.11346 11.00000 0.02068 0.01861 = 0.01773 0.00272 0.00218 0.00025 SI1 5 1.06241 0.70065 0.12059 11.00000 0.02103 0.02635 = 0.02554 0.00002 0.00244 -0.00084 SI2 5 0.66656 0.81439 0.20919 11.00000 0.03339 0.03516 = 0.02575 -0.00596 0.00977 0.00277 O1 4 0.95949 0.61042 0.14992 11.00000 0.02729 0.03070 = 0.01954 0.00718 -0.00405 -0.00515 O2 4 0.71915 0.72639 0.25317 11.00000 0.04556 0.05158 = 0.03084 -0.00059 0.00938 0.00457 N1 3 0.71687 0.51060 0.11564 11.00000 0.01902 0.01772 = 0.01842 0.00294 0.00415 -0.00077 N2 3 0.68121 0.74384 0.06685 11.00000 0.02289 0.01717 = 0.02078 0.00362 0.00133 0.00246 C1 1 0.60601 0.48815 0.09877 11.00000 0.02540 0.02430 = 0.02056 -0.00577 0.00994 0.00087 C2 1 0.53676 0.57804 0.07539 11.00000 0.01921 0.02711 = 0.03153 0.00059 0.00008 -0.00083 AFIX 43 H2A 2 0.45371 0.55706 0.07030 11.00000 -1.20000 AFIX 0 C3 1 0.57298 0.69457 0.05849 11.00000 0.02673 0.03134 = 0.02628 -0.00225 0.00044 0.00906 C4 1 0.54953 0.35898 0.10242 11.00000 0.02813 0.02955 = 0.04332 0.00165 -0.00336 -0.00224 AFIX 33 H4A 2 0.60353 0.30363 0.11899 11.00000 -1.50000 H4B 2 0.47534 0.36471 0.11957 11.00000 -1.50000 H4C 2 0.53402 0.32693 0.07099 11.00000 -1.50000 AFIX 0 C5 1 0.48297 0.76390 0.02735 11.00000 0.03196 0.04133 = 0.03829 0.01068 -0.00384 0.00777 AFIX 33 H5A 2 0.51660 0.84267 0.01765 11.00000 -1.50000 H5B 2 0.46464 0.71441 -0.00035 11.00000 -1.50000 H5C 2 0.41071 0.77852 0.04503 11.00000 -1.50000 AFIX 0 C6 1 0.71329 0.85260 0.03812 11.00000 0.02577 0.02222 = 0.02057 0.00961 -0.00110 0.00484 C7 1 0.69111 0.97508 0.05340 11.00000 0.02825 0.02579 = 0.02195 0.00496 -0.00108 0.00364 C8 1 0.73886 1.07269 0.02672 11.00000 0.03472 0.02212 = 0.03238 0.00774 0.00172 0.00724 AFIX 43 H8A 2 0.72925 1.15718 0.03784 11.00000 -1.20000 AFIX 0 C9 1 0.79938 1.05187 -0.01507 11.00000 0.03398 0.03599 = 0.03871 0.02089 0.00620 0.00098 AFIX 43 H9A 2 0.83259 1.12081 -0.03260 11.00000 -1.20000 AFIX 0 C10 1 0.81189 0.93082 -0.03158 11.00000 0.03032 0.03377 = 0.02365 0.00527 0.00512 0.00789 AFIX 43 H10A 2 0.85077 0.91632 -0.06153 11.00000 -1.20000 AFIX 0 C11 1 0.76935 0.82998 -0.00569 11.00000 0.02745 0.03219 = 0.01826 0.00619 -0.00223 0.00590 C12 1 0.61430 1.00646 0.09585 11.00000 0.05072 0.02509 = 0.03896 0.00298 0.01104 0.01440 AFIX 33 H12A 2 0.61130 1.09576 0.09986 11.00000 -1.50000 H12B 2 0.53442 0.97485 0.09076 11.00000 -1.50000 H12C 2 0.64827 0.96877 0.12395 11.00000 -1.50000 AFIX 0 C13 1 0.78127 0.69900 -0.02512 11.00000 0.04516 0.03272 = 0.02000 0.00064 0.00376 0.00399 AFIX 33 H13A 2 0.82176 0.70170 -0.05522 11.00000 -1.50000 H13B 2 0.82687 0.64872 -0.00311 11.00000 -1.50000 H13C 2 0.70279 0.66310 -0.02941 11.00000 -1.50000 AFIX 0 C14 1 0.78028 0.40002 0.13125 11.00000 0.02038 0.01738 = 0.03251 0.00123 -0.00124 -0.00254 C15 1 0.85706 0.34061 0.09875 11.00000 0.02671 0.02177 = 0.03047 -0.00087 0.00465 0.00021 C16 1 0.91800 0.23240 0.11277 11.00000 0.03305 0.02920 = 0.05537 -0.00108 -0.00005 0.00864 AFIX 43 H16A 2 0.97053 0.19086 0.09082 11.00000 -1.20000 AFIX 0 C17 1 0.90313 0.18503 0.15785 11.00000 0.03819 0.02610 = 0.06757 0.00931 -0.01046 0.00716 AFIX 43 H17A 2 0.94482 0.11004 0.16716 11.00000 -1.20000 AFIX 0 C18 1 0.82881 0.24432 0.18986 11.00000 0.03944 0.03479 = 0.03440 0.01222 -0.00526 -0.00538 AFIX 43 H18A 2 0.81923 0.21016 0.22127 11.00000 -1.20000 AFIX 0 C19 1 0.76778 0.35263 0.17723 11.00000 0.02318 0.02080 = 0.02926 0.00558 -0.00129 -0.00478 C20 1 0.87244 0.39085 0.04939 11.00000 0.03844 0.03534 = 0.03585 -0.00845 0.00971 0.00594 AFIX 33 H20A 2 0.92781 0.33883 0.03228 11.00000 -1.50000 H20B 2 0.79612 0.39117 0.03318 11.00000 -1.50000 H20C 2 0.90324 0.47480 0.05103 11.00000 -1.50000 AFIX 0 C21 1 0.68347 0.41265 0.21253 11.00000 0.03603 0.04071 = 0.02401 0.00501 0.00586 -0.00586 AFIX 33 H21A 2 0.68680 0.36749 0.24211 11.00000 -1.50000 H21B 2 0.70715 0.49806 0.21784 11.00000 -1.50000 H21C 2 0.60289 0.41053 0.20006 11.00000 -1.50000 AFIX 0 C22 1 0.95412 0.77273 0.08091 11.00000 0.02426 0.02864 = 0.02060 0.00489 0.00487 -0.00025 AFIX 23 H22A 2 0.95123 0.86230 0.08393 11.00000 -1.20000 H22B 2 0.96471 0.74915 0.04817 11.00000 -1.20000 AFIX 0 C23 1 1.14199 0.80409 0.16389 11.00000 0.03716 0.04136 = 0.04396 -0.00177 0.00073 -0.02017 AFIX 33 H23A 2 1.22726 0.79544 0.15994 11.00000 -1.50000 H23B 2 1.11913 0.88963 0.15831 11.00000 -1.50000 H23C 2 1.12064 0.78058 0.19577 11.00000 -1.50000 AFIX 0 C24 1 1.17367 0.59392 0.09286 11.00000 0.03867 0.05827 = 0.05202 -0.00584 0.00455 0.01227 AFIX 33 H24A 2 1.25352 0.62137 0.10084 11.00000 -1.50000 H24B 2 1.16178 0.51030 0.10455 11.00000 -1.50000 H24C 2 1.16326 0.59490 0.05886 11.00000 -1.50000 AFIX 0 C25 1 0.96877 0.57733 0.20147 11.00000 0.04371 0.04713 = 0.05197 0.00973 -0.00672 -0.01395 AFIX 23 H25A 2 0.89212 0.54906 0.21275 11.00000 -1.20000 H25B 2 0.99178 0.64992 0.21958 11.00000 -1.20000 AFIX 0 C26 1 1.05801 0.47878 0.20787 11.00000 0.05583 0.06247 = 0.08690 0.02457 -0.01574 -0.00507 AFIX 33 H26A 2 1.06400 0.45746 0.24105 11.00000 -1.50000 H26B 2 1.03421 0.40613 0.18994 11.00000 -1.50000 H26C 2 1.13464 0.50777 0.19682 11.00000 -1.50000 AFIX 0 C27 1 0.78966 0.81860 0.16505 11.00000 0.02270 0.03764 = 0.02643 -0.00721 0.00654 0.00371 AFIX 23 H27A 2 0.78374 0.89743 0.14870 11.00000 -1.20000 H27B 2 0.86387 0.82010 0.18273 11.00000 -1.20000 AFIX 0 C28 1 0.62948 0.97416 0.23248 11.00000 0.04803 0.04635 = 0.04738 -0.01539 0.02536 -0.00348 AFIX 33 H28A 2 0.70150 1.01375 0.24405 11.00000 -1.50000 H28B 2 0.59505 1.02380 0.20731 11.00000 -1.50000 H28C 2 0.57289 0.96683 0.25802 11.00000 -1.50000 AFIX 0 C29 1 0.52236 0.74600 0.18779 11.00000 0.04218 0.03629 = 0.03125 -0.00265 0.01157 0.00498 AFIX 33 H29A 2 0.53656 0.66348 0.17540 11.00000 -1.50000 H29B 2 0.46691 0.74111 0.21380 11.00000 -1.50000 H29C 2 0.48908 0.79807 0.16309 11.00000 -1.50000 AFIX 0 C30 1 0.65820 0.71132 0.29645 11.00000 0.06201 0.10887 = 0.03407 0.01233 0.01053 -0.00559 AFIX 23 H30A 2 0.59107 0.65634 0.29118 11.00000 -1.20000 H30B 2 0.62669 0.79125 0.30591 11.00000 -1.20000 AFIX 0 C31 1 0.72807 0.66297 0.33441 11.00000 0.09482 0.14356 = 0.05698 0.03390 0.00704 0.03872 AFIX 33 H31A 2 0.67924 0.65592 0.36238 11.00000 -1.50000 H31B 2 0.75822 0.58175 0.32589 11.00000 -1.50000 H31C 2 0.79428 0.71835 0.34080 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for jpb26 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CR 1.240 Cr1 - N2 C27 N1 O1 C22 Si1 Si1 - O1 C22 C24 C23 Cr1 Si2 - O2 C27 C29 C28 O1 - C25 Si1 Cr1 O2 - C30 Si2 N1 - C1 C14 Cr1 N2 - C3 C6 Cr1 C1 - N1 C2 C4 C2 - C3 C1 C3 - N2 C2 C5 C4 - C1 C5 - C3 C6 - C7 C11 N2 C7 - C8 C6 C12 C8 - C9 C7 C9 - C8 C10 C10 - C9 C11 C11 - C10 C6 C13 C12 - C7 C13 - C11 C14 - C19 C15 N1 C15 - C16 C14 C20 C16 - C17 C15 C17 - C16 C18 C18 - C17 C19 C19 - C18 C14 C21 C20 - C15 C21 - C19 C22 - Si1 Cr1 C23 - Si1 C24 - Si1 C25 - C26 O1 C26 - C25 C27 - Si2 Cr1 C28 - Si2 C29 - Si2 C30 - O2 C31 C31 - C30 20378 Reflections read, of which 6414 rejected -12 =< h =< 12, -10 =< k =< 11, -28 =< l =< 30, Max. 2-theta = 45.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 2 805.92 3.74 2 21.21 1 Inconsistent equivalents 4628 Unique reflections, of which 0 suppressed R(int) = 0.0625 R(sigma) = 0.0870 Friedel opposites merged Maximum memory for data reduction = 3855 / 46088 Default effective X-H distances for T = -126.0 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 = 4957 / 435267 wR2 = 0.1636 before cycle 1 for 4628 data and 343 / 343 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0852 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11116 0.00028 -0.011 OSF Mean shift/esd = 0.004 Maximum = 0.101 for z Cr1 Max. shift = 0.000 A for C31 Max. dU = 0.000 for C31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4957 / 435267 wR2 = 0.1636 before cycle 2 for 4628 data and 343 / 343 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0852 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11116 0.00028 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.038 for z Cr1 Max. shift = 0.000 A for C29 Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4957 / 435267 wR2 = 0.1636 before cycle 3 for 4628 data and 343 / 343 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0852 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11116 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for z Cr1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C31 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4957 / 435267 wR2 = 0.1636 before cycle 4 for 4628 data and 343 / 343 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0852 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11116 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Si1 Max. shift = 0.000 A for H28A Max. dU = 0.000 for C31 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4546 0.5573 0.0703 43 0.950 0.000 C2 C3 C1 H4A 0.6047 0.3025 0.1193 33 0.980 0.000 C4 C1 H4A H4B 0.5337 0.3263 0.0703 33 0.980 0.000 C4 C1 H4A H4C 0.4738 0.3648 0.1199 33 0.980 0.000 C4 C1 H4A H5A 0.5173 0.8443 0.0174 33 0.980 0.000 C5 C3 H5A H5B 0.4092 0.7788 0.0454 33 0.980 0.000 C5 C3 H5A H5C 0.4643 0.7134 -0.0009 33 0.980 0.000 C5 C3 H5A H8A 0.7294 1.1563 0.0377 43 0.950 0.000 C8 C9 C7 H9A 0.8323 1.1201 -0.0324 43 0.950 0.000 C9 C8 C10 H10A 0.8504 0.9165 -0.0612 43 0.950 0.000 C10 C9 C11 H12A 0.6112 1.0976 0.0999 33 0.980 0.000 C12 C7 H12A H12B 0.6490 0.9680 0.1245 33 0.980 0.000 C12 C7 H12A H12C 0.5328 0.9742 0.0907 33 0.980 0.000 C12 C7 H12A H13A 0.8226 0.7018 -0.0558 33 0.980 0.000 C13 C11 H13A H13B 0.7012 0.6624 -0.0295 33 0.980 0.000 C13 C11 H13A H13C 0.8278 0.6477 -0.0026 33 0.980 0.000 C13 C11 H13A H16A 0.9700 0.1913 0.0911 43 0.950 0.000 C16 C17 C15 H17A 0.9444 0.1108 0.1671 43 0.950 0.000 C17 C16 C18 H18A 0.8193 0.2105 0.2209 43 0.950 0.000 C18 C17 C19 H20A 0.9290 0.3377 0.0319 33 0.980 0.000 C20 C15 H20A H20B 0.9039 0.4765 0.0511 33 0.980 0.000 C20 C15 H20A H20C 0.7945 0.3912 0.0328 33 0.980 0.000 C20 C15 H20A H21A 0.6869 0.3666 0.2427 33 0.980 0.000 C21 C19 H21A H21B 0.6012 0.4105 0.1998 33 0.980 0.000 C21 C19 H21A H21C 0.7076 0.4998 0.2180 33 0.980 0.000 C21 C19 H21A H22A 0.9650 0.7484 0.0472 23 0.990 0.000 C22 Si1 Cr1 H22B 0.9511 0.8651 0.0840 23 0.990 0.000 C22 Si1 Cr1 H23A 1.2290 0.7952 0.1599 33 0.980 0.000 C23 Si1 H23A H23B 1.1202 0.7801 0.1964 33 0.980 0.000 C23 Si1 H23A H23C 1.1187 0.8914 0.1582 33 0.980 0.000 C23 Si1 H23A H24A 1.2552 0.6219 0.1010 33 0.980 0.000 C24 Si1 H24A H24B 1.1630 0.5949 0.0581 33 0.980 0.000 C24 Si1 H24A H24C 1.1615 0.5086 0.1048 33 0.980 0.000 C24 Si1 H24A H25A 0.9925 0.6522 0.2201 23 0.990 0.000 C25 C26 O1 H25B 0.8897 0.5482 0.2131 23