ࡱ> M bjbj== DWWlTpppp<'vxxxxxx$A aE&vvbvv 0,tp"vv0'vv     Table 1. Crystal data and structure refinement for BAS23. Identification code bas23 Empirical formula C8 H13 Cl2 Cr O Si Formula weight 276.17 Temperature 150(2) K Wavelength 0.71073 Crystal system Monoclinic Space group P2(1)/c Unit cell dimensions a = 8.9900(8) a= 90. b = 11.1003(10) b= 107.261(2). c = 12.5960(11) g = 90. Volume 1200.37(18) 3 Z 4 Density (calculated) 1.528 Mg/m3 Absorption coefficient 1.459 mm-1 F(000) 564 Crystal size 0.28 x 0.24 x 0.15 mm3 Theta range for data collection 2.37 to 28.21. Index ranges -11<=h<=11, -14<=k<=13, -16<=l<=7 Reflections collected 6958 Independent reflections 2670 [R(int) = 0.0239] Completeness to theta = 28.21 90.2 % Absorption correction None Max. and min. transmission 0.8108 and 0.6854 Refinement method Full-matrix least-squares on F2 Data / restraints / parameters 2670 / 0 / 118 Goodness-of-fit on F2 1.040 Final R indices [I>2sigma(I)] R1 = 0.0328, wR2 = 0.0804 R indices (all data) R1 = 0.0424, wR2 = 0.0842 Largest diff. peak and hole 0.566 and -0.334 e.-3 Table 2. Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (2x 103) for BAS23. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Si(1) 1514(1) 7710(1) -500(1) 25(1) O(1) 3917(2) 7591(2) 2609(1) 34(1) Cr(1) 4754(1) 6898(1) 1859(1) 23(1) Cl(1) 3469(1) 5148(1) 1520(1) 29(1) Cl(2) 6920(1) 6185(1) 3082(1) 47(1) C(1) 3693(3) 7646(2) 171(2) 23(1) C(2) 4762(3) 6729(2) 13(2) 26(1) C(3) 6262(3) 7015(2) 620(2) 31(1) C(4) 6209(3) 8133(2) 1187(2) 32(1) C(5) 4657(3) 8542(2) 856(2) 28(1) C(6) 1197(3) 9044(2) -1427(2) 37(1) C(7) 524(3) 7922(3) 593(2) 38(1) C(8) 893(3) 6276(2) -1268(2) 40(1) ________________________________________________________________________________ Table 3. Bond lengths [] and angles [] for BAS23. _____________________________________________________ Si(1)-C(6) 1.855(2) Si(1)-C(8) 1.859(3) Si(1)-C(7) 1.862(2) Si(1)-C(1) 1.891(2) O(1)-Cr(1) 1.5717(16) Cr(1)-C(5) 2.207(2) Cr(1)-C(1) 2.218(2) Cr(1)-C(4) 2.229(2) Cr(1)-Cl(1) 2.2353(7) Cr(1)-Cl(2) 2.2382(7) Cr(1)-C(2) 2.336(2) Cr(1)-C(3) 2.355(2) C(1)-C(5) 1.429(3) C(1)-C(2) 1.453(3) C(2)-C(3) 1.376(3) C(3)-C(4) 1.439(3) C(4)-C(5) 1.408(3) C(6)-Si(1)-C(8) 112.91(13) C(6)-Si(1)-C(7) 110.28(12) C(8)-Si(1)-C(7) 110.94(13) C(6)-Si(1)-C(1) 104.82(11) C(8)-Si(1)-C(1) 108.17(11) C(7)-Si(1)-C(1) 109.49(11) O(1)-Cr(1)-C(5) 89.68(9) O(1)-Cr(1)-C(1) 104.26(9) C(5)-Cr(1)-C(1) 37.68(8) O(1)-Cr(1)-C(4) 111.50(9) C(5)-Cr(1)-C(4) 37.00(9) C(1)-Cr(1)-C(4) 62.55(9) O(1)-Cr(1)-Cl(1) 103.19(7) C(5)-Cr(1)-Cl(1) 132.76(6) C(1)-Cr(1)-Cl(1) 95.25(6) C(4)-Cr(1)-Cl(1) 142.21(7) O(1)-Cr(1)-Cl(2) 103.50(7) C(5)-Cr(1)-Cl(2) 124.38(7) C(1)-Cr(1)-Cl(2) 146.20(6) C(4)-Cr(1)-Cl(2) 89.43(7) Cl(1)-Cr(1)-Cl(2) 96.82(3) O(1)-Cr(1)-C(2) 141.33(8) C(5)-Cr(1)-C(2) 60.48(8) C(1)-Cr(1)-C(2) 37.12(7) C(4)-Cr(1)-C(2) 59.68(9) Cl(1)-Cr(1)-C(2) 83.92(6) Cl(2)-Cr(1)-C(2) 113.43(6) O(1)-Cr(1)-C(3) 147.47(9) C(5)-Cr(1)-C(3) 60.49(8) C(1)-Cr(1)-C(3) 60.80(8) C(4)-Cr(1)-C(3) 36.46(9) Cl(1)-Cr(1)-C(3) 106.73(6) Cl(2)-Cr(1)-C(3) 85.48(7) C(2)-Cr(1)-C(3) 34.11(8) C(5)-C(1)-C(2) 105.2(2) C(5)-C(1)-Si(1) 127.35(17) C(2)-C(1)-Si(1) 127.17(17) C(5)-C(1)-Cr(1) 70.75(12) C(2)-C(1)-Cr(1) 75.85(12) Si(1)-C(1)-Cr(1) 122.42(10) C(3)-C(2)-C(1) 109.9(2) C(3)-C(2)-Cr(1) 73.72(14) C(1)-C(2)-Cr(1) 67.03(11) C(2)-C(3)-C(4) 107.7(2) C(2)-C(3)-Cr(1) 72.17(13) C(4)-C(3)-Cr(1) 66.98(13) C(5)-C(4)-C(3) 107.9(2) C(5)-C(4)-Cr(1) 70.66(13) C(3)-C(4)-Cr(1) 76.56(13) C(4)-C(5)-C(1) 108.9(2) C(4)-C(5)-Cr(1) 72.34(13) C(1)-C(5)-Cr(1) 71.57(12) _____________________________________________________________ Table 4. Anisotropic displacement parameters (2x 103) for BAS23. The anisotropic displacement factor exponent takes the form: -2p2[ h2 a*2U11 + ... + 2 h k a* b* U12 ] ______________________________________________________________________________ U11 U22 U33 U23 U13 U12 ______________________________________________________________________________ Si(1) 23(1) 31(1) 21(1) 2(1) 7(1) 1(1) O(1) 38(1) 41(1) 26(1) -7(1) 14(1) -3(1) Cr(1) 21(1) 29(1) 19(1) -1(1) 7(1) 0(1) Cl(1) 34(1) 28(1) 29(1) 0(1) 14(1) -2(1) Cl(2) 25(1) 65(1) 43(1) 21(1) -1(1) -2(1) C(1) 26(1) 26(1) 19(1) 3(1) 9(1) 1(1) C(2) 30(1) 29(1) 22(1) 1(1) 14(1) 3(1) C(3) 26(1) 39(1) 32(1) 5(1) 15(1) 4(1) C(4) 29(1) 38(1) 32(1) 2(1) 11(1) -9(1) C(5) 33(1) 24(1) 26(1) 0(1) 10(1) -1(1) C(6) 31(1) 44(2) 39(1) 15(1) 14(1) 8(1) C(7) 30(1) 58(2) 30(1) 6(1) 14(1) 7(1) C(8) 39(2) 43(2) 33(1) -6(1) 4(1) -9(1) ______________________________________________________________________________ Table 5. Hydrogen coordinates ( x 104) and isotropic displacement parameters (2x 10 3) for BAS23. ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ H(2A) 4451 5993 -459 31 H(3A) 7217 6533 661 37 H(4A) 7133 8599 1638 39 H(5A) 4300 9352 1028 33 H(6A) 82 9135 -1807 56 H(6B) 1758 8935 -1979 56 H(6C) 1585 9767 -984 56 H(7A) -606 7955 245 57 H(7B) 878 8677 992 57 H(7C) 779 7247 1117 57 H(8A) -236 6291 -1622 60 H(8B) 1161 5598 -748 60 H(8C) 1426 6185 -1838 60 ________________________________________________________________________________   68|~BF  _ `  ' ( ^ _ c d p q "#  HL  CJOJQJCJEHOJQJaJCJOJQJaJjCJOJQJUaJj~CJOJQJUaJj-CJOJQJUaJCJOJQJaJ jCJUCJC  HcVH^2M| 4!'|.dh1$7$8$H$ K g  f   r  % G h  @  |.dh1$7$8$H$ @  |.dh1$7$8$H$ 4!'|.dh1$7$8$H$  7 #8Mdy#7K_`a @ |.dh1$7$8$H$ @  |.dh1$7$8$H$ab}7Pj"=Xr  @ |.dh1$7$8$H$ 'AZs (B\x(B\t @ |.dh1$7$8$H$!A%fx|(4ڽ|̂jVZ^2TzF[ J0;eYƸ/]gVrވxP5p$eJjlB)R iH\ qsScCAF^(2kV~-^i,(B;N-gVXf\`5ZLJv@>IL)Foy^$1OvԲaCnc$Rˆr0-x *$ӯB!ˬ1䲽P)|\+~`l ޓa)ބ_[Po-w屬fژ,͞HW,A`0+ITpǪQ5۷׋ )y\BaаtX*6RujXFΪwVh+'%C/H*`Bc7G*+*[l/ZJY?̳'H} 8֐n<u@m#rU~MZ a:j2w,pBT'oj4DfD٩ e5AY~g 2 rS om(E|\aL\f/NZiѱ|A_&o>Sa;̶}<$($Fc3F4~95OWhn|}.|({)*$RK,XXnvjp#lO$vB:@~p ّVHbrw\|gm^pi1bQmik $K/g-mNVd|cu` Q="/ Nƒ4d"8 rђa.($PE{gá׋q&XRT(ˈô#\[D{W ao{em,AMb2$/&.$lV^X}ApmW?ț}[dmSb H<J7}z=z!\৉ *@&|.L. _=j鋀nS \C`aChdlq4OlaT;Z!êg]b2wzEC%za+Q}͂ݷ4Kv^AîZpK~њyj^27'ʿeM#ȯ37<3MRF7 ‘B ( $?z|q00Ԇdxަ/rqGmjuԃ̫8tpRl,"Β<Ѧ~휍E$;k^3!^G_Y0׃U-/d\S,)_JOoU&q(>e-Xi}UV8 ?|Ik 4;M7Q^4wKai9+ 0rjcդ{o ];|IX,WeYF* YF]Ga)pe&">64 'nU)̓ia<@T/U꘲ pxR:4k߮گәR_nzG[9H% =5$P(7:if <.Xfլ}rz22 [\Oё|9B(P- V=NvFD 뢞9<".fec8eu\Oj$dy Hs9YaXOYXP!\#tl)U}75AZԸcp~zʋ?P~wS+QT^}e@H,+_Bg"e+@nTQ@=+75nc8LBD5:XjRbQ(3k. 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