Table 1. Crystal data and structure refinement for 94SRC127. Identification code 94SRC127 Empirical formula C35 H66 Cl2 N2 P2 Se2 Ti Formula weight 853.56 Temperature 120(2) K Wavelength 0.71069 A Crystal system Orthorhombic. Space group Pbca. Unit cell dimensions a = 13.233(7) A b = 17.2161(10) A c = 35.163(11) A Volume 8011(5) A^3 Z 8 Density (calculated) 1.415 Mg/m^3 Absorption coefficient 2.271 mm^-1 F(000) 3552 Crystal size 0.2 x 0.1 x 0.07 mm Theta range for data collection 1.93 to 25.15 deg. Index ranges -15<=h<=10, -19<=k<=19, -41<=l<=40 Reflections collected 36613 Independent reflections 6457 [R(int) = 0.0786] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 6452 / 0 / 398 Goodness-of-fit on F^2 0.971 Final R indices [I>2sigma(I)] R1 = 0.0420, wR2 = 0.0829 R indices (all data) R1 = 0.0736, wR2 = 0.0906 Largest diff. peak and hole 0.736 and -0.365 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 94src127. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Ti(1) -440(1) 229(1) 3556(1) 13(1) Se(1) 1094(1) 843(1) 3942(1) 18(1) Se(2) -825(1) 1495(1) 3160(1) 16(1) Cl(1) -441(1) -854(1) 3950(1) 22(1) Cl(2) -1547(1) -435(1) 3157(1) 20(1) P(1) 1844(1) 313(1) 3462(1) 14(1) P(2) -1761(1) 1653(1) 3659(1) 14(1) N(1) 840(2) -36(2) 3239(1) 13(1) N(2) -1435(2) 860(2) 3891(1) 12(1) C(1) 2538(3) 1090(2) 3184(1) 19(1) C(2) 3149(3) 1611(2) 3453(1) 30(1) C(3) 3242(3) 762(2) 2878(1) 30(1) C(4) 1748(3) 1602(2) 2996(1) 23(1) C(5) 2729(3) -469(2) 3636(1) 20(1) C(6) 2152(3) -982(2) 3914(1) 25(1) C(7) 3628(3) -95(3) 3852(1) 32(1) C(8) 3156(3) -989(2) 3317(1) 25(1) C(9) 982(3) -530(2) 2895(1) 13(1) C(10) 657(3) -1368(2) 2968(1) 18(1) C(11) 791(3) -1872(2) 2613(1) 22(1) C(12) 222(3) -1532(2) 2280(1) 23(1) C(13) 607(3) -718(2) 2197(1) 18(1) C(14) 459(3) -189(2) 2544(1) 18(1) C(15) -3132(3) 1672(2) 3505(1) 22(1) C(16) -3855(3) 1865(3) 3832(1) 31(1) C(17) -3288(3) 2258(3) 3177(1) 33(1) C(18) -3380(3) 867(2) 3343(1) 25(1) C(19) -1416(3) 2580(2) 3919(1) 17(1) C(20) -274(3) 2603(2) 3954(1) 27(1) C(21) -1865(3) 2652(2) 4318(1) 26(1) C(22) -1747(3) 3282(2) 3678(1) 27(1) C(23) -1858(3) 719(2) 4280(1) 17(1) C(24) -2557(3) 4(2) 4292(1) 22(1) C(25) -2969(3) -120(2) 4692(1) 30(1) C(26) -2142(4) -167(3) 4990(1) 36(1) C(27) -1482(4) 548(3) 4977(1) 30(1) C(28) -1027(3) 666(2) 4583(1) 20(1) C(50) -4551(2) 1529(2) 5011(1) 39(1) C(51) -5342(3) 1276(1) 4782(1) 46(2) C(52) -5834(2) 1797(2) 4543(1) 45(2) C(53) -5537(2) 2571(2) 4534(1) 45(1) C(54) -4747(2) 2824(1) 4763(1) 33(1) C(55) -4254(2) 2303(2) 5002(1) 33(1) C(56) -3380(4) 2570(3) 5239(2) 47(1) ________________________________________________________________ Table 3. Selected bond lengths [A] and angles [deg] for 1. _____________________________________________________________ _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Bond lengths [A] and angles [deg] for 94src127. _____________________________________________________________ Ti(1)-N(2) 2.073(3) Ti(1)-N(1) 2.078(3) Ti(1)-Cl(1) 2.3231(12) Ti(1)-Cl(2) 2.3292(13) Ti(1)-Se(2) 2.6379(8) Ti(1)-Se(1) 2.6592(12) Ti(1)-P(2) 3.0320(13) Ti(1)-P(1) 3.044(2) Se(1)-P(1) 2.1602(12) Se(2)-P(2) 2.1665(13) P(1)-N(1) 1.654(3) P(1)-C(5) 1.885(4) P(1)-C(1) 1.894(4) P(02)-N(2) 1.649(3) P(2)-C(15) 1.894(4) P(02)-C(19) 1.896(4) N(1)-C(9) 1.492(5) N(02)-C(23) 1.496(5) C(1)-C(4) 1.518(6) C(01)-C(3) 1.531(6) C(1)-C(2) 1.535(6) C(05)-C(6) 1.524(6) C(5)-C(8) 1.542(6) C(05)-C(7) 1.553(6) C(9)-C(10) 1.527(5) C(09)-C(14) 1.531(5) C(10)-C(11) 1.530(5) C(011)-C(12) 1.512(6) C(12)-C(13) 1.519(5) C(013)-C(14) 1.537(5) C(15)-C(16) 1.534(6) C(015)-C(18) 1.534(5) C(15)-C(17) 1.545(6) C(019)-C(20) 1.517(6) C(19)-C(21) 1.529(6) C(019)-C(22) 1.540(5) C(23)-C(28) 1.534(6) C(023)-C(24) 1.540(5) C(24)-C(25) 1.521(6) C(025)-C(26) 1.518(6) C(26)-C(27) 1.510(6) C(027)-C(28) 1.526(6) C(50)-C(51) 1.39 C(50)-0C(55) 1.39 C(51)-C(52) 1.39 C(52)-C(53) 1.39 C(53)-C(54) 1.39 C(54)-C(55) 1.39 C(55)-C(56) 1.499(5) N(2)-Ti(1)-N(1) 159.56(12) N(2)-Ti(1)-Cl(1) 94.67(9) N(1)-Ti(1)-Cl(1) 98.28(9) N(2)-Ti(1)-Cl(2) 101.54(10) N(1)-Ti(1)-Cl(2) 94.67(10) Cl(1)-Ti(1)-Cl(2) 88.02(4) N(2)-Ti(1)-Se(2) 75.24(9) N(1)-Ti(1)-Se(2) 93.14(9) Cl(1)-Ti(1)-Se(2) 168.17(4) Cl(2)-Ti(1)-Se(2) 88.01(4) N(2)-Ti(1)-Se(1) 89.27(9) N(1)-Ti(1)-Se(1) 74.82(9) Cl(1)-Ti(1)-Se(1) 90.90(4) Cl(2)-Ti(1)-Se(1) 169.18(4) Se(2)-Ti(1)-Se(1) 95.06(3) N(2)-Ti(1)-P(2) 31.02(8) N(1)-Ti(1)-P(2) 135.32(9) Cl(1)-Ti(1)-P(2) 125.29(4) Cl(2)-Ti(1)-P(2) 96.08(5) Se(2)-Ti(1)-P(2) 44.25(3) Se(1)-Ti(1)-P(2) 93.33(4) N(2)-Ti(1)-P(1) 131.91(9) N(1)-Ti(1)-P(1) 30.96(9) Cl(1)-Ti(1)-P(1) 95.94(4) Cl(2)-Ti(1)-P(1) 125.56(5) Se(2)-Ti(1)-P(1) 95.43(3) Se(1)-Ti(1)-P(1) 43.87(3) P(2)-Ti(1)-P(1) 123.18(4) P(1)-Se(1)-Ti(1) 77.57(4) P(2)-Se(2)-Ti(1) 77.58(4) N(1)-P(1)-C(5) 113.2(2) N(1)-P(1)-C(1) 113.7(2) C(5)-P(1)-C(1) 111.7(2) N(1)-P(1)-Se(1) 98.82(12) C(5)-P(1)-Se(1) 109.48(14) C(1)-P(1)-Se(1) 109.09(13) N(1)-P(1)-Ti(1) 40.27(11) C(5)-P(1)-Ti(1) 123.18(13) C(1)-P(1)-Ti(1) 124.85(13) Se(1)-P(1)-Ti(1) 58.56(3) N(2)-P(2)-C(15) 114.0(2) N(2)-P(2)-C(19) 113.3(2) C(15)-P(2)-C(19) 110.7(2) N(2)-P(2)-Se(2) 98.52(12) C(15)-P(2)-Se(2) 108.5(2) C(19)-P(2)-Se(2) 111.03(13) N(2)-P(2)-Ti(1) 40.39(11) C(15)-P(2)-Ti(1) 122.16(13) C(19)-P(2)-Ti(1) 126.84(13) Se(2)-P(2)-Ti(1) 58.17(3) C(9)-N(1)-P(1) 119.3(2) C(9)-N(1)-Ti(1) 131.6(2) P(1)-N(1)-Ti(1) 108.8(2) C(23)-N(2)-P(2) 119.2(2) C(23)-N(2)-Ti(1) 132.2(2) P(2)-N(2)-Ti(1) 108.6(2) C(4)-C(1)-C(3) 109.1(4) C(4)-C(1)-C(2) 106.9(3) C(3)-C(1)-C(2) 109.2(3) C(4)-C(1)-P(1) 107.5(3) C(3)-C(1)-P(1) 113.4(3) C(2)-C(1)-P(1) 110.5(3) C(6)-C(5)-C(8) 108.2(3) C(6)-C(5)-C(7) 108.0(4) C(8)-C(5)-C(7) 108.4(3) C(6)-C(5)-P(1) 108.1(3) C(8)-C(5)-P(1) 114.0(3) C(7)-C(5)-P(1) 109.9(3) N(1)-C(9)-C(10) 111.5(3) N(1)-C(9)-C(14) 112.2(3) C(10)-C(9)-C(14) 111.7(3) C(9)-C(10)-C(11) 111.5(3) C(12)-C(11)-C(10) 110.8(3) C(11)-C(12)-C(13) 109.8(3) C(12)-C(13)-C(14) 110.6(3) C(9)-C(14)-C(13) 110.8(3) C(16)-C(15)-C(18) 109.9(4) C(16)-C(15)-C(17) 109.5(3) C(18)-C(15)-C(17) 106.6(4) C(16)-C(15)-P(2) 112.7(3) C(18)-C(15)-P(2) 107.2(3) C(17)-C(15)-P(2) 110.7(3) C(20)-C(19)-C(21) 108.1(4) C(20)-C(19)-C(22) 107.9(3) C(21)-C(19)-C(22) 109.4(3) C(20)-C(19)-P(2) 107.5(3) C(21)-C(19)-P(2) 114.7(3) C(22)-C(19)-P(2) 109.0(3) N(2)-C(23)-C(28) 112.1(3) N(2)-C(23)-C(24) 112.4(3) C(28)-C(23)-C(24) 111.3(3) C(25)-C(24)-C(23) 110.7(3) C(26)-C(25)-C(24) 112.8(4) C(27)-C(26)-C(25) 110.6(4) C(26)-C(27)-C(28) 111.4(4) C(27)-C(28)-C(23) 110.9(3) C(51)-C(50)-C(55) 120.0 C(50)-C(51)-C(52) 120.0 C(51)-C(52)-C(53) 120.0 C(52)-C(53)-C(54) 120.0 C(53)-C(54)-C(55) 120.0 C(54)-C(55)-C(50) 120.0 C(54)-C(55)-C(56) 120.0(3) C(50)-C(55)-C(56) 120.0(3) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 94src127. The anisotropic displacement factor exponent takes the form: -2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ] _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ Ti(1) 14(1) 9(1) 16(1) 0(1) 2(1) 1(1) Se(1) 18(1) 18(1) 17(1) -4(1) 1(1) 1(1) Se(2) 21(1) 12(1) 16(1) 2(1) 3(1) 2(1) Cl(1) 25(1) 14(1) 27(1) 7(1) 6(1) 3(1) Cl(2) 16(1) 15(1) 30(1) -5(1) 1(1) -2(1) P(1) 14(1) 14(1) 15(1) -1(1) 2(1) 1(1) P(2) 14(1) 11(1) 16(1) -1(1) 1(1) 1(1) N(1) 12(2) 12(2) 15(2) 2(1) 0(2) 2(1) N(2) 10(2) 12(2) 12(2) 1(1) 0(1) 2(1) C(1) 15(2) 21(2) 22(3) -1(2) 4(2) -1(2) C(2) 30(3) 22(3) 38(3) 0(2) -1(2) -11(2) C(3) 30(3) 27(3) 34(3) 1(2) 12(2) -2(2) C(4) 23(3) 17(2) 31(3) 4(2) 5(2) -6(2) C(5) 16(3) 18(2) 26(3) 2(2) -2(2) 5(2) C(6) 29(3) 22(2) 24(3) 8(2) -2(2) 12(2) C(7) 26(3) 33(3) 38(3) 1(2) -6(2) 2(2) C(8) 19(3) 23(3) 33(3) 2(2) 0(2) 8(2) C(9) 12(2) 11(2) 15(2) -1(2) 5(2) 2(2) C(10) 20(3) 12(2) 22(3) -1(2) -2(2) 3(2) C(11) 24(3) 11(2) 30(3) -7(2) 5(2) 2(2) C(12) 27(3) 16(2) 27(3) -7(2) -2(2) 1(2) C(13) 19(2) 17(2) 17(2) -4(2) 0(2) -3(2) C(14) 21(3) 14(2) 18(2) 1(2) 1(2) -2(2) C(15) 19(3) 16(2) 31(3) -5(2) -5(2) 5(2) C(16) 13(3) 35(3) 45(3) -15(2) 0(2) 6(2) C(17) 31(3) 32(3) 36(3) -1(2) -13(2) 6(2) C(18) 14(2) 26(2) 35(3) -9(2) -10(2) 0(2) C(19) 18(2) 13(2) 20(3) -3(2) 0(2) 2(2) C(20) 28(3) 10(2) 44(3) -9(2) -4(2) -4(2) C(21) 26(3) 24(3) 28(3) -9(2) 1(2) -6(2) C(22) 27(3) 13(2) 41(3) 0(2) 6(2) 2(2) C(23) 16(2) 14(2) 22(3) 1(2) 5(2) 2(2) C(24) 23(3) 17(2) 26(3) -1(2) 8(2) -3(2) C(25) 34(3) 20(2) 37(3) -1(2) 21(3) -5(2) C(26) 54(4) 29(3) 26(3) 7(2) 17(3) -1(2) C(27) 41(3) 27(3) 22(3) 2(2) 3(2) 1(2) C(28) 22(3) 18(2) 19(3) 1(2) -1(2) 1(2) C(50) 60(4) 24(3) 32(3) -1(2) 20(3) 3(3) C(51) 55(4) 34(3) 50(4) 3(3) 27(3) -3(3) C(52) 28(3) 59(4) 49(4) -14(3) 13(3) -14(3) C(53) 42(4) 43(3) 49(4) 4(3) 13(3) 4(3) C(54) 35(3) 21(3) 42(3) 4(2) 4(3) -1(2) C(55) 36(3) 33(3) 29(3) -1(2) 13(2) 7(2) C(56) 43(4) 60(4) 39(4) -6(3) 10(3) 13(3) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 94src127. ________________________________________________________________ x y z U(iso) ________________________________________________________________ H(2A) 3689(13) 1316(5) 3564(6) 45 H(2B) 2715(6) 1804(13) 3651(5) 45 H(2C) 3425(17) 2040(9) 3313(2) 45 H(3A) 2873(6) 408(12) 2719(5) 45 H(3B) 3793(11) 492(14) 2997(1) 45 H(3C) 3503(16) 1179(3) 2726(5) 45 H(4A) 1355(13) 1297(4) 2822(5) 35 H(4B) 2077(3) 2014(9) 2861(6) 35 H(4C) 1313(12) 1817(12) 3187(1) 35 H(6A) 1581(11) -1210(12) 3787(2) 38 H(6B) 1922(17) -674(4) 4124(4) 38 H(6C) 2589(6) -1386(9) 4005(6) 38 H(7A) 4057(11) 172(14) 3675(2) 48 H(7B) 4008(13) -493(3) 3979(7) 48 H(7C) 3375(3) 267(12) 4037(5) 48 H(8A) 3442(17) -670(2) 3121(4) 38 H(8B) 2622(5) -1300(11) 3212(5) 38 H(8C) 3670(14) -1322(10) 3420(2) 38 H(9) 1709(3) -540(2) 2840(1) 15 H(10A) -47(3) -1376(2) 3045(1) 22 H(10B) 1056(3) -1582(2) 3174(1) 22 H(11A) 1503(3) -1908(2) 2551(1) 26 H(11B) 544(3) -2392(2) 2664(1) 26 H(12A) -494(3) -1513(2) 2337(1) 28 H(12B) 315(3) -1858(2) 2058(1) 28 H(13A) 245(3) -504(2) 1981(1) 21 H(13B) 1319(3) -740(2) 2132(1) 21 H(14A) 736(3) 321(2) 2491(1) 22 H(14B) -257(3) -129(2) 2595(1) 22 H(16A) -3732(14) 2385(6) 3919(5) 47 H(16B) -3747(14) 1508(10) 4038(3) 47 H(16C) -4541(3) 1823(16) 3745(2) 47 H(17A) -2766(13) 2190(11) 2991(4) 50 H(17B) -3260(21) 2778(3) 3276(2) 50 H(17C) -3936(10) 2171(11) 3061(5) 50 H(18A) -3250(19) 478(3) 3533(3) 37 H(18B) -2965(14) 769(7) 3124(4) 37 H(18C) -4079(6) 849(5) 3271(7) 37 H(20A) -54(3) 2199(10) 4123(6) 41 H(20B) -69(3) 3099(6) 4053(7) 41 H(20C) 24(3) 2527(15) 3708(2) 41 H(21A) -2585(4) 2588(14) 4305(2) 39 H(21B) -1711(16) 3155(6) 4420(3) 39 H(21C) -1582(14) 2258(9) 4479(2) 39 H(22A) -2466(4) 3346(9) 3697(6) 40 H(22B) -1566(18) 3195(7) 3417(2) 40 H(22C) -1417(16) 3742(3) 3769(5) 40 H(23) -2274(3) 1171(2) 4344(1) 21 H(24A) -3114(3) 78(2) 4117(1) 26 H(24B) -2184(3) -453(2) 4213(1) 26 H(25A) -3420(3) 305(2) 4755(1) 36 H(25B) -3359(3) -597(2) 4697(1) 36 H(26A) -2445(4) -214(3) 5241(1) 44 H(26B) -1732(4) -625(3) 4946(1) 44 H(27A) -943(4) 497(3) 5163(1) 36 H(27B) -1882(4) 1000(3) 5045(1) 36 H(28A) -580(3) 235(2) 4524(1) 23 H(28B) -629(3) 1139(2) 4581(1) 23 H(50) -4222(2) 1180(2) 5170(1) 46 H(51) -5541(4) 758(2) 4788(1) 56 H(52) -6363(3) 1628(3) 4390(1) 54 H(53) -5866(3) 2920(2) 4375(1) 53 H(54) -4548(3) 3342(1) 4757(1) 39 H(56A) -2826(9) 2710(18) 5076(2) 71 H(56B) -3174(16) 2159(7) 5406(7) 71 H(56C) -3579(8) 3014(12) 5386(7) 71 ________________________________________________________________