Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 Table 1. Crystal data and structure refinement for sx444. Identification code sx444 Empirical formula C40 H52 N4 O10 Sn4 Formula weight 1223.62 Temperature 223(2) K Wavelength 0.71073 A Crystal system, space group Monoclinic, C2/c Unit cell dimensions a = 25.532(4) A alpha = 90 deg. b = 10.6914(15) A beta = 92.325(19) deg. c = 16.236(5) A gamma = 90 deg. Volume 4428.4(16) A^3 Z, Calculated density 4, 1.835 Mg/m^3 Absorption coefficient 2.288 mm^-1 F(000) 2400 Crystal size 0.38 x 0.26 x 0.08 mm Theta range for data collection 2.07 to 23.00 deg. Limiting indices -1<=h<=28, -1<=k<=11, -17<=l<=17 Reflections collected / unique 3763 / 3090 [R(int) = 0.0264] Completeness to theta = 23.00 99.9 % Absorption correction Semi-empirical Max. and min. transmission 1.000 and 0.765 Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 3090 / 91 / 294 Goodness-of-fit on F^2 1.060 Final R indices [I>2sigma(I)] R1 = 0.0351, wR2 = 0.0803 R indices (all data) R1 = 0.0496, wR2 = 0.0924 Largest diff. peak and hole 0.889 and -0.921 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for sx444. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Sn(1) 4628(1) 1000(1) 3339(1) 29(1) Sn(2) 4443(1) 3163(1) 1879(1) 29(1) N(1) 4697(2) 3033(5) 3215(3) 28(1) C(11) 4416(3) 3860(6) 3728(4) 25(2) C(12) 4647(3) 4989(6) 3999(4) 26(2) C(13) 4374(3) 5783(7) 4490(5) 32(2) C(14) 3874(3) 5495(7) 4731(4) 32(2) C(15) 3646(3) 4401(7) 4457(5) 34(2) C(16) 3917(3) 3577(7) 3962(4) 30(2) O(131) 4569(2) 6900(4) 4788(3) 40(1) C(132) 5038(3) 7359(7) 4448(5) 43(2) O(151) 3150(2) 4020(5) 4626(3) 41(1) C(152) 2885(3) 4724(9) 5214(6) 61(3) N(2) 4539(2) 1108(5) 1981(3) 27(1) C(21) 4211(3) 261(7) 1534(4) 30(2) C(22) 4126(3) -937(7) 1858(4) 32(2) C(23) 3819(3) -1786(6) 1415(5) 32(2) C(24) 3593(3) -1476(7) 653(5) 34(2) C(25) 3684(3) -306(7) 341(4) 29(2) C(26) 3988(3) 567(7) 765(4) 30(2) O(231) 3717(2) -2980(5) 1676(3) 49(2) C(232) 3947(4) -3357(7) 2442(5) 53(2) O(251) 3447(2) -88(5) -420(3) 43(1) C(252) 3476(4) 1135(8) -748(5) 54(2) O(31) 2627(7) 1266(13) 2644(10) 212(5) C(32) 2576(7) 2728(14) 2718(9) 126(4) C(33) 2968(11) 3030(20) 2241(17) 100(6) C(34) 3328(8) 2096(15) 2333(11) 71(5) C(35) 3075(13) 1080(30) 2340(20) 131(7) C(33) 2589(12) 3020(30) 1871(16) 98(7) C(34) 2752(14) 2170(30) 1470(20) 116(8) C(35) 2657(18) 1080(30) 1720(30) 165(9) ________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for sx444. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(12) 4986 5200 3844 31 H(14) 3694 6039 5076 39 H(16) 3758 2824 3788 35 H(13A) 5329 6816 4610 64 H(13B) 5109 8199 4651 64 H(13C) 4997 7376 3851 64 H(15A) 3090 4736 5730 91 H(15B) 2546 4348 5301 91 H(15C) 2836 5573 5015 91 H(22) 4277 -1160 2375 38 H(24) 3382 -2054 356 41 H(26) 4044 1361 536 36 H(23A) 4324 -3246 2436 80 H(23B) 3868 -4231 2536 80 H(23C) 3807 -2854 2879 80 H(25A) 3321 1723 -373 82 H(25B) 3287 1166 -1278 82 H(25C) 3840 1355 -818 82 H(32A) 2237 3034 2497 151 H(32B) 2635 3020 3287 151 H(32C) 2245 2979 2955 151 H(32D) 2871 3098 3037 151 H(33A) 3122 3835 2413 120 H(33B) 2842 3099 1664 120 H(34A) 3566 2104 1875 85 H(34B) 3534 2200 2850 85 H(35A) 3271 457 2671 157 H(35B) 3028 755 1776 157 H(33C) 2234 3230 1665 118 H(33D) 2811 3753 1801 118 H(34C) 3133 2260 1445 139 H(34D) 2605 2248 904 139 H(35C) 2939 501 1589 198 H(35D) 2325 768 1477 198 Table 3. Bond lengths [A] and angles [deg] for sx444. _____________________________________________________________ Sn(1)-N(1) 2.191(6) Sn(1)-N(2)#1 2.211(6) Sn(1)-N(2) 2.211(6) Sn(2)-N(1)#1 2.213(6) Sn(2)-N(2) 2.216(5) Sn(2)-N(1) 2.242(6) N(1)-C(11) 1.427(8) N(1)-Sn(2)#1 2.213(6) C(11)-C(16) 1.379(10) C(11)-C(12) 1.406(9) C(12)-C(13) 1.373(10) C(13)-O(131) 1.374(8) C(13)-C(14) 1.386(10) C(14)-C(15) 1.372(10) C(15)-O(151) 1.369(9) C(15)-C(16) 1.394(10) O(131)-C(132) 1.426(9) O(151)-C(152) 1.410(9) N(2)-C(21) 1.415(9) N(2)-Sn(1)#1 2.211(6) C(21)-C(26) 1.389(10) C(21)-C(22) 1.405(10) C(22)-C(23) 1.381(10) C(23)-O(231) 1.373(8) C(23)-C(24) 1.385(10) C(24)-C(25) 1.374(10) C(25)-O(251) 1.373(8) C(25)-C(26) 1.381(10) O(231)-C(232) 1.411(10) O(251)-C(252) 1.415(9) O(31)-C(35) 1.28(3) O(31)-C(35) 1.52(4) O(31)-C(32) 1.573(19) C(32)-C(33) 1.33(3) C(32)-C(33) 1.41(3) C(33)-C(34) 1.36(3) C(34)-C(35) 1.27(3) C(33)-C(34) 1.20(3) C(34)-C(35) 1.26(4) N(1)-Sn(1)-N(2)#1 81.1(2) N(1)-Sn(1)-N(2) 82.0(2) N(2)#1-Sn(1)-N(2) 79.9(2) N(1)#1-Sn(2)-N(2) 80.5(2) N(1)#1-Sn(2)-N(1) 79.2(2) N(2)-Sn(2)-N(1) 80.8(2) C(11)-N(1)-Sn(1) 121.1(4) C(11)-N(1)-Sn(2)#1 121.6(4) Sn(1)-N(1)-Sn(2)#1 98.7(2) C(11)-N(1)-Sn(2) 113.2(4) Sn(1)-N(1)-Sn(2) 97.4(2) Sn(2)#1-N(1)-Sn(2) 100.3(2) C(16)-C(11)-C(12) 118.8(6) C(16)-C(11)-N(1) 121.1(6) C(12)-C(11)-N(1) 120.1(6) C(13)-C(12)-C(11) 119.8(7) O(131)-C(13)-C(12) 123.8(7) O(131)-C(13)-C(14) 114.8(6) C(12)-C(13)-C(14) 121.4(7) C(15)-C(14)-C(13) 118.8(7) O(151)-C(15)-C(14) 124.9(7) O(151)-C(15)-C(16) 114.3(7) C(14)-C(15)-C(16) 120.8(7) C(11)-C(16)-C(15) 120.4(7) C(13)-O(131)-C(132) 117.4(6) C(15)-O(151)-C(152) 116.8(6) C(21)-N(2)-Sn(1)#1 113.7(4) C(21)-N(2)-Sn(1) 120.9(4) Sn(1)#1-N(2)-Sn(1) 99.8(2) C(21)-N(2)-Sn(2) 122.3(4) Sn(1)#1-N(2)-Sn(2) 98.0(2) Sn(1)-N(2)-Sn(2) 97.6(2) C(26)-C(21)-C(22) 119.2(7) C(26)-C(21)-N(2) 121.5(6) C(22)-C(21)-N(2) 119.3(6) C(23)-C(22)-C(21) 119.8(7) O(231)-C(23)-C(22) 124.1(7) O(231)-C(23)-C(24) 114.9(7) C(22)-C(23)-C(24) 121.0(7) C(25)-C(24)-C(23) 118.6(7) O(251)-C(25)-C(24) 114.3(6) O(251)-C(25)-C(26) 123.6(7) C(24)-C(25)-C(26) 122.1(7) C(25)-C(26)-C(21) 119.4(7) C(23)-O(231)-C(232) 117.4(6) C(25)-O(251)-C(252) 117.9(6) C(35)-O(31)-C(35) 61(2) C(35)-O(31)-C(32) 105.3(17) C(35)-O(31)-C(32) 102.2(18) C(33)-C(32)-C(33) 48.0(16) C(33)-C(32)-O(31) 97.6(15) C(33)-C(32)-O(31) 97.9(16) C(32)-C(33)-C(34) 106(2) C(35)-C(34)-C(33) 107(2) C(34)-C(35)-O(31) 109(2) C(34)-C(33)-C(32) 113(3) C(33)-C(34)-C(35) 116(4) C(34)-C(35)-O(31) 103(3) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x+1,y,-z+1/2 Table 4. Anisotropic displacement parameters (A^2 x 10^3) for sx444. 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 _______________________________________________________________________ Sn(1) 34(1) 25(1) 30(1) 1(1) 6(1) -2(1) Sn(2) 31(1) 24(1) 31(1) 1(1) 2(1) 1(1) N(1) 32(3) 23(3) 29(3) -8(3) 5(3) 5(3) C(11) 29(4) 23(4) 23(4) 4(3) -1(3) 4(3) C(12) 32(4) 21(4) 25(4) 0(3) 4(3) 0(3) C(13) 33(4) 28(4) 37(4) -3(3) 3(4) 2(3) C(14) 34(4) 35(4) 29(4) 1(3) 5(3) 2(4) C(15) 27(4) 37(4) 38(4) 10(4) 1(3) 7(4) C(16) 24(4) 27(4) 38(4) -3(3) -1(3) 0(3) O(131) 43(3) 25(3) 53(3) -8(3) 7(3) 0(2) C(132) 48(5) 31(4) 49(5) -1(4) 4(4) -16(4) O(151) 28(3) 41(3) 55(3) 0(3) 14(3) 4(3) C(152) 37(5) 61(6) 87(7) -14(6) 35(5) 5(5) N(2) 27(3) 17(3) 36(3) 0(3) 2(3) 4(3) C(21) 24(4) 27(4) 38(4) -7(3) 8(3) -4(3) C(22) 38(4) 29(4) 28(4) -2(3) -4(3) -7(4) C(23) 38(4) 19(4) 38(4) 0(3) 6(4) 1(3) C(24) 32(4) 34(4) 37(4) -4(4) 5(4) -4(4) C(25) 25(4) 35(4) 28(4) -2(3) -3(3) 2(3) C(26) 29(4) 28(4) 32(4) 7(3) -1(3) -2(3) O(231) 68(4) 29(3) 48(3) 8(3) -10(3) -15(3) C(232) 78(7) 29(4) 52(5) 6(4) 1(5) -7(5) O(251) 46(3) 43(3) 40(3) 1(3) -7(3) -10(3) C(252) 71(6) 44(5) 46(5) 12(4) -21(5) -4(5) O(31) 244(12) 145(8) 256(12) 44(9) 114(11) 7(9) C(32) 130(10) 135(9) 114(8) -9(8) 21(8) 42(9) C(33) 109(14) 82(9) 108(14) 6(11) 2(11) 32(9) C(34) 105(10) 51(9) 55(10) -31(8) -16(9) 29(7) C(35) 157(17) 72(9) 166(19) 3(14) 48(15) 11(10) C(33) 102(17) 106(11) 84(11) -25(9) -31(13) 64(14) C(34) 150(20) 77(12) 123(12) -27(10) -1(15) 53(14) C(35) 170(20) 93(10) 240(16) -36(13) 95(19) -19(18) _______________________________________________________________________ ________________________________________________________________ Table 1. Crystal data and structure refinement for sx445. Identification code sx445 Empirical formula C40 H52 N4 O6 Sn4 Formula weight 1159.62 Temperature 223(2) K Wavelength 0.71073 A Crystal system, space group Monoclinic, C2/c Unit cell dimensions a = 26.134(7) A alpha = 90 deg. b = 13.7154(18) A beta = 117.453(15) deg. c = 26.706(4) A gamma = 90 deg. Volume 8494(3) A^3 Z, Calculated density 8, 1.814 Mg/m^3 Absorption coefficient 2.374 mm^-1 F(000) 4544 Crystal size 0.20mm x 0.36mm x 0.38mm mm Theta range for data collection 1.80 to 23.00 deg. Limiting indices -28<=h<=1, -1<=k<=15, -26<=l<=29 Reflections collected / unique 6914 / 5843 [R(int) = 0.0727] Completeness to theta = 23.00 98.9 % Absorption correction Semi-emprical Max. and min. transmission 1.000 and 0.801 Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 5843 / 57 / 516 Goodness-of-fit on F^2 0.983 Final R indices [I>2sigma(I)] R1 = 0.0569, wR2 = 0.1370 R indices (all data) R1 = 0.1061, wR2 = 0.1699 Largest diff. peak and hole 1.214 and -1.291 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for sx445. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Sn(1) 1804(1) 590(1) 1907(1) 31(1) Sn(2) 1789(1) -1815(1) 1992(1) 34(1) Sn(3) 779(1) -531(1) 2158(1) 34(1) Sn(4) 689(1) -679(1) 890(1) 30(1) N(1) 1735(4) -542(8) 2472(4) 29(2) C(11) 2058(5) -507(10) 3057(5) 29(3) C(12) 2093(6) 350(10) 3375(6) 39(4) C(13) 2429(6) 302(12) 3965(6) 43(4) C(14) 2698(6) -517(12) 4246(6) 42(4) C(15) 2657(6) -1349(10) 3950(5) 33(3) C(16) 2338(5) -1348(11) 3356(6) 38(3) C(121) 1804(7) 1279(12) 3103(6) 59(5) O(151) 2905(5) -2229(9) 4173(4) 60(3) C(152) 3162(7) -2327(13) 4769(5) 69(6) N(2) 1667(4) -692(7) 1356(4) 28(2) C(21) 1978(6) -822(9) 1033(6) 38(4) C(22) 1897(6) -1644(9) 704(5) 31(3) C(23) 2219(6) -1768(11) 416(6) 42(4) C(24) 2602(6) -1055(11) 434(6) 44(4) C(25) 2676(5) -245(10) 762(5) 37(3) C(26) 2369(6) -130(10) 1039(5) 35(3) C(221) 1483(7) -2481(11) 638(7) 52(4) O(251) 3075(5) 409(8) 753(5) 63(3) C(252) 3267(7) 1160(12) 1160(7) 76(6) N(3) 824(4) -1682(8) 1598(4) 34(3) C(31) 497(5) -2560(10) 1474(6) 33(3) C(32) 472(6) -3114(10) 1920(6) 37(3) C(33) 142(7) -3954(12) 1755(6) 50(4) C(34) -175(6) -4262(11) 1199(7) 45(4) C(35) -142(6) -3710(9) 767(6) 37(3) C(36) 184(5) -2879(9) 914(5) 30(3) C(321) 797(8) -2871(12) 2521(6) 63(5) O(351) -419(4) -3936(7) 207(4) 49(3) C(352) -690(7) -4852(10) 42(7) 65(5) N(4) 841(4) 435(7) 1545(4) 23(2) C(41) 481(6) 1289(10) 1356(6) 36(3) C(42) 435(6) 1871(10) 907(5) 30(3) C(43) 64(6) 2625(10) 759(6) 42(4) C(44) -285(6) 2846(10) 1001(6) 40(4) C(45) -230(6) 2325(10) 1452(7) 46(4) C(46) 157(6) 1549(10) 1643(7) 43(4) C(421) 807(6) 1720(10) 628(6) 42(4) O(451) -538(5) 2443(8) 1754(5) 71(4) C(452) -750(20) 3385(19) 1760(30) 82(17) C(453) -960(30) 3180(50) 1550(30) 100(20) O(51) 2962(5) -348(9) 2513(5) 71(3) C(52) 3320(8) -1005(14) 2421(8) 76(6) C(53) 3860(30) -1130(50) 2930(20) 66(14) C(53) 3650(30) -1500(40) 2950(20) 76(14) C(54) 3756(7) -705(16) 3367(8) 80(5) C(55) 3313(8) 99(15) 3020(9) 74(5) O(61) -380(4) -680(8) 1005(5) 68(3) C(62) -783(6) -11(12) 605(6) 49(4) C(63) -1238(8) 112(14) 802(9) 72(5) C(64) -1243(7) -865(14) 1051(8) 70(5) C(65) -701(6) -1324(13) 1177(7) 58(4) ________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for sx445. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(13) 2468 872 4176 52 H(14) 2912 -512 4641 50 H(16) 2312 -1926 3156 45 H(12A) 2063 1669 3017 88 H(12B) 1703 1638 3359 88 H(12C) 1457 1137 2758 88 H(15A) 3507 -1927 4940 104 H(15B) 3265 -3004 4871 104 H(15C) 2892 -2118 4902 104 H(23) 2177 -2341 207 51 H(24) 2807 -1124 226 53 H(26) 2419 446 1248 42 H(22A) 1566 -2732 1007 78 H(22B) 1531 -2997 415 78 H(22C) 1089 -2244 449 78 H(25A) 2939 1460 1175 115 H(25B) 3472 1647 1058 115 H(25C) 3524 889 1527 115 H(33) 130 -4344 2038 60 H(34) -406 -4824 1112 54 H(36) 200 -2504 626 36 H(32A) 1189 -2697 2608 94 H(32B) 803 -3431 2746 94 H(32C) 615 -2326 2607 94 H(35A) -400 -5361 165 98 H(35B) -915 -4872 -366 98 H(35C) -943 -4954 213 98 H(43) 42 3032 466 50 H(44) -557 3352 856 47 H(46) 205 1196 1964 51 H(42A) 641 2057 269 63 H(42B) 834 1028 568 63 H(42C) 1189 1976 867 63 H(45A) -438 3792 2022 122 H(45B) -1050 3346 1877 122 H(45C) -907 3664 1385 122 H(45D) -777 3814 1608 152 H(45E) -1185 3161 1761 152 H(45F) -1217 3082 1155 152 H(52A) 3398 -759 2118 91 H(52B) 3125 -1635 2302 91 H(52C) 3575 -656 2304 91 H(52D) 3089 -1474 2126 91 H(53A) 3958 -1827 3007 79 H(53B) 4177 -799 2902 79 H(53C) 4018 -1747 2978 92 H(53D) 3437 -2039 3001 92 H(54A) 4107 -425 3670 96 H(54B) 3590 -1177 3527 96 H(54C) 4152 -459 3522 96 H(54D) 3687 -937 3678 96 H(55A) 3090 311 3211 89 H(55B) 3508 666 2962 89 H(62A) -951 -279 222 59 H(62B) -597 613 612 59 H(63A) -1133 629 1085 86 H(63B) -1615 263 485 86 H(64A) -1284 -789 1395 84 H(64B) -1565 -1260 781 84 H(65A) -485 -1455 1582 70 H(65B) -769 -1945 974 70 ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for sx445. _____________________________________________________________ Sn(1)-N(2) 2.213(10) Sn(1)-N(1) 2.229(10) Sn(1)-N(4) 2.252(10) Sn(2)-N(2) 2.205(10) Sn(2)-N(1) 2.209(10) Sn(2)-N(3) 2.246(10) Sn(3)-N(4) 2.169(9) Sn(3)-N(3) 2.217(11) Sn(3)-N(1) 2.239(10) Sn(3)-Sn(4) 3.2920(13) Sn(4)-N(4) 2.217(9) Sn(4)-N(3) 2.231(11) Sn(4)-N(2) 2.268(10) N(1)-C(11) 1.392(15) C(11)-C(16) 1.402(18) C(11)-C(12) 1.428(18) C(12)-C(13) 1.408(19) C(12)-C(121) 1.49(2) C(13)-C(14) 1.35(2) C(13)-H(13) 0.9400 C(14)-C(15) 1.364(19) C(14)-H(14) 0.9400 C(15)-O(151) 1.369(16) C(15)-C(16) 1.411(17) C(16)-H(16) 0.9400 C(121)-H(12A) 0.9700 C(121)-H(12B) 0.9700 C(121)-H(12C) 0.9700 O(151)-C(152) 1.418(13) C(152)-H(15A) 0.9700 C(152)-H(15B) 0.9700 C(152)-H(15C) 0.9700 N(2)-C(21) 1.443(17) C(21)-C(22) 1.384(18) C(21)-C(26) 1.390(18) C(22)-C(23) 1.390(18) C(22)-C(221) 1.531(19) C(23)-C(24) 1.384(19) C(23)-H(23) 0.9400 C(24)-C(25) 1.371(18) C(24)-H(24) 0.9400 C(25)-C(26) 1.328(18) C(25)-O(251) 1.383(15) C(26)-H(26) 0.9400 C(221)-H(22A) 0.9700 C(221)-H(22B) 0.9700 C(221)-H(22C) 0.9700 O(251)-C(252) 1.411(14) C(252)-H(25A) 0.9700 C(252)-H(25B) 0.9700 C(252)-H(25C) 0.9700 N(3)-C(31) 1.426(16) C(31)-C(36) 1.404(18) C(31)-C(32) 1.439(17) C(32)-C(33) 1.384(19) C(32)-C(321) 1.466(19) C(33)-C(34) 1.39(2) C(33)-H(33) 0.9400 C(34)-C(35) 1.415(19) C(34)-H(34) 0.9400 C(35)-C(36) 1.368(17) C(35)-O(351) 1.363(15) C(36)-H(36) 0.9400 C(321)-H(32A) 0.9700 C(321)-H(32B) 0.9700 C(321)-H(32C) 0.9700 O(351)-C(352) 1.410(13) C(352)-H(35A) 0.9700 C(352)-H(35B) 0.9700 C(352)-H(35C) 0.9700 N(4)-C(41) 1.439(15) C(41)-C(42) 1.398(18) C(41)-C(46) 1.426(19) C(42)-C(43) 1.346(18) C(42)-C(421) 1.487(18) C(43)-C(44) 1.372(19) C(43)-H(43) 0.9400 C(44)-C(45) 1.350(19) C(44)-H(44) 0.9400 C(45)-O(451) 1.387(16) C(45)-C(46) 1.393(18) C(46)-H(46) 0.9400 C(421)-H(42A) 0.9700 C(421)-H(42B) 0.9700 C(421)-H(42C) 0.9700 O(451)-C(452) 1.407(17) O(451)-C(453) 1.414(17) C(452)-H(45A) 0.9730 C(452)-H(45B) 0.9722 C(452)-H(45C) 0.9725 C(453)-H(45D) 0.9700 C(453)-H(45E) 0.9700 C(453)-H(45F) 0.9700 O(51)-C(55) 1.38(2) O(51)-C(52) 1.401(19) C(52)-C(53) 1.44(5) C(52)-C(53) 1.45(5) C(52)-H(52A) 0.9800 C(52)-H(52B) 0.9800 C(52)-H(52C) 0.9800 C(52)-H(52D) 0.9800 C(53)-C(54) 1.44(5) C(53)-H(53A) 0.9800 C(53)-H(53B) 0.9800 C(53)-C(54) 1.49(5) C(53)-H(53C) 0.9800 C(53)-H(53D) 0.9800 C(54)-C(55) 1.56(3) C(54)-H(54A) 0.9800 C(54)-H(54B) 0.9800 C(54)-H(54C) 0.9800 C(54)-H(54D) 0.9800 C(55)-H(55A) 0.9800 C(55)-H(55B) 0.9800 O(61)-C(65) 1.433(18) O(61)-C(62) 1.433(18) C(62)-C(63) 1.51(2) C(62)-H(62A) 0.9800 C(62)-H(62B) 0.9800 C(63)-C(64) 1.50(2) C(63)-H(63A) 0.9800 C(63)-H(63B) 0.9800 C(64)-C(65) 1.44(2) C(64)-H(64A) 0.9800 C(64)-H(64B) 0.9800 C(65)-H(65A) 0.9800 C(65)-H(65B) 0.9800 N(2)-Sn(1)-N(1) 81.9(4) N(2)-Sn(1)-N(4) 80.4(3) N(1)-Sn(1)-N(4) 78.6(3) N(2)-Sn(2)-N(1) 82.5(4) N(2)-Sn(2)-N(3) 81.3(4) N(1)-Sn(2)-N(3) 81.4(4) N(4)-Sn(3)-N(3) 83.1(4) N(4)-Sn(3)-N(1) 80.1(4) N(3)-Sn(3)-N(1) 81.4(4) N(4)-Sn(3)-Sn(4) 41.9(2) N(3)-Sn(3)-Sn(4) 42.4(3) N(1)-Sn(3)-Sn(4) 85.6(2) N(4)-Sn(4)-N(3) 81.7(4) N(4)-Sn(4)-N(2) 80.0(3) N(3)-Sn(4)-N(2) 80.3(4) N(4)-Sn(4)-Sn(3) 40.8(2) N(3)-Sn(4)-Sn(3) 42.1(3) N(2)-Sn(4)-Sn(3) 84.7(3) C(11)-N(1)-Sn(2) 120.7(9) C(11)-N(1)-Sn(1) 122.6(8) Sn(2)-N(1)-Sn(1) 96.4(4) C(11)-N(1)-Sn(3) 114.5(7) Sn(2)-N(1)-Sn(3) 98.4(4) Sn(1)-N(1)-Sn(3) 99.5(4) N(1)-C(11)-C(16) 119.9(12) N(1)-C(11)-C(12) 122.4(12) C(16)-C(11)-C(12) 117.6(12) C(13)-C(12)-C(11) 117.7(13) C(13)-C(12)-C(121) 119.9(13) C(11)-C(12)-C(121) 122.4(12) C(14)-C(13)-C(12) 123.7(15) C(14)-C(13)-H(13) 118.2 C(12)-C(13)-H(13) 118.1 C(13)-C(14)-C(15) 119.4(13) C(13)-C(14)-H(14) 120.3 C(15)-C(14)-H(14) 120.3 C(14)-C(15)-O(151) 126.2(11) C(14)-C(15)-C(16) 119.9(12) O(151)-C(15)-C(16) 114.0(12) C(11)-C(16)-C(15) 121.7(13) C(11)-C(16)-H(16) 119.2 C(15)-C(16)-H(16) 119.2 C(12)-C(121)-H(12A) 109.5 C(12)-C(121)-H(12B) 109.5 H(12A)-C(121)-H(12B) 109.5 C(12)-C(121)-H(12C) 109.5 H(12A)-C(121)-H(12C) 109.5 H(12B)-C(121)-H(12C) 109.5 C(15)-O(151)-C(152) 117.2(11) O(151)-C(152)-H(15A) 109.5 O(151)-C(152)-H(15B) 109.5 H(15A)-C(152)-H(15B) 109.5 O(151)-C(152)-H(15C) 109.4 H(15A)-C(152)-H(15C) 109.5 H(15B)-C(152)-H(15C) 109.5 C(21)-N(2)-Sn(2) 116.9(8) C(21)-N(2)-Sn(1) 122.1(8) Sn(2)-N(2)-Sn(1) 96.9(4) C(21)-N(2)-Sn(4) 118.4(8) Sn(2)-N(2)-Sn(4) 98.9(4) Sn(1)-N(2)-Sn(4) 98.9(4) C(22)-C(21)-C(26) 117.4(13) C(22)-C(21)-N(2) 121.0(12) C(26)-C(21)-N(2) 121.6(12) C(21)-C(22)-C(23) 119.8(13) C(21)-C(22)-C(221) 125.3(12) C(23)-C(22)-C(221) 114.8(11) C(24)-C(23)-C(22) 120.4(13) C(24)-C(23)-H(23) 119.8 C(22)-C(23)-H(23) 119.8 C(25)-C(24)-C(23) 118.9(12) C(25)-C(24)-H(24) 120.6 C(23)-C(24)-H(24) 120.6 C(26)-C(25)-C(24) 120.5(12) C(26)-C(25)-O(251) 125.8(12) C(24)-C(25)-O(251) 113.6(12) C(25)-C(26)-C(21) 122.9(13) C(25)-C(26)-H(26) 118.5 C(21)-C(26)-H(26) 118.6 C(22)-C(221)-H(22A) 109.5 C(22)-C(221)-H(22B) 109.4 H(22A)-C(221)-H(22B) 109.5 C(22)-C(221)-H(22C) 109.5 H(22A)-C(221)-H(22C) 109.5 H(22B)-C(221)-H(22C) 109.5 C(25)-O(251)-C(252) 117.7(11) O(251)-C(252)-H(25A) 109.5 O(251)-C(252)-H(25B) 109.4 H(25A)-C(252)-H(25B) 109.5 O(251)-C(252)-H(25C) 109.5 H(25A)-C(252)-H(25C) 109.5 H(25B)-C(252)-H(25C) 109.5 C(31)-N(3)-Sn(3) 123.0(8) C(31)-N(3)-Sn(4) 118.8(8) Sn(3)-N(3)-Sn(4) 95.5(4) C(31)-N(3)-Sn(2) 117.7(8) Sn(3)-N(3)-Sn(2) 98.0(4) Sn(4)-N(3)-Sn(2) 98.8(4) C(36)-C(31)-N(3) 120.0(11) C(36)-C(31)-C(32) 119.5(12) N(3)-C(31)-C(32) 120.4(12) C(33)-C(32)-C(31) 115.7(13) C(33)-C(32)-C(321) 120.0(12) C(31)-C(32)-C(321) 124.2(13) C(32)-C(33)-C(34) 124.8(13) C(32)-C(33)-H(33) 117.6 C(34)-C(33)-H(33) 117.6 C(33)-C(34)-C(35) 118.5(13) C(33)-C(34)-H(34) 120.8 C(35)-C(34)-H(34) 120.7 C(36)-C(35)-O(351) 116.7(12) C(36)-C(35)-C(34) 118.5(12) O(351)-C(35)-C(34) 124.8(11) C(35)-C(36)-C(31) 122.9(12) C(35)-C(36)-H(36) 118.5 C(31)-C(36)-H(36) 118.6 C(32)-C(321)-H(32A) 109.5 C(32)-C(321)-H(32B) 109.5 H(32A)-C(321)-H(32B) 109.5 C(32)-C(321)-H(32C) 109.5 H(32A)-C(321)-H(32C) 109.5 H(32B)-C(321)-H(32C) 109.5 C(35)-O(351)-C(352) 118.9(11) O(351)-C(352)-H(35A) 109.5 O(351)-C(352)-H(35B) 109.4 H(35A)-C(352)-H(35B) 109.5 O(351)-C(352)-H(35C) 109.5 H(35A)-C(352)-H(35C) 109.5 H(35B)-C(352)-H(35C) 109.5 C(41)-N(4)-Sn(3) 119.9(8) C(41)-N(4)-Sn(4) 115.7(7) Sn(3)-N(4)-Sn(4) 97.3(4) C(41)-N(4)-Sn(1) 119.6(8) Sn(3)-N(4)-Sn(1) 101.0(4) Sn(4)-N(4)-Sn(1) 99.3(4) C(42)-C(41)-C(46) 118.7(12) C(42)-C(41)-N(4) 123.3(11) C(46)-C(41)-N(4) 118.0(12) C(43)-C(42)-C(41) 117.2(12) C(43)-C(42)-C(421) 120.6(12) C(41)-C(42)-C(421) 122.1(12) C(42)-C(43)-C(44) 125.1(13) C(42)-C(43)-H(43) 117.4 C(44)-C(43)-H(43) 117.4 C(45)-C(44)-C(43) 118.9(13) C(45)-C(44)-H(44) 120.6 C(43)-C(44)-H(44) 120.5 C(44)-C(45)-O(451) 127.3(12) C(44)-C(45)-C(46) 119.5(12) O(451)-C(45)-C(46) 113.2(13) C(45)-C(46)-C(41) 120.3(14) C(45)-C(46)-H(46) 119.9 C(41)-C(46)-H(46) 119.8 C(42)-C(421)-H(42A) 109.5 C(42)-C(421)-H(42B) 109.5 H(42A)-C(421)-H(42B) 109.5 C(42)-C(421)-H(42C) 109.4 H(42A)-C(421)-H(42C) 109.5 H(42B)-C(421)-H(42C) 109.5 C(452)-O(451)-C(45) 116.7(16) C(452)-O(451)-C(453) 26(3) C(45)-O(451)-C(453) 115.3(15) O(451)-C(452)-H(45A) 111.3 O(451)-C(452)-H(45B) 108.4 O(451)-C(452)-H(45C) 109.5 O(451)-C(453)-H(45D) 113.5 O(451)-C(453)-H(45E) 109.8 H(45D)-C(453)-H(45E) 109.5 O(451)-C(453)-H(45F) 105.0 H(45D)-C(453)-H(45F) 109.5 H(45E)-C(453)-H(45F) 109.5 C(55)-O(51)-C(52) 105.2(13) O(51)-C(52)-C(53) 106(3) O(51)-C(52)-C(53) 111(2) C(53)-C(52)-C(53) 30(2) O(51)-C(52)-H(52A) 109.5 C(53)-C(52)-H(52A) 135.4 C(53)-C(52)-H(52A) 109.8 O(51)-C(52)-H(52B) 109.6 C(53)-C(52)-H(52B) 83.5 C(53)-C(52)-H(52B) 109.1 H(52A)-C(52)-H(52B) 108.1 O(51)-C(52)-H(52C) 110.4 C(53)-C(52)-H(52C) 110.7 C(53)-C(52)-H(52C) 81.6 H(52A)-C(52)-H(52C) 30.7 H(52B)-C(52)-H(52C) 131.0 O(51)-C(52)-H(52D) 110.5 C(53)-C(52)-H(52D) 110.3 C(53)-C(52)-H(52D) 130.2 H(52A)-C(52)-H(52D) 81.0 H(52B)-C(52)-H(52D) 29.0 H(52C)-C(52)-H(52D) 108.6 C(54)-C(53)-C(52) 104(3) C(54)-C(53)-H(53A) 111.3 C(52)-C(53)-H(53A) 111.4 C(54)-C(53)-H(53B) 110.6 C(52)-C(53)-H(53B) 110.6 H(53A)-C(53)-H(53B) 109.0 C(52)-C(53)-C(54) 102(3) C(52)-C(53)-H(53C) 111.1 C(54)-C(53)-H(53C) 111.1 C(52)-C(53)-H(53D) 111.6 C(54)-C(53)-H(53D) 111.6 H(53C)-C(53)-H(53D) 109.2 C(53)-C(54)-C(53) 30(2) C(53)-C(54)-C(55) 100(2) C(53)-C(54)-C(55) 104(2) C(53)-C(54)-H(54A) 112.1 C(53)-C(54)-H(54A) 133.0 C(55)-C(54)-H(54A) 111.7 C(53)-C(54)-H(54B) 111.4 C(53)-C(54)-H(54B) 82.8 C(55)-C(54)-H(54B) 111.8 H(54A)-C(54)-H(54B) 109.5 C(53)-C(54)-H(54C) 85.9 C(53)-C(54)-H(54C) 111.2 C(55)-C(54)-H(54C) 110.9 H(54A)-C(54)-H(54C) 27.4 H(54B)-C(54)-H(54C) 129.6 C(53)-C(54)-H(54D) 136.8 C(53)-C(54)-H(54D) 110.7 C(55)-C(54)-H(54D) 111.0 H(54A)-C(54)-H(54D) 84.0 H(54B)-C(54)-H(54D) 29.1 H(54C)-C(54)-H(54D) 109.0 O(51)-C(55)-C(54) 104.2(14) O(51)-C(55)-H(55A) 110.9 C(54)-C(55)-H(55A) 110.9 O(51)-C(55)-H(55B) 110.9 C(54)-C(55)-H(55B) 111.0 H(55A)-C(55)-H(55B) 108.9 C(65)-O(61)-C(62) 107.1(11) O(61)-C(62)-C(63) 103.8(13) O(61)-C(62)-H(62A) 111.0 C(63)-C(62)-H(62A) 111.0 O(61)-C(62)-H(62B) 111.0 C(63)-C(62)-H(62B) 111.0 H(62A)-C(62)-H(62B) 109.0 C(64)-C(63)-C(62) 102.9(13) C(64)-C(63)-H(63A) 111.2 C(62)-C(63)-H(63A) 111.2 C(64)-C(63)-H(63B) 111.2 C(62)-C(63)-H(63B) 111.2 H(63A)-C(63)-H(63B) 109.1 C(65)-C(64)-C(63) 106.6(14) C(65)-C(64)-H(64A) 110.4 C(63)-C(64)-H(64A) 110.4 C(65)-C(64)-H(64B) 110.4 C(63)-C(64)-H(64B) 110.4 H(64A)-C(64)-H(64B) 108.6 O(61)-C(65)-C(64) 108.3(14) O(61)-C(65)-H(65A) 110.0 C(64)-C(65)-H(65A) 110.0 O(61)-C(65)-H(65B) 110.0 C(64)-C(65)-H(65B) 110.0 H(65A)-C(65)-H(65B) 108.4 _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Anisotropic displacement parameters (A^2 x 10^3) for sx445. 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 _______________________________________________________________________ Sn(1) 28(1) 32(1) 36(1) -1(1) 18(1) 0(1) Sn(2) 31(1) 32(1) 40(1) 4(1) 18(1) 6(1) Sn(3) 31(1) 38(1) 39(1) 8(1) 23(1) 5(1) Sn(4) 29(1) 30(1) 34(1) 4(1) 16(1) 1(1) N(1) 32(6) 35(6) 24(5) -5(5) 16(5) -6(5) C(11) 26(7) 45(9) 23(6) -2(6) 16(6) -1(7) C(12) 27(8) 44(9) 44(9) -6(7) 15(7) -4(7) C(13) 25(8) 71(12) 33(8) -11(8) 13(7) -9(8) C(14) 27(7) 69(12) 35(8) 3(8) 19(7) -9(8) C(15) 35(8) 42(9) 23(7) 9(7) 15(6) -3(7) C(16) 27(8) 40(9) 50(9) 2(7) 21(7) 1(7) C(121) 62(11) 61(11) 49(10) 0(9) 22(9) 17(9) O(151) 63(7) 76(8) 39(6) 14(6) 22(6) 27(7) C(152) 71(12) 99(15) 37(9) 33(9) 24(9) 39(11) N(2) 25(5) 30(6) 29(5) 0(5) 11(5) 0(5) C(21) 31(8) 22(8) 54(9) 8(6) 13(7) 6(6) C(22) 36(8) 20(7) 37(7) -1(6) 18(7) 9(6) C(23) 49(9) 33(8) 55(9) -7(7) 32(8) 11(7) C(24) 52(10) 50(10) 50(9) -13(8) 40(8) -5(8) C(25) 20(7) 51(9) 35(8) -2(7) 8(6) -15(7) C(26) 38(8) 39(8) 36(8) -1(7) 23(7) -7(7) C(221) 62(11) 42(9) 70(11) -11(8) 46(9) 3(8) O(251) 64(7) 52(7) 89(9) -27(6) 49(7) -24(6) C(252) 49(11) 107(16) 78(13) -3(12) 34(10) -44(11) N(3) 29(6) 28(7) 46(7) 5(5) 18(6) -1(5) C(31) 25(7) 36(8) 41(8) 5(7) 19(7) 3(6) C(32) 43(8) 25(8) 43(8) 17(7) 21(7) 8(7) C(33) 54(10) 55(10) 47(9) 12(8) 28(8) -16(9) C(34) 33(8) 33(9) 65(10) 5(8) 19(8) -6(7) C(35) 36(8) 23(8) 63(10) -7(7) 32(8) -13(7) C(36) 30(7) 24(7) 39(8) 13(6) 19(6) 12(6) C(321) 83(12) 50(10) 45(9) 25(8) 20(9) -30(10) O(351) 56(7) 33(6) 41(6) 2(5) 8(5) -6(5) C(352) 60(11) 39(10) 76(12) 1(9) 13(10) -21(9) N(4) 26(6) 18(6) 30(6) 2(4) 16(5) 4(5) C(41) 33(8) 29(8) 49(9) -7(7) 22(7) 11(7) C(42) 38(8) 37(8) 20(6) 2(6) 16(6) 0(7) C(43) 45(9) 36(9) 56(9) 18(7) 32(8) -3(7) C(44) 30(8) 31(8) 57(9) 17(7) 20(7) 1(7) C(45) 52(10) 31(8) 73(11) -8(8) 44(9) 3(8) C(46) 35(8) 31(8) 73(10) 2(8) 34(8) -1(7) C(421) 36(8) 22(7) 67(10) -2(7) 23(8) -3(7) O(451) 72(8) 65(8) 111(10) 7(7) 73(8) 26(7) C(452) 50(30) 60(30) 140(40) -60(20) 50(30) 0(20) C(453) 100(30) 70(30) 210(50) 10(30) 140(40) 30(30) O(51) 40(6) 92(10) 75(7) -6(6) 22(5) 18(6) C(52) 70(12) 68(12) 73(8) -10(8) 18(9) 29(9) C(53) 70(20) 60(30) 57(14) 30(20) 22(14) 40(20) C(53) 80(30) 30(20) 92(16) 15(12) 20(20) 0(16) C(54) 41(9) 126(16) 67(8) -16(10) 19(7) -13(10) C(55) 55(10) 76(12) 111(13) -36(9) 54(9) -9(8) O(61) 36(6) 63(7) 106(9) 25(7) 33(6) 6(5) C(62) 49(9) 54(10) 52(9) 2(7) 30(7) 2(7) C(63) 63(11) 72(11) 105(15) 18(10) 60(11) 21(9) C(64) 59(10) 96(13) 79(12) 30(10) 52(10) 27(9) C(65) 37(8) 62(10) 79(12) 12(8) 29(9) 7(7) _______________________________________________________________________