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Chiral organometallic complexes promoted cycloaddition and insertion reactions 2

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A (1) Table A1.1 X-ray Crystallographic Data for Complex (Sc)-60 : _______________________________________________________________________ Empirical formula C20 H28 Cl2 N2 Pt2 Formula weight 757.52 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Monoclinic Space group P2(1) Unit cell dimensions a = 9.7623(6) Å α= 90° b = 9.1417(5) Å β= 100.4790(10)° c = 12.1747(7) Å γ = 90° Volume 1068.40(11) Å3 Z Density (calculated) 2.355 Mg/m3 R indices (all data) R1 = 0.0288, wR2 = 0.0597 Absolute structure parameter 0.014(10) _______________________________________________________________________ Table A1.2 Atomic coordinates (x 104) and equivalent isotropic displacement parameters (Å2x 103) for (Sc)-60 __________________________________________________________________________________ x y z U(eq) __________________________________________________________________________________ Pt(1) 2209(1) 9498(1) 6288(1) 22(1) Pt(2) 4390(1) 10620(1) 8805(1) 20(1) Cl(1) 1926(2) 10363(3) 8015(2) 34(1) Cl(2) 4655(2) 10290(2) 6957(1) 29(1) N(1) 2354(7) 8699(7) 4714(5) 24(1) N(2) 4123(7) 10855(6) 10432(5) 23(1) C(1) -1517(8) 8383(9) 4156(7) 33(2) C(2) -2473(9) 8198(10) 4840(8) 41(2) C(3) -2119(9) 8360(9) 5988(7) 37(2) C(4) -744(9) 8740(9) 6458(7) 35(2) C(5) 259(8) 8948(7) 5798(6) 23(2) C(6) -137(9) 8762(8) 4630(6) 26(2) C(7) 986(8) 9070(8) 3961(6) 27(2) C(8) 782(10) 8263(12) 2847(6) 43(2) C(9) 2603(10) 7096(8) 4791(7) 35(2) C(10) 3523(9) 9386(10) 4294(6) 34(2) C(11) 6384(8) 10770(8) 9469(6) 21(1) C(12) 7516(8) 10531(10) 8953(6) 29(2) C(13) 8865(8) 10653(12) 9515(7) 43(2) C(14) 9099(11) 11019(12) 10655(8) 53(3) C(15) 8006(10) 11236(11) 11184(7) 40(2) C(16) 6642(9) 11143(7) 10605(6) 25(2) C(17) 5412(9) 11580(9) 11098(6) 27(2) C(18) 5588(10) 11332(10) 12362(6) 34(2) C(19) 3905(10) 9373(10) 10862(6) 40(2) C(20) 2872(10) 11761(11) 10507(8) 43(2) _____________________________________________________________________________________ A (2) Table A2.1 X-ray Crystallographic Data for Complex (Rc)-62 : ___________________________________________________________________ Empirical formula C25 H27 Cl N P Pd Formula weight 514.30 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Monoclinic Space group P2(1) Unit cell dimensions a = 14.6368(16) Å α= 90° b = 9.4380(10) Å β= 108.704(2)° c = 17.7293(19) Å γ= 90° Volume 2319.8(4) Å3 Z Density (calculated) 1.473 Mg/m3 R indices (all data) R1 = 0.0665, wR2 = 0.1267 Absolute structure parameter 0.01(5) _______________________________________________________________________ Table A2.1 Atomic coordinates (x 104) and equivalent isotropic displacement parameters (Å2x 103) for (Rc)-62 ____________________________________________________________________________________ x y z U(eq) ____________________________________________________________________________________ Pd(1) 7893(1) 7114(1) 9725(1) 30(1) Cl(1) 7339(2) 4770(3) 9298(2) 48(1) P(1) 6729(2) 8054(3) 8703(1) 31(1) N(1) 9102(6) 6359(11) 10694(5) 40(2) C(1) 8348(7) 8969(12) 10245(5) 34(2) C(2) 7844(7) 10255(13) 10210(5) 43(3) C(3) 8216(8) 11365(13) 10686(6) 52(3) C(4) 9115(9) 11288(13) 11222(7) 57(3) C(5) 9643(8) 10062(17) 11285(6) 60(4) C(6) 9275(8) 8925(12) 10794(6) 37(3) C(7) 9817(7) 7555(15) 10817(6) 54(3) C(8) 10741(7) 7417(14) 11457(7) 86(4) C(9) 8801(8) 6140(14) 11404(6) 57(3) C(10) 9533(8) 5040(14) 10500(8) 66(4) C(11) 6939(7) 9712(12) 8303(5) 34(2) C(12) 6960(7) 10767(12) 7981(6) 37(2) C(13) 6948(7) 12122(13) 7580(5) 47(3) C(14) 6408(6) 6948(11) 7809(5) 32(2) C(15) 7143(7) 6477(13) 7557(6) 43(3) C(16) 6935(9) 5672(12) 6862(6) 47(3) C(17) 6000(9) 5374(12) 6434(6) 50(3) C(18) 5260(8) 5830(12) 6694(6) 49(3) C(19) 5468(7) 6623(10) 7389(5) 37(2) C(20) 5644(7) 8402(11) 8930(5) 35(2) C(21) 5062(7) 9549(12) 8660(6) 39(3) C(22) 4257(8) 9792(15) 8879(7) 52(3) C(23) 4002(8) 8893(12) 9388(6) 42(3) C(24) 4568(7) 7689(15) 9650(6) 46(3) C(25) 5384(7) 7447(15) 9437(5) 46(3) Pd(2) 1998(1) 2484(1) 5132(1) 26(1) Cl(2) 2560(2) 4821(3) 5566(1) 37(1) P(2) 3074(2) 1535(3) 6208(1) 27(1) N(2) 906(6) 3226(10) 4084(5) 35(2) C(26) 1569(7) 620(11) 4597(5) 32(2) C(27) 2079(7) -649(10) 4699(6) 35(2) C(28) 1711(8) -1832(12) 4223(6) 43(3) C(29) 847(9) -1745(12) 3637(6) 56(3) C(30) 333(9) -484(12) 3500(6) 48(3) C(31) 699(8) 707(11) 3980(6) 33(2) C(32) 153(6) 2106(12) 3874(5) 34(2) C(33) -490(6) 2153(10) 4392(5) 45(2) C(34) 457(7) 4619(11) 4159(6) 45(3) C(35) 1348(8) 3357(14) 3434(6) 54(3) C(36) 2814(7) -57(11) 6606(5) 33(2) C(37) 2719(7) -1159(11) 6914(6) 37(2) C(38) 2638(7) -2521(15) 7291(6) 55(3) C(39) 4214(6) 1178(10) 6023(5) 29(2) C(40) 4733(7) -79(12) 6292(6) 37(2) C(41) 5556(8) -326(13) 6109(6) 43(3) C(42) 5866(7) 633(13) 5653(6) 40(3) C(43) 5354(6) 1826(12) 5389(5) 36(3) C(44) 4526(6) 2103(11) 5577(5) 31(2) C(45) 3362(6) 2657(11) 7107(5) 31(2) C(46) 2618(7) 3118(13) 7352(6) 41(3) C(47) 2795(9) 3900(14) 8042(7) 54(3) C(48) 3735(9) 4200(13) 8493(7) 52(3) C(49) 4480(8) 3763(13) 8240(6) 51(3) C(50) 4291(7) 2976(12) 7543(5) 40(3) _______________________________________________________________________ A (3) Table A3.1 X-ray Crystallographic Data for Complex (Rc,Rc)-63 : _______________________________________________________________________ Empirical formula C35 H41 Cl2 N2 P Pd2 Formula weight 804.37 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Orthorhombic Space group P2(1)2(1)2(1) Unit cell dimensions a = 12.9410(7) Å α= 90° b = 13.1391(7) Å β= 90° c = 19.6736(11) Å γ = 90° Volume 3345.2(3) Å3 Z Density (calculated) 1.597 Mg/m3 R indices (all data) R1 = 0.0250, wR2 = 0.0529 Absolute structure parameter -0.023(15) _______________________________________________________________________ Table A3.2 Atomic coordinates (x 104) and equivalent isotropic displacement parameters (Å2x 103) for (Rc,Rc)-63 _________________________________________________________________________________ x y z U(eq) _________________________________________________________________________________ Pd(1) 3488(1) 3039(1) 1924(1) 26(1) Pd(2) 1093(1) 2919(1) 2411(1) 30(1) P(1) 3205(1) 2482(1) 2986(1) 26(1) Cl(1) 345(1) 2901(1) 1278(1) 61(1) Cl(2) 2148(1) 4290(1) 2090(1) 35(1) N(1) 3776(2) 3563(2) 914(1) 35(1) N(2) 40(2) 1849(2) 2830(1) 39(1) C(1) 5036(2) 2228(2) 1051(1) 41(1) C(2) 4762(2) 2223(2) 1740(1) 33(1) C(3) 5439(2) 1771(2) 2193(1) 38(1) C(4) 6365(2) 1345(2) 1973(2) 47(1) C(5) 6617(2) 1357(2) 1296(2) 58(1) C(6) 5957(2) 1799(2) 838(2) 55(1) C(7) 4285(2) 2689(2) 558(1) 45(1) C(8) 3515(3) 1896(3) 329(2) 66(1) C(9) 2857(2) 3929(3) 542(1) 50(1) C(10) 4516(3) 4420(2) 969(2) 49(1) C(11) 1964(1) 2964(2) 3249(1) 27(1) C(12) 1663(2) 3419(2) 3825(1) 30(1) C(13) 2332(2) 3644(2) 4433(1) 39(1) C(14) 557(2) 3743(2) 3884(1) 32(1) C(15) 329(2) 4740(2) 4069(1) 39(1) C(16) -671(2) 5076(3) 4147(2) 51(1) C(17) -1464(2) 4395(3) 4057(2) 59(1) C(18) -1264(2) 3399(3) 3883(2) 54(1) C(19) -260(2) 3052(2) 3787(1) 39(1) C(20) -48(2) 1956(2) 3596(1) 39(1) C(21) -782(3) 1186(3) 3927(2) 57(1) C(22) 404(3) 802(2) 2651(2) 51(1) C(23) -989(2) 2001(3) 2511(2) 56(1) C(24) 3064(2) 1125(2) 3129(1) 34(1) C(25) 2707(2) 772(2) 3759(2) 48(1) C(26) 2532(3) -250(2) 3861(2) 62(1) C(27) 2700(3) -936(2) 3348(2) 64(1) C(28) 3052(3) -603(2) 2731(2) 58(1) C(29) 3235(2) 434(2) 2618(1) 42(1) C(30) 4239(2) 2896(2) 3552(1) 30(1) C(31) 4689(2) 2298(2) 4052(2) 48(1) C(32) 5433(3) 2725(4) 4472(2) 68(1) C(33) 5746(2) 3693(3) 4395(2) 64(1) C(34) 5311(3) 4298(3) 3898(2) 60(1) C(35) 4575(2) 3894(2) 3477(1) 43(1) _________________________________________________________________________________ A (4) Table A4.1 X-ray Crystallographic Data for Complex (Rc,Rc)-64 : _______________________________________________________________________ Empirical formula C39 H43 Cl2 N2 P Pd2(1/2{CH2Cl2}) Formula weight 896.89 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Tetragonal Space group P4(3)2(1)2 Unit cell dimensions a = 13.2981(2) Å α= 90°. b = 13.2981(2) Å β= 90°. c = 43.1686(11) Å γ = 90°. Volume 7633.9(3) Å3 Z Density (calculated) 1.561 Mg/m3 R indices (all data) R1 = 0.0485, wR2 = 0.0935 Absolute structure parameter -0.01(3) _______________________________________________________________________ Table A4.2 Atomic coordinates (x 104) and equivalent isotropic displacement parameters (Å2x 103) for (Rc,Rc)-64 ____________________________________________________________________________________ x y z U(eq) ____________________________________________________________________________________ Pd(1) 1759(1) 924(1) 1458(1) 26(1) Pd(2) 1550(1) -1349(1) 1267(1) 31(1) P(1) 1057(1) 647(1) 991(1) 25(1) Cl(1) 2990(1) -349(1) 1337(1) 33(1) Cl(2) 1633(2) -1934(2) 1794(1) 93(1) N(1) 2380(3) 1183(3) 1908(1) 33(1) N(2) 417(3) -2392(3) 1138(1) 34(1) C(1) 1000(3) 2356(3) 1884(1) 30(1) C(2) 960(3) 2143(3) 1574(1) 26(1) C(3) 463(3) 2827(3) 1374(1) 31(1) C(4) 39(3) 3690(3) 1486(1) 29(1) C(5) 77(3) 3931(4) 1806(1) 30(1) C(6) -328(4) 4826(4) 1925(1) 41(1) C(7) -252(5) 5038(5) 2233(1) 55(2) C(8) 236(4) 4371(5) 2433(1) 56(2) C(9) 634(3) 3502(4) 2328(1) 40(1) C(10) 571(3) 3248(3) 2009(1) 30(1) C(11) 1510(4) 1597(3) 2092(1) 35(1) C(12) 771(4) 782(4) 2190(1) 48(1) C(13) 3170(4) 1962(4) 1882(1) 46(1) C(14) 2826(4) 298(4) 2066(1) 49(1) C(15) 1463(3) -590(3) 871(1) 28(1) C(16) 1753(3) -951(3) 597(1) 32(1) C(17) 1783(4) -403(4) 290(1) 44(1) C(18) 2100(4) -2027(3) 587(1) 31(1) C(19) 3066(4) -2240(4) 477(1) 38(1) C(20) 3433(4) -3214(4) 477(1) 43(1) C(21) 2834(5) -3990(4) 575(1) 48(1) C(22) 1865(4) -3792(4) 673(1) 44(1) C(23) 1487(4) -2811(3) 686(1) 33(1) C(24) 415(4) -2579(4) 790(1) 37(1) C(25) -352(4) -3348(5) 679(1) 53(2) A (19) Table A19.1 X-ray Crystallographic Data for Complex Pt-exo-123 : _______________________________________________________________________ Empirical formula C26 H24 As Cl2 O2 P Pt Formula weight 740.33 Temperature 295(2) K Wavelength 0.71073 Å Crystal system Monoclinic Space group P2(1) Unit cell dimensions a = 7.8529(4) Å α= 90° b = 19.6257(10) Å β= 113.9670(10)° c = 9.2303(5) Å γ = 90° Volume 1299.91(12) Å3 Z Density (calculated) 1.891 Mg/m3 R indices (all data) R1 = 0.0243, wR2 = 0.0534 Absolute structure parameter 0.005(6) _____________________________________________________________________________________ Table A19.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for Pt-exo-123 ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Pt(1) -495(1) 7501(1) 7415(1) 32(1) As(1) 1363(1) 6561(1) 7587(1) 31(1) Cl(1) -3212(2) 6855(1) 6080(2) 55(1) Cl(2) -2229(2) 8465(1) 7431(2) 56(1) P(1) 2099(2) 8095(1) 8609(1) 36(1) O(1) 3712(5) 6752(2) 10699(4) 37(1) O(2) 2111(7) 5261(2) 9081(6) 67(1) C(1) 3822(7) 6810(3) 9191(6) 35(1) C(2) 5570(8) 6434(3) 9449(8) 54(1) C(3) 6656(8) 6539(3) 10958(8) 56(2) C(4) 5565(9) 6979(3) 11605(8) 46(1) C(5) 5477(8) 7721(2) 10938(6) 43(1) C(6) 4362(9) 8171(3) 11582(7) 52(1) C(7) 2716(9) 8381(3) 10598(7) 51(1) C(8) 4242(6) 7588(3) 9150(5) 36(1) C(9) 7434(9) 8012(4) 11284(9) 73(2) C(10) 5187(13) 8367(4) 13296(8) 87(3) C(11) 2309(8) 8823(3) 7456(7) 47(1) C(12) 1302(10) 8821(3) 5821(7) 58(2) C(13) 1543(12) 9366(4) 4959(9) 71(2) C(14) 2692(11) 9894(4) 5664(10) 78(2) C(15) 3637(11) 9901(3) 7284(9) 73(2) C(16) 3462(9) 9360(3) 8179(8) 59(2) C(17) 816(7) 5760(2) 8473(6) 39(1) C(18) -665(9) 5640(3) 8793(9) 67(2) C(19) -266(16) 5010(4) 9673(11) 83(3) C(20) 1341(14) 4811(3) 9787(9) 74(2) C(21) 1742(7) 6292(3) 5733(6) 37(1) C(22) 1668(8) 6797(3) 4680(6) 46(1) C(23) 1979(8) 6631(4) 3353(7) 55(2) C(24) 2354(10) 5979(4) 3098(7) 63(2) C(25) 2417(14) 5476(4) 4137(9) 86(3) C(26) 2119(12) 5638(3) 5472(9) 73(2) ________________________________________________________________________________ A (20) Table A20.1 X-ray Crystallographic Data for Complex Pt-exo-133a : _______________________________________________________________________ Empirical formula C44 H42 As B F4 N O P Pt Formula weight 988.58 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Orthorhombic Space group P2(1)2(1)2(1) Unit cell dimensions a = 11.6961(7) Å α= 90° b = 15.7061(9) Å β= 90° c = 21.1977(12) Å γ = 90° Volume 3894.0(4) Å3 Z Density (calculated) 1.686 Mg/m3 R indices (all data) R1 = 0.0902, wR2 = 0.1430 Absolute structure parameter 0.038(12) _____________________________________________________________________________________ Table A20.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for Pt-exo-133a ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Pt(1) 7058(1) 4753(1) 5159(1) 36(1) As(1) 8265(1) 4844(1) 6037(1) 49(1) P(1) 8729(2) 4418(2) 4612(1) 28(1) N(1) 5862(8) 4662(7) 4428(4) 50(2) O(1) 9761(8) 3330(6) 5443(5) 74(3) C(1) 5613(8) 5159(8) 5617(4) 36(2) C(2) 5395(9) 5186(9) 6276(5) 47(3) C(3) 4369(10) 5469(7) 6513(5) 48(3) C(4) 3493(9) 5782(7) 6110(5) 42(3) C(5) 2447(10) 6150(7) 6312(6) 50(3) C(6) 1689(10) 6483(8) 5935(6) 49(3) C(7) 1885(9) 6460(8) 5280(6) 52(3) C(8) 2834(8) 6104(7) 5039(5) 47(3) C(9) 3698(8) 5778(7) 5441(5) 37(2) C(10) 4760(9) 5452(6) 5219(5) 38(2) C(11) 5008(10) 5395(9) 4524(5) 49(3) C(12) 5536(10) 6268(8) 4306(6) 53(3) C(13) 6272(9) 4680(10) 3766(4) 51(3) C(14) 5149(11) 3877(9) 4514(7) 63(4) C(15) 9914(10) 4148(9) 5158(8) 65(3) C(16) 11103(10) 4109(10) 4932(8) 88(6) C(17) 11681(14) 3631(12) 5318(10) 103(7) C(18) 10829(16) 3377(11) 5829(9) 94(6) C(19) 10595(12) 4112(9) 6231(7) 67(4) C(20) 9923(10) 4719(10) 5795(6) 60(3) C(21) 7825(12) 3975(8) 6641(6) 57(3) C(22) 7519(19) 3202(10) 6394(8) 116(9) C(23) 7130(20) 2557(10) 6842(9) 107(7) C(24) 6984(17) 2742(12) 7463(8) 97(6) C(25) 7307(16) 3530(12) 7695(8) 99(6) C(26) 7700(11) 4179(11) 7294(6) 75(4) C(27) 8369(10) 5905(8) 6467(4) 47(3) C(28) 9206(10) 5988(9) 6955(6) 56(3) C(29) 9395(12) 6752(10) 7231(6) 63(4) C(30) 8847(12) 7490(10) 7003(6) 64(4) C(31) 8035(14) 7387(8) 6516(6) 64(4) C(32) 7796(11) 6599(8) 6236(5) 55(3) C(33) 8839(10) 3656(8) 3977(6) 50(3) C(38) 8796(11) 3867(9) 3347(6) 58(3) C(37) 8820(12) 3247(12) 2900(7) 77(5) C(36) 8845(16) 2391(12) 3059(8) 89(5) C(35) 8919(16) 2172(11) 3664(8) 89(5) C(34) 8894(12) 2825(10) 4138(7) 68(4) C(39) 9285(9) 5438(7) 4280(5) 41(3) C(44) 8830(9) 6188(8) 4473(5) 41(3) C(43) 9200(10) 6962(8) 4260(6) 48(3) C(42) 10029(11) 6991(9) 3799(6) 55(3) C(41) 10527(11) 6267(9) 3595(7) 60(3) C(40) 10155(10) 5474(9) 3826(6) 60(4) B(1) 3008(10) 4963(9) 3007(6) 101(8) F(1A) 3360(20) 4143(11) 2859(13) 167(13) F(2A) 2660(17) 4970(20) 3623(7) 212(19) F(3A) 3985(16) 5480(12) 2964(12) 168(11) F(4A) 2212(14) 5230(17) 2616(8) 159(12) F(1) 3002(12) 5400(12) 3537(9) 103(9) F(2) 1988(11) 4531(10) 2912(7) 67(4) F(3) 3020(20) 5585(13) 2491(11) 245(18) F(4) 3897(12) 4456(12) 2917(10) 103(8) ________________________________________________________________________________ A (21) Table A21.1 X-ray Crystallographic Data for Complex Pt-exo-140a : _______________________________________________________________________ Empirical formula C44 H42 As B F4 N O P Pt Formula weight 988.58 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Orthorhombic Space group P2(1)2(1)2(1) Unit cell dimensions a = 11.7784(6) Å α= 90° b = 15.6568(8) Å β= 90° c = 21.1588(11) Å γ = 90° Volume 3901.9(3) Å3 Z Density (calculated) 1.683 Mg/m3 R indices (all data) R1 = 0.0756, wR2 = 0.1054 Absolute structure parameter 0.001(10) _____________________________________________________________________________________ Table A21.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for Pt-exo-140a ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Pt(1) 2067(1) 4774(1) 5243(1) 30(1) As(1) 3764(1) 4396(1) 4647(1) 34(1) P(1) 3218(2) 4840(2) 6093(1) 33(1) N(1) 878(5) 4697(5) 4498(3) 35(2) O(1) 4826(6) 3275(4) 5524(3) 58(2) C(1) 630(6) 5210(6) 5693(4) 28(2) C(2) 387(7) 5242(6) 6348(4) 38(2) C(3) -626(7) 5514(6) 6559(4) 36(2) C(4) -1497(7) 5803(6) 6151(4) 33(2) C(5) -2559(7) 6130(6) 6364(4) 39(2) C(6) -3313(7) 6451(6) 5954(5) 42(2) C(7) -3109(7) 6432(6) 5323(5) 43(2) C(8) -2133(8) 6102(5) 5076(4) 39(2) C(9) -1301(7) 5775(5) 5495(4) 32(2) C(10) -203(6) 5468(5) 5280(4) 30(2) C(11) 56(7) 5425(5) 4584(4) 30(2) C(12) 535(8) 6278(6) 4359(4) 44(2) C(13) 1327(8) 4678(8) 3835(4) 52(3) C(14) 205(9) 3874(6) 4580(5) 53(3) C(15) 4919(7) 4117(6) 5280(5) 45(2) C(16) 6146(9) 4139(7) 5094(6) 63(3) C(17) 6674(11) 3668(9) 5524(7) 80(4) C(18) 5803(10) 3343(7) 5961(6) 65(4) C(19) 5454(9) 4126(7) 6361(5) 53(3) C(20) 4749(7) 4650(6) 5891(4) 39(2) C(21) 3360(8) 5875(6) 6473(4) 38(2) C(22) 2822(8) 6594(5) 6243(4) 38(2) C(23) 3073(9) 7387(6) 6491(5) 47(3) C(24) 3832(9) 7475(7) 6985(5) 52(3) C(25) 4340(8) 6764(7) 7231(5) 47(3) C(26) 4138(8) 5967(6) 6980(4) 41(2) C(27) 2805(9) 4050(6) 6671(4) 43(2) C(28) 2646(8) 4218(7) 7312(4) 50(3) C(29) 2250(11) 3615(9) 7709(6) 76(4) C(30) 2023(12) 2821(8) 7499(6) 75(4) C(31) 2166(12) 2617(6) 6872(6) 77(4) C(32) 2547(10) 3247(7) 6450(6) 64(4) C(33) 4358(6) 5437(5) 4296(4) 29(2) C(34) 3899(8) 6203(6) 4473(5) 40(2) C(35) 4253(8) 6965(6) 4237(5) 43(3) C(36) 5109(8) 6974(7) 3793(5) 47(3) C(37) 5588(8) 6222(7) 3600(5) 51(3) C(38) 5216(8) 5437(7) 3841(5) 49(3) C(39) 3933(8) 3537(6) 3993(5) 41(2) C(40) 3806(9) 3752(7) 3359(5) 53(3) C(41) 3869(10) 3143(9) 2898(5) 63(3) C(42) 4054(11) 2308(9) 3072(6) 78(4) C(43) 4216(12) 2097(7) 3691(6) 75(4) C(44) 4153(9) 2704(7) 4154(5) 54(3) F(1) 7167(8) 4922(9) 2744(5) 140(5) F(2) 8770(12) 5536(8) 3047(7) 177(7) F(3) 7796(8) 4781(10) 3727(4) 133(5) F(4) 8703(9) 4183(7) 2951(6) 130(6) F(5) 7170(12) 4371(10) 3066(9) 82(3) F(6) 9016(11) 4532(11) 2973(9) 82(3) F(7) 8082(17) 5420(10) 3591(7) 82(3) F(8) 7835(15) 5484(10) 2577(6) 82(3) B(1) 8059(7) 4900(6) 3095(4) 100 ________________________________________________________________________________ A (22) Table A22.1 X-ray Crystallographic Data for Complex Pt-exo-144 : _______________________________________________________________________ Empirical formula C30 H26 As Cl2 O P Pt Formula weight 774.39 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Orthorhombic Space group P2(1)2(1)2(1) Unit cell dimensions a = 10.1554(4) Å α= 90° b = 15.8084(7) Å β= 90° c = 17.1282(8) Å γ = 90° Volume 2749.8(2) Å3 Z Density (calculated) 1.871 Mg/m3 R indices (all data) R1 = 0.0368, wR2 = 0.0659 Absolute structure parameter 0.011(6) _______________________________________________________________________ Table A22.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for Pt-exo-144 ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Pt(1) 3388(1) 7037(1) 7896(1) 21(1) As(1) 1225(1) 7375(1) 7626(1) 26(1) P(1) 3972(1) 8314(1) 7487(1) 15(1) Cl(1) 2702(2) 5721(1) 8398(1) 38(1) Cl(2) 5607(1) 6688(1) 8091(1) 33(1) O(1) 1441(4) 8319(3) 6246(2) 33(1) C(1) 1433(7) 9214(4) 6039(4) 41(2) C(2) 214(7) 9516(5) 6443(4) 44(2) C(3) 115(5) 9054(4) 7075(4) 33(1) C(4) 1257(5) 8457(4) 7056(3) 28(1) C(5) 2508(5) 8990(4) 7261(3) 27(1) C(6) 2610(6) 9543(4) 6505(4) 34(2) C(7) 195(5) 7614(4) 8539(3) 27(1) C(8) 764(7) 8114(4) 9102(3) 37(2) C(9) 20(9) 8324(5) 9762(4) 48(2) C(10) -1178(8) 8075(6) 9862(4) 59(2) C(11) -1762(9) 7545(8) 9316(4) 84(3) C(12) -1051(7) 7302(6) 8647(4) 62(3) C(13) 237(6) 6631(4) 6952(3) 29(1) C(14) 851(7) 5919(4) 6656(4) 37(2) C(15) 155(10) 5399(5) 6157(5) 61(2) C(16) -1129(9) 5571(6) 5969(5) 63(3) C(17) -1731(8) 6270(5) 6267(4) 56(2) C(18) -1052(7) 6824(5) 6760(4) 44(2) C(19) 4806(6) 8970(4) 8218(3) 23(1) C(20) 5098(7) 8652(4) 8948(3) 39(2) C(21) 5614(9) 9178(5) 9521(4) 55(2) C(22) 5838(7) 10018(5) 9356(4) 44(2) C(23) 5519(8) 10338(5) 8640(4) 47(2) C(24) 5010(6) 9826(4) 8070(3) 31(1) C(25) 4989(6) 8247(4) 6623(3) 24(1) C(26) 6228(6) 8627(4) 6580(3) 36(2) C(27) 6958(7) 8535(5) 5886(4) 44(2) C(28) 6475(7) 8075(5) 5279(3) 43(2) C(29) 5266(7) 7697(5) 5322(3) 44(2) C(30) 4547(6) 7780(4) 5998(3) 38(2) ________________________________________________________________________________ A (23) Table A23.1 X-ray Crystallographic Data for Complex Pt-exo-156 : _______________________________________________________________________ Empirical formula C26 H24 As Cl2 O P Pt Formula weight 724.33 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Orthorhombic Space group P2(1)2(1)2(1) Unit cell dimensions a = 11.1267(15) Å α= 90° b = 14.251(2) Å β= 90° c = 15.797(2) Å γ = 90° Volume 2504.8(6) Å3 Z Density (calculated) 1.921 Mg/m3 R indices (all data) R1 = 0.0288, wR2 = 0.0537 Absolute structure parameter -0.013(5) _______________________________________________________________________ Table A23.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for Pt-exo-156 ________________________________________________________________________________ x y z U(eq) _____________________________________________________________________________ Pt(1) 1889(1) 6105(1) 7808(1) 31(1) As(1) 2410(1) 4535(1) 7866(1) 35(1) Cl(1) 1371(1) 7685(1) 7623(1) 54(1) Cl(2) 3683(1) 6328(1) 7045(1) 47(1) P(1) 264(1) 5764(1) 8547(1) 31(1) O(1) 1051(3) 4493(2) 9693(2) 45(1) C(1) 333(4) 4532(3) 8932(3) 34(1) C(2) -795(5) 4012(4) 9187(3) 48(1) C(3) -457(5) 3398(4) 9754(4) 58(2) C(4) 894(5) 3492(4) 9832(4) 55(2) C(5) 1419(5) 3072(3) 9009(3) 50(1) C(6) 1061(4) 3836(3) 8360(3) 35(1) C(7) 2672(5) 4027(5) 6751(4) 73(2) C(8) 1989(8) 3590(7) 6325(5) 119(3) C(9) 3852(4) 4293(3) 8517(3) 41(1) C(10) 4787(4) 3783(4) 8197(4) 57(2) C(11) 5792(5) 3639(4) 8669(5) 65(2) C(12) 5883(5) 3989(4) 9459(5) 63(2) C(13) 4933(5) 4501(6) 9792(5) 81(2) C(14) 3930(5) 4660(5) 9306(4) 73(2) C(15) -42(4) 6453(3) 9489(3) 38(1) C(16) 620(5) 7255(4) 9639(4) 52(1) C(17) 357(6) 7798(5) 10349(4) 67(2) C(18) -516(5) 7551(5) 10899(4) 62(2) C(19) -1125(5) 6741(5) 10771(4) 58(2) C(20) -900(5) 6189(4) 10067(3) 51(1) C(21) -1089(3) 5761(3) 7902(3) 34(1) C(22) -2157(4) 6163(5) 8149(4) 61(2) C(23) -3168(5) 6104(5) 7629(4) 80(2) C(24) -3112(5) 5664(4) 6875(3) 53(1) C(25) -2046(4) 5273(4) 6606(3) 57(2) C(26) -1045(4) 5327(4) 7114(3) 50(1) A (24) Table A24.1 X-ray Crystallographic Data for Complex (±) Pt-exo-168 : _______________________________________________________________________ Empirical formula C26 H24 As Cl2 O P Pt Formula weight 724.33 Temperature 223(2) K Wavelength 0.71073 Å Crystal system Monoclinic Space group P2(1)/n Unit cell dimensions a = 10.835(2) Å α= 90° b = 14.908(3) Å β= 98.093(4)° c = 15.410(3) Å γ = 90° Volume 2464.3(8) Å3 Z Density (calculated) 1.952 Mg/m3 R indices (all data) R1 = 0.0494, wR2 = 0.0771 _______________________________________________________________________ Table A24.2 Atomic coordinates ( x 104) and equivalent isotropic displacement parameters (Å2x 103) for (±) Pt-exo-168 ________________________________________________________________________________ x y z U(eq) ________________________________________________________________________________ Pt(1) 5886(1) 6745(1) 3955(1) 25(1) As(1) 7091(1) 7680(1) 4935(1) 24(1) Cl(1) 7626(1) 6469(1) 3219(1) 36(1) Cl(2) 4591(1) 5817(1) 2988(1) 41(1) P(1) 4315(1) 6964(1) 4703(1) 29(1) O(1) 5365(4) 8934(2) 5364(2) 39(1) C(1) 5982(5) 8134(3) 5728(3) 28(1) C(2) 6474(6) 8425(4) 6655(4) 42(1) C(3) 5647(6) 9020(4) 6855(4) 53(2) C(4) 4665(6) 9088(4) 6082(4) 49(2) C(5) 3900(6) 8198(4) 6070(4) 47(2) C(6) 4844(5) 7518(4) 5777(3) 34(1) C(7) 3604(5) 5936(3) 5011(4) 39(1) C(8) 3279(7) 5762(4) 5764(4) 56(2) C(9) 3052(5) 7591(3) 4083(4) 33(1) C(10) 1816(6) 7361(4) 4090(4) 44(1) C(11) 878(6) 7850(5) 3590(5) 58(2) C(12) 1172(7) 8566(5) 3090(4) 54(2) C(13) 2385(7) 8798(4) 3080(4) 54(2) C(14) 3346(6) 8313(4) 3580(4) 46(2) C(15) 8435(5) 7054(3) 5644(3) 29(1) C(16) 8478(7) 6126(4) 5579(4) 55(2) C(17) 9436(8) 5647(4) 6071(5) 69(2) C(18) 10330(7) 6084(5) 6608(4) 58(2) C(19) 10287(6) 6997(5) 6675(5) 61(2) C(20) 9355(6) 7485(4) 6187(4) 51(2) C(21) 7750(5) 8760(3) 4500(3) 26(1) C(22) 8115(5) 9466(3) 5068(3) 34(1) C(23) 8544(5) 10258(3) 4737(4) 38(1) C(24) 8589(5) 10339(3) 3847(4) 37(1) C(25) 8216(6) 9643(3) 3287(4) 38(1) C(26) 7804(5) 8847(3) 3614(3) 33(1) [...]... 8974 (2) 23 (1) C(15) 1591(4) -24 28(4) 8991 (2) 29 (1) C(16) 1388(6) -3547(4) 9336 (2) 45(1) C(17) 24 19(6) -4101(5) 96 62( 2) 57 (2) C(18) 3605(6) -3546(4) 9668 (2) 50 (2) C(19) 3813(5) -24 24(4) 9 322 (2) 36(1) C (20 ) 4418(4) 373(4) 8 826 (2) 22 (1) C (21 ) 40 82( 5) 126 2(5) 928 6 (2) 47 (2) C (22 ) 4985(5) 20 44(5) 9580(3) 55 (2) C (23 ) 627 7(5) 1 922 (4) 9397 (2) 42( 1) C (24 ) 6619(4) 1 024 (4) 8946 (2) 37(1) C (25 ) 5698(4) 25 9(4) 8656 (2) ... C(3) 29 76(3) 334(3) 69 42( 2) 17(1) C(4) 3 125 (3) 636(4) 628 4 (2) 23 (1) C(5) 25 97(4) 17 42( 4) 6 023 (2) 28 (1) C(6) 1955(4) 25 93(4) 6415 (2) 26 (1) C(7) 1179(4) 324 1(3) 7 520 (2) 22 (1) C(8) 22 08(4) 4 020 (4) 7868 (2) 31(1) C(9) -766(4) 1966(4) 7635 (2) 28 (1) C(10) -89(4) 326 1(4) 8515 (2) 31(1) C(11) 3819(3) -13 12( 3) 7743 (2) 16(1) C( 12) 3645(3) - 827 (4) 71 52( 2) 18(1) C(13) 4554(4) -25 63(4) 7 829 (2) 28 (1) C(14) 28 20(4)... Pt(1) 9583(1) 3434(1) 1699(1) 21 (1) P(1) 74 92( 2) 4893 (2) 122 8(1) 21 (1) Cl(1) 10 120 (3) 5347 (2) 19 92( 2) 35(1) N(1) 11737(7) 1 925 (6) 20 07(4) 29 (1) C(1) 925 5(9) 1 729 (7) 1537(5) 21 (1) C (2) 8137(9) 1 526 (7) 1144(5) 26 (2) C(3) 81 72( 10) 21 6(7) 1093(6) 33 (2) C(4) 924 7(11) -947(8) 1 420 (6) 42( 2) C(5) 1 029 7(8) -818(7) 1815(5) 34 (2) C(6) 10 327 (7) 495(6) 1893(4) 26 (1) C(7) 114 42( 5) 6 42( 5) 23 96(3) 34(1) C(8) 10749(7)... C (22 ) 4764(3) 5 328 (3) 26 21(1) 35 (2) C (23 ) 3617(3) 59 72( 3) 3393(1) 38 (2) C (24 ) 3615(4) 7150(4) 3716(1) 40 (2) C (25 ) 4760(4) 7684(3) 326 7(1) 35(1) C (26 ) 5907(3) 7039(3) 24 95(1) 27 (1) C(31) 7880 (2) 620 7(3) 320 (1) 28 (2) C( 32) 6717(3) 7478 (2) 175(1) 37 (2) C(33) 6978(4) 8349(3) - 622 (2) 47 (2) C(34) 84 02( 4) 7949(4) - 127 4 (2) 47 (2) C(35) 9566(3) 6678(4) -1130 (2) 48 (2) C(36) 9305 (2) 5807(3) -333 (2) 38 (2) ... 4435 (2) 25 (1) C(14) 5541(3) 124 4(3) 3890 (2) 22 (1) C(15) 5318(4) 23 6(3) 4064 (2) 26 (1) C(16) 4308(4) -97(4) 41 42( 2) 34(1) C(17) 3511(4) 587(4) 4055(3) 41(1) C(18) 3714(4) 1589(4) 3885(3) 37(1) C(19) 4731(3) 1940(4) 3793 (2) 26 (1) C (20 ) 4950(3) 3048(4) 3603 (2) 26 (1) C (21 ) 420 9(4) 3 821 (4) 3935 (2) 39(1) C (22 ) 4000(3) 3013(5) 25 15(3) 44(1) C (23 ) 5406(4) 421 2(4) 26 64 (2) 34(1) C (24 ) 923 6(3) 20 84(3) 35 62( 2) 21 (1)... C(9) 128 58(6) 1648(6) 1035(3) 44(1) C(10) 124 80(9) 23 49(9) 25 86(6) 46 (2) C(11) 6951(9) 27 10(8) 739(5) 29 (2) C( 12) 6574(8) 4104(8) 677(5) 21 (2) C(13) 5377(3) 4985 (2) 126 (2) 24 (1) C(14) 3798(3) 5565(3) 535 (2) 34(1) C(15) 27 74(3) 6450(3) -14 (2) 41 (2) C(16) 3330(3) 6755(3) -973 (2) 38 (2) C(17) 4910(3) 6175(3) -13 82( 1) 33(1) C(18) 5933(3) 529 0 (2) -8 32( 1) 26 (1) C (21 ) 5909(3) 58 62( 2) 21 72( 1) 20 (1) C (22 ) 4764(3)... 6018(9) 47(4) C (21 ) 4 727 (11) 9940 (20 ) 629 3(10) 61(5) C (22 ) 5550(11) 1 024 0 (20 ) 6093(11) 54(5) C (23 ) 58 82( 12) 925 0 (20 ) 5657(9) 54(5) C (24 ) 5378( 12) 8050 (20 ) 5406(9) 62( 6) C (25 ) 4539(10) 7750 (20 ) 5576(8) 52( 4) C (26 ) 796(13) 5990 (20 ) -795(10) 49(5) C (27 ) 1667(11) 5900 (20 ) -23 9(9) 53(5) C (28 ) 21 60(11) 4655(19) -179(10) 50(5) C (29 ) 1773( 12) 3 520 (20 ) -668(10) 64(6) C(30) 895(15) 3 620 (20 ) - 121 4(11) 78(7) C(31)... C (2) 9780(3) 27 66(3) 1739 (2) 21 (1) C(3) 10464(3) 323 2(3) 21 87 (2) 27 (1) C(4) 11389(3) 3668(3) 1977(3) 33(1) C(5) 11650(4) 3649(4) 128 7(3) 41(1) C(6) 10995(4) 3194(4) 8 32( 3) 39(1) C(7) 9 320 (4) 22 92( 4) 557 (2) 32( 1) C(8) 85 42( 4) 3107(4) 314 (2) 46(1) C(9) 9537(4) 549(4) 966 (2) 33(1) C(10) 7870(4) 1066(4) 546 (2) 35(1) C(11) 6955(3) 20 20(3) 325 2 (2) 20 (1) C( 12) 6656(3) 1566(3) 3 826 (2) 19(1) C(13) 7 329 (3) 1 326 (3)... 5674(1) 38(1) C (23 ) 21 83(4) 6453(4) 5686(1) 28 (1) C (24 ) 24 16(4) 5371(4) 5789(1) 30(1) C (25 ) 1661(5) 4607(5) 5678(1) 44 (2) C (26 ) 1659(5) 5 527 (5) 6308(1) 49 (2) C (27 ) 3019(5) 43 62( 5) 623 2(1) 45 (2) C (28 ) 6 622 (4) 6441(3) 5719(1) 21 (1) C (29 ) 6880(4) 7463(4) 5 724 (1) 35(1) C(30) 7644(5) 7814(5) 5537 (2) 45 (2) C(31) 8150(5) 7169(6) 5347(1) 46 (2) C( 32) 7 923 (5) 6165(5) 53 42( 1) 42( 2) C(33) 7148(4) 5809(4) 5 528 (1) 34(1)... 4860(30) - 129 1(10) 79(7) C( 32) 190(11) 729 0 (20 ) -801(11) 67(5) C(33) -659( 12) 7530 (20 ) -1504( 12) 129 (10) C(34) 126 6(13) 8830 (20 ) -1363(10) 70(6) C(35) 501(13) 9850 (20 ) -483( 12) 79(6) C(36) 3054(11) 5191(19) 1709(9) 43(4) C(37) 30 32( 12) 4190 (20 ) 20 04(9) 50(4) C(38) 3036(9) 28 20 (20 ) 24 15(8) 54(4) C(39) 3601(10) 7916(19) 21 72( 7) 44(4) C(40) 28 76(14) 8460 (20 ) 24 60(10) 66(5) C(41) 3098(13) 922 0 (20 ) 3141(9) . C (22 ) 404(3) 8 02( 2) 26 51 (2) 51(1) C (23 ) -989 (2) 20 01(3) 25 11 (2) 56(1) C (24 ) 3064 (2) 1 125 (2) 3 129 (1) 34(1) C (25 ) 27 07 (2) 7 72( 2) 3759 (2) 48(1) C (26 ) 25 32( 3) -25 0 (2) 3861 (2) 62( 1) C (27 ) 27 00(3). -936 (2) 3348 (2) 64(1) C (28 ) 30 52( 3) -603 (2) 27 31 (2) 58(1) C (29 ) 323 5 (2) 434 (2) 26 18(1) 42( 1) C(30) 423 9 (2) 28 96 (2) 35 52( 1) 30(1) C(31) 4689 (2) 22 98 (2) 40 52( 2) 48(1) C( 32) 5433(3) 27 25(4) 44 72( 2). N (2) 40 (2) 1849 (2) 28 30(1) 39(1) C(1) 5036 (2) 22 28 (2) 1051(1) 41(1) C (2) 47 62( 2) 22 23 (2) 1740(1) 33(1) C(3) 5439 (2) 1771 (2) 21 93(1) 38(1) C(4) 6365 (2) 1345 (2) 1973 (2) 47(1) C(5) 6617 (2)

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