Диссертация (1150170), страница 23
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// Chem. Rev. 2013 - 113 -p. 3686-3733.150. Diaz, P., Norton, A. E., Abdolmaleki, M. K., Taylor, S. D., Kennedy,S., Calhoun, A., Krause, J. A., Connick, W. B. Study of a vapochormic Pt(II) salt.2014: American Chemical Society.155ПРИЛОЖЕНИЕП1.Кристаллографические данные комплексов 1, 4, 9, 10, 11, 13, 17, 20, 23, 24, 26, 28, 30.EmpiricalformulaFormula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensionsVolume, Å3ZDensity(calculated)AbsorptioncoefficientReflectionscollectedIndependentreflectionsGoodness-of-fiton F2Final R indices[I>2sigma(I)]R indices (alldata)1C100 H0 Au6 F12 N2O2 P82918.58100(2) K0.71073 Å4C130 H111 Au6 Cl3F12 N2 P83465.12210(2) K0.71073 ÅMonoclinicC 2/c9Au3BCuC67H52F4P3O61787.25210(2) K0.71073 ÅTrigonalR310Au3BCuC64H43F4P3N31688.17150(2) K0.71073 ÅTrigonalR311Au3BCuC64H52F4P3O31703.22170(2) K0.71073 ÅTrigonalR313C75H62Au3Cl4CuF6Fe3P42164.92100(2) K0.71073 ÅTriclinicP -117C62H66Au3Cl2CuF6P41774.37100(2) K0.71073 ÅMonoclinicP21/na =16.2957(9) Åa =30.2941(17) Åa = 17.1354(7) Åa = 16.9942(7) Åa = 17.1541(8) Åa =12.1162(2) Åa = 19.1840(10) Åb = 18.2873(10) Åb = 34.3378(19) Åb = 17.1354(7) Åb = 17.1541(8) Åb = 14.7280(2) Åb = 17.0920(9) Åc = 18.9512(10) Åc = 26.6065(15) Åc = 17.8646(8) Åc = 16.7640(8) Åc = 21.2767(3) Åc = 19.6003(10) Åα =90.00°β = 91.857(2) °γ =90.00°5644.6(5) Å32α =90.00°β = 99.7320(10)°γ =90.00°27278.7 Å38α =90.00°β = 90.00°γ =120.00°4542.7(3) Å33b = 16.9942(7) Åc = 16.6654(11)Åα =90.00°β = 90.00°γ =120.00°4168.2(4) Å33α =90.00°β = 90.00°γ =120.00°4272.1(3) Å33α =88.873(1) °β = 77.501(1) °γ =68.620(1) °3444.37(9) Å32α = 90°β = 106.770(1)°γ = 90°6153.5(6) Å341.717 Mg/m31.687 Mg/m31.9602.0181.9862.087 Mg/m31.915 Mg/m37.9426.6447.7358.4178.2157.590 mm–17.719 mm–1977010884219 55418 62018 9517993352161[R(int) = 0.0000]24020[R(int) =0.0860]5889[R(int) =0.0405]5424[R(int) =0.0355]5509[R(int) =0.0306]20103[R(int) =0.0505]12827 [R(int) =0.0478]1.0881.0091.0231.036R1 = 0.0706,wR2 = 0.1598R1 = 0.0952,wR2 = 0.1697R1 = 0.0725,wR2 = 0.2263R1 = 0.1316,wR2 = 0.2541R1 = 0.0365,wR2 = 0.0802R1 = 0.0556,wR2 = 0.0871R1 = 0.0465,wR2 = 0.1076R1 = 0.0857,wR2 = 0.1270R1 = 0.0273,wR2 = 0.0436R1 = 0.0515,wR2 = 0.0469R1 = 0.0231,wR2 = 0.0416R1 = 0.0292,wR2 = 0.0427R1 = 0.0217,wR2 = 0.0395R1 = 0.0319,wR2 = 0.0412156EmpiricalformulaFormula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensionsVolumeZDensity(calculated)AbsorptioncoefficientReflectionscollectedIndependentreflectionsGoodness-of-fiton F2Final R indices[I>2sigma(I)]R indices (alldata)202324252628C64H70Au3CuO4F6P4C59H65Au3Cl3CuF6O3P4C83H68Au3CuO4F6P4C85H70Au3ClCuO4P3C85H70Au3BrCuO4P3C122H86Au6Cu2P8F121795.52100(2) K0.71073 ÅTetragonalI–41820.78100(2)MoKTriclinicP−12021.69100(2) K0.71073 ÅMonoclinicP21/c1938.21100(2) K0.71073 ÅMonoclinicP21/n3336.55210(2) K0.71073 ÅMonoclinicC2/ca = 24.1779(9) Åa = 14.9267(9) Åa = 11.6977(5) Åa = 21.3278(5) Åb = 24.1779(9) Åb = 16.8107(11) Åb = 21.4438(9) Åb = 14.3896(4) Åc = 25.2815(9) Åc = 17.3211(11) Åc = 29.1247(12) Åc = 25.1547(7) Åα = 90°α = 117.475(1) °α = 90°α = 90°β = 90° = 110.611(1) °β = 98.5880(10)°β = 112.140(1)°γ = 90°14778.8(9) Å38γ = 93.073(1) °3485.1(4) Å32γ = 90°7223.8(5) Å34γ = 90°7150.7(3) Å341982.67210(2) K0.71073 ÅMonoclinicP21/ca = 21.4610(15)Åb = 14.7834(9) Åc = 25.4063(16)Åα = 90°β=112.3210(10)°γ = 90°7456.6(8) Å341.614 Mg/m31.735 Mg/m31.859 Mg/m31.800 Mg/m36.363 mm–16.857 mm-16.520 mm–1616662474913008 [R(int) =0.0743]30C268 H184 Au12Cu4 P12,3(F6P),2(B0.5 F2)100(2) K0.71073 ÅR -3 ca = 28.857(9) Åa = 31.4159(11) Åb = 14.019(4) Åb = 31.4159(11)Åc = 31.055(10) Åc = 137.131(8) Åα = 90°α = 90°β = 105.180(6) °β = 90 °γ = 90°12125(6) Å34γ = 120°117210 Å3121.766 Mg/m31.828 Mg/m31.176 Mg/m36.586 mm–16.816 mm–17.743 mm–19.399 mm–151443558663719631157515589775 [R(int) =0.1071]16566 [R(int) =0.0898]16406 [R(int) =0.0804]12423 [R(int) =0.0636]9209[R(int) =0.1151]8407[R(int) =0.1151]0.9201.0570.7451.0020.8620.8911.821R1 = 0.0400,wR2 = 0.1064R1 = 0.0550,wR2 = 0.1128R1 = 0.0593,wR2 = 0.1786R1 = 0.0675,wR2 = 0.1786R1 = 0.0347,wR2 = 0.0525R1 = 0.0780,wR2 = 0.0581R1 = 0.0444,wR2 = 0.0817R1 = 0.1052,wR2 = 0.1011R1 = 0.0438,wR2 = 0.1026R1 = 0.0925,wR2 = 0.1193R1 = 0.0466wR2 = 0.1204R1 = 0.1155wR2 = 0.1375R1 =wR2 = 0.1587R1 =wR2 = 0.2182157П2.
Избранные длины связей (Å) и углы (°) комплексов 1, 4, 9, 10, 11, 13, 17, 20, 23,24, 26, 28, 30.Таблица П.2.1. Избранные длинысвязей (Å) и углы (°) комплекса 1.Таблица П.2.2. Избранные длинысвязей и углы комплекса 4.Таблица П.2.3. Избранные длинысвязей (Å) и углы (°) комплекса 9.Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−N(1)Au(2)−N(1)Au(3)−N(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)2.9831(8)3.0696(9)2.965(1)2.06(1)2.07(1)2.05(1)2.241(3)2.227(4)2.239(4)N(1)−Au(1)−P(1)N(1)−Au(2)−P(2)N(1)−Au(3)−P(3)Au(1)−N(1)−Au(2)Au(1)−N(1)−Au(3)Au(2)−N(1)−Au(3)173.5(3)174.4(3)173.4(3)92.7(5)96.7(5)92.1(5)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(4)−Au(5)Au(4)−Au(6)Au(5)−Au(6)Au(1)−N(1)Au(2)−N(1)Au(3)−N(1)Au(4)−N(2)Au(5)−N(2)Au(6)−N(2)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)P(4)−Au(4)P(5)−Au(5)P(6)−Au(6)2.943(1)3.147(1)3.054(1)3.023(1)3.027(1)3.144(1)2.08(2)2.04(1)2.04(1)2.07(2)2.06(1)2.06(2)2.268(6)2.235(5)2.228(5)2.237(5)2.235(5)2.223(6)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.2388(3)3.2388(3)3.2388(3)2.9564(9)2.9564(9)2.9564(9)2.2816(13)2.2816(13)2.2816(13)2.138(5)2.138(5)2.138(5)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)178.74(18)178.74(18)178.74(18)N(1)−Au(1)−P(1)N(1)−Au(2)−P(2)N(1)−Au(3)−P(3)N(2)−Au(4)−P(4)N(2)−Au(5)−P(5)N(2)−Au(6)−P(6)Au(1)−N(1)−Au(2)Au(1)−N(1)−Au(3)Au(2)−N(1)−Au(3)Au(4)−N(2)−Au(5)Au(4)−N(2)−Au(6)Au(5)−N(2)−Au(6)171.0(4)174.2(4)173.5(4)174.2(4)174.8(4)174.8(4)91.0(6)99.7(6)96.9(6)94.2(6)94.3(6)99.4(6)Таблица П.2.4.
Избранные длинысвязей (Å) и углы (°) комплекса 10.Таблица П.2.5. Избранные длинысвязей (Å) и углы (°) комплекса 11.Таблица П.2.6. Избранные длинысвязей (Å) и углы (°) комплекса 13.Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)2.9538(7)2.9538(7)2.9538(7)3.1843(3)3.1843(3)3.1843(3)2.2851(11)2.2851(11)2.2851(11)2.123(4)2.123(4)2.123(4)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.1938(3)3.1938(3)3.1938(3)2.9278(7)2.9278(7)2.9278(7)2.2828(10)2.2828(10)2.2828(10)2.130(4)2.130(4)2.130(4)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.2300(3)3.1939(3)3.2203(3)2.8427(6)2.9948(7)2.8998(7)2.2817(12)2.2811(12)2.2751(13)2.120(5)2.128(5)2.151(5)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)178.25(14)178.25(14)178.25(14)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)177.84(13)177.84(13)177.84(13)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)178.32(14)174.34(14)171.80(14)158Таблица П.2.7.
Избранные длинысвязей (Å) и углы (°) комплекса 17.Таблица П.2.8. Избранные длинысвязей (Å) и углы (°) комплекса 20.Таблица П.2.9. Избранные длинысвязей (Å) и углы (°) комплекса 23.u(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.2657(5)3.1102(6)3.2413(6)3.2413(6)2.9697(16)2.9818(19)2.285(2)2.274(2)2.269(2)2.170(10)2.093(16)2.153(17)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.1319(6)3.1940(6)3.2309(6)3.0850(16)2.9184(15)3.0133(17)2.2832(1)2.3014(1)2.2654(1)2.215(13)2.122(12)2.104(12)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.2585(7)3.2073(7)3.1946(8)2.9906(17)2.9669(16)3.0388(17)2.275(3)2.275(3)2.282(3)2.11(2)2.13(2)2.21(2)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)178.2(3)175.9(4)178.7(4)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)178.30179.17178.82C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)179.1(5)178.8(5)179.1(5)Таблица П.2.10.
Избранные длинысвязей (Å) и углы (°) комплекса 24.Таблица П.2.11. Избранные длинысвязей (Å) и углы (°) комплекса 25.Таблица П.2.12. Избранные длинысвязей (Å) и углы (°) комплекса 26.Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)Au(1)−Cu(1)Au(2)−Cu(1)Au(3)−Cu(1)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)C(6)−Cu(1)3.2291(3)3.1973(3)3.1700(3)3.0606(6)2.9196(9)2.8931(8)2.284(2)2.281(2)2.284(2)2.200(5)2.145(6)2.114(6)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)Cl(1)−Cu(1)3.0266(4)3.2250(4)3.1717(4)2.276(2)2.284(2)2.276(2)2.101(8)2.162(8)2.314(2)Au(1)−Au(2)Au(1)−Au(3)Au(2)−Au(3)P(1)−Au(1)P(2)−Au(2)P(3)−Au(3)C(2)−Cu(1)C(4)−Cu(1)Br(1)−Cu(1)3.0396(7)3.2603(7)3.1950(7)2.280(3)2.285(3)2.282(3)2.151(10)2.187(10)2.424(2)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)175.0(2)176.0(2)170.9(2)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)175.9(3)175.8(3)172.5(3)C(2)−Au(1)−P(1)C(4)−Au(2)−P(2)C(6)−Au(3)−P(3)176.7(2)178.1(2)175.1(2)Таблица П.2.13.