Диссертация (1150264), страница 24

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Di-organoiron Mixed Valent Complexes Featuring “(η2-dppe)(η5-C5Me5)Fe”Endgroups:  Smooth Class-III to Class-II Transition Induced by SuccessiveInsertion of 1,4-Phenylene Units in a Butadiyne-Diyl Bridge. // J. Am. Chem. Soc.– 2006 – 128 (7) – с. 2463–247673.Appel, R., Geisler, K., Schöler, H.-F. Über ein neues Darstellungsverfahrenund eine ungewöhnliche Spaltung der Methylenbis(diorganylphosphane) durchAlkalimetalle.

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– 2012 – 134 – с. 6564−6567.171ПРИЛОЖЕНИЕТаблица П.1.1. Кристаллографические данные комплексов 1-3, 6, 8-12, 14, 15, 17-19, 21-25Empirical formulaFormula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensions,Volume, Å3ZDensity(calculated)Absorptioncoefficient, mm–1ReflectionscollectedIndependentreflectionsGoodness-of-fit F2Final R indices[I>2sigma(I)]R indices (all data)1Au6Cu2C144H144P8F12N63743.29210(2) K0.71073 ÅMonoclinicCc2Au6Cu2C138H126P8F12O63665.03210(2) K0.71073 ÅTriclinicP-13Au6Cu2C138H126P8F12O23601.03210(2) K0.71073 ÅMonoclinicC2/c6Au6Cu2C123H144P8F12O93551.02100(2) K0.71073 ÅTriclinicP-18C611H624Ag8Au24F48O28P325429.99100(2) K0.71073 ÅMonoclinicC2/c9C126H150Ag2Au6F12O2P83569.76100(2) K0.71073 ÅTriclinicP-110C120H138Ag2Au6Cl2O16P63490.56100(2) K0.71073 ÅTriclinicP-1a = 18.638(3) Åa = 15.9623(10) Åa = 29.4255(9) Åa = 13.4807(7) Åa = 39.2864(4) Åa = 13.5411(3) Åa = 13.1001(5) Åb = 25.012(5) Åc = 31.313(6) Åα = 90°β = 102.205(4) °γ = 90°14268(5)4b = 16.6885(11) Åc = 29.0327(19) Åα = 94.3580(10)°β = 103.8970(10)°γ = 109.8850(10)°6953.8(8)2b = 17.8352(6) Åc = 25.9788(8) Åα = 90°β = 106.6380(10)°γ = 90°13063.1(7)4b = 16.6916(9) Åc = 29.9528(16) Åα = 88.3200(10)°β = 84.0550(10)°γ = 89.8230(10)°6700.7(6)2b = 32.6616(4) Åc = 27.3632(3) Åα = 90°β = 117.1250(10)°γ = 90°31249.5(6)2b = 14.1769(3) Åc = 17.8341(4) Åα = 101.8670(10)°β = 99.8630(10)°γ = 97.3180(10)°3253.66(12)1b = 14.0229(6) Åc = 17.8852(8) Åα = 100.807(3)°β = 98.707(2)°γ = 98.553(3)°3136.6(2)11.743 g/cm31.750 g/cm31.859 g/cm31.760 g/cm31.691 g/cm31.822 g/cm31.848 g/cm36.5926.7627.1957.0166.0037.1937.471790106268686264171294121291505394228432667 [R(int) =0.0592]24485 [R(int) =0.0673]19070 [R(int) =0.0555]39054 [R(int) =0.1131]R1 = 0.0386,wR2 = 0.0895R1 = 0.0743,wR2 = 0.0982R1 = 0.0516,wR2 = 0.1334R1 = 0.1016,wR2 = 0.1485R1 = 0.0349,wR2 = 0.0840R1 = 0.0679,wR2 = 0.0912R1 = 0.0371,wR2 = 0.0986R1 = 0.0503,wR2 = 0.102829073 [R(int) =0.0418]1.051R1 = 0.0369,wR2 = 0.089912791 [R(int) =0.0237]1.056R1 = 0.0243,wR2 = 0.060111663 [R(int) =0.0596]1.029R1 = 0.0423,wR2 = 0.1039172Empirical formulaFormula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensions,Volume, Å3ZDensity(calculated)AbsorptioncoefficientReflectionscollectedIndependentreflectionsGoodness-of-fit onF2Final R indices[I>2sigma(I)]11C144H176Ag2Au6F12O11P83956.15100(2) K0.71073 ÅmonoclinicP21/c12C658H826Ag8Au24Cl20O63P2416785.63100(2) K0.71073 ÅmonoclinicP2114C102H92Au5Cl4CuF12OP82999.69100(2) K0.71073 ÅmonoclinicP21/c15aC60H70Au3Cl8CuF6O3P42015.08150(2) K0.71073 ÅTriclinicP-115бC123H146Au6Cl4Cu2F12O9P83694.84150(2) K0.71073 ÅmonoclinicC2/c17C144H184Au6Cu2F12O10P83859.55100(2) K0.71073 ÅmonoclinicP2118C146H184Ag2Au6Cl8F12O8P84223.83100(2) K0.71073 ÅmonoclinicP21a = 26.7717(11) Åa = 19.386(3) Åa = 20.7801(4) Åa = 12.5790(4) Åa = 33.6618(9) Åa = 15.6466(4) Åa = 15.6391(7) Åb = 28.0375(12) Åc = 21.8698(10) Åα = 90°β = 113.6790(10)°γ = 90°15033.7(11)4b = 29.357(5) Åc = 29.755(5) Åα = 90°β = 90.469(4)°γ = 90°16934(5)1b = 23.2258(5) Åc = 21.9267(5) Åα = 90°β = 96.7120(10)°γ = 90°10510.0(4)4b = 22.2737(7) Åc = 26.5801(8) Åα = 98.668(2)°β = 103.591(2)°γ = 93.497(2)°7119.9(4)4b = 16.3116(5) Åc = 25.0341(7) Åα = 90°β = 97.286(2)°γ = 90°13634.7(7)4b = 23.6922(7) Åc = 20.4620(4) Åα = 90°β = 93.0240(10)°γ = 90°7574.8(3)2b = 24.0712(10) Åc = 20.4371(8) Åα = 90°β = 90.928(2)°γ = 90°7692.6(6)21.748 g/cm31.646 g/cm31.896 g/cm31.880 g/cm31.800 g/cm31.692 g/cm31.824 g/cm36.2405.5967.4436.9046.9756.2146.2371417511899098145116800477499643598014129495 [R(int) =0.0357]62540 [R(int) =0.0362]18589 [R(int) =0.0549]26371 [R(int) =0.0380]18071 [R(int) =0.0703]25649 [R(int) =0.0421]28312 [R(int) =0.0345]1.0421.0191.0621.0601.1121.0631.042R1 = 0.0357,wR2 = 0.0927R1 = 0.0357,wR2 = 0.0799R1 = 0.0523,wR2 = 0.1212R1 = 0.0363,wR2 = 0.0915R1 = 0.0622,wR2 = 0.1370R1 = 0.0455,wR2 = 0.1213R1 = 0.0243,wR2 = 0.0610173C272H380Ag4Au12F24O17P167668.36150(2) K0.71073 ÅMonoclinicC2/c21a(несольватированная форма)C226H192Cl12Cu12F24O8P165175.18120(2) K0.71073 ÅMonoclinicP21/c21б(ацетонитрильный сольват)C118H102Cu6F12N4O4P82497.03100(2) K1.54184 ÅTriclinicP-1a = 47.7559(10) Åa = 21.0775(12) Åa = 12.7133 (2) Åb = 13.9314(3) Åb = 26.4675(16) Åb = 17.8070(3) Åc = 22.5632(5) Åα = 90°β = 105.8410(10)°γ = 90°14441.3(5)2c = 20.7522(13) Åα = 90°β = 96.572(4)°γ = 90°11500.9(12)21.763 g/cm319Empirical formulaFormula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensions,Volume, Å3ZDensity(calculated)AbsorptioncoefficientReflectionscollectedIndependentreflectionsGoodness-of-fit onF2Final R indices[I>2sigma(I)]R indices (all data)22a(несольватированная форма)C111H90Cl10Cu6F12P22б (ацетоновыйсольват)C118H104Cu6F12O4P22в(ацетонитрильный сольват)C114H94Cu6F12N4P823 (ацетоновыйсольват)C151H140Cu6F12O7P882443.01120(2) K0.71073 ÅMonoclinicP21/c2376.93120(2) K0.71073 ÅMonoclinicP21/c2923.62120(2) K0.71073 ÅTriclinicP-1a = 13.9694(2) Åa = 14.2002(9) Åa = 14.8094(9) Åb = 16.8813(3) Åb = 16.4108(11)Åb = 17.2631(10) Åc = 24.1678(2) Åα = 88.578(1)°β = 81.020(1)°γ = 78.540(1)°5296.31 (13)22635.39100(2) K1.54184 ÅMonoclinicP21/ca = 13.98014(10)Åb = 16.50234(15)Åc = 23.7091(2) Åα = 90°β = 97.3259(8) °γ = 90°5425.15(8)2c = 23.4512(4) Åα = 90°β = 97.0500(10)°γ = 90°5488.49(16)2c = 23.8156(15) Åα = 90 °β = 97.2910(10) °γ = 90 °5505.0(6)2c = 17.5524(10) Åα = 62.521(3)°β = 65.262(3)°γ = 65.959(3)°3485.5(4)11.494 g/cm31.566 g/cm31.613 g/cm31.478 g/cm31.434 g/cm31.393 g/cm36.4921.4103.1125.2451.3311.3231.06281117787161754517287253585981137086017394 [R(int) =0.0271]19768 [R(int) =0.0600]20061 [R(int) =0.128]10747 [R(int) =0.0539]11963 [R(int) =0.0409]14635 [R(int) =0.0238]16529 [R(int) =0.0263]1.0347871617545172872535859811370860R1 = 0.0256,wR2 = 0.0583R1 = 0.0845, wR2 =0.1979R1 = 0.1246, wR2 =0.2254R1 = 0.074, wR2 =0.1532R1 = 0.0849, wR2 =0.1644R1 = 0.0456, wR2 =0.1341R1 = 0.0540, wR2 =0.1425R1 = 0.0354, wR2 =0.1004R1 = 0.0450, wR2 =0.1066R1 = 0.0548, wR2 = R1 = 0.0447, wR2 =0.13780.1098R1 = 0.0603, wR2 = R1 = 0.0610, wR2 =0.14210.11758174Empirical formula24 (ацетоновыйсольват)C128H114Cu6F24O6P2833.19120(2) K0.71073 ÅMonoclinicP21/n25а (кристаллы израствора CH2Cl2)C106H68Cl8Cu6F12N4P82556.38120(2) K0.71073 ÅMonoclinicP21/c25б (кристаллы израствора CH3CN2)C54.6H45.2Cu3F6N3O0.4P41178.23100(2) K0.71073 ÅTriclinicP-1a = 14.9882(12) Åa = 14.1905(4) Åa = 11.9838 (5) Åb = 19.5040(15) Åc = 22.5166(17) Åα = 90°β = 104.454(2)°γ = 90°6373.9(9)2b = 15.7189(4) Åc = 23.2832(7) Åα = 90°β = 94.3330(10)°γ = 90°5178.7(3)2b = 14.5634 (7) Åc = 15.0567 (4) Åα = 98.586 (3)°β = 105.357 (3)°γ = 92.078 (4)°2497.62(19)21.476 g/cm31.639 g/cm31.567 g/cm31.1711.6121.45963647664062275315373 [R(int) =0.0315]18481 [R(int) =0.0579]11067 [R(int) =0.0473]1.0241.0241.087R1 = 0.0407, wR2 =0.0998R1 = 0.0617, wR2 =0.1130R1 = 0.0573, wR2 =0.1114R1 = 0.1262, wR2 =0.1344R1 = 0.0598, wR2 =0.1272R1 = 0.0970, wR2 =0.10698Formula weightTemperatureWavelengthCrystal systemSpace groupUnit celldimensions,Volume, Å3ZDensity(calculated)AbsorptioncoefficientReflectionscollectedIndependentreflectionsGoodness-of-fit onF2Final R indices[I>2sigma(I)]R indices (all data)175П.2 Структуры полученных комплексов в твердой фазеРисунок П.2.1.

Структуры комплексов 1 (слева) и 2 (справа) в твердой фазе,полученные методом РСА. Атомы водорода не отображены для простоты визуализации.Рисунок П.2.2. Структуры комплексов 9 (слева) и 12 (справа) в твердой фазе,полученные методом РСА. Атомы водорода не отображены для простоты визуализации.176Рисунок П.2.3.

Структура комплекса 18 в твердой фазе, полученная методом РСА.Атомы водорода не отображены для простоты визуализации.177Рисунок П.2.4. Структуры комплексов 21 (несольватированная форма), 21б(ацетонитрильный сольват), 23 (сольват с ацетоном), 24 (сольват с ацетоном), 25а (формаполученная из раствора CH2Cl2) и 22б (сольват с ацетоном) в твердой фазе, полученныеметодом РСА. Атомы водорода не отображены для простоты визуализации.178П.3 ЭСИ масс-спектры полученных комплексовРисунок П.3.1. ЭСИ+ масс-спектры (экспериментальный, слева, и расчетный,справа) комплекса 1Рисунок П.3.2.

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