STRUCTURE REPORT **************** diaquatetranitrato[5-(pyridinium-4-yl)-10,15,20-tri-4- pyridylporphyrin]lanthanum(III) 1,2-dichlorobenzene trisolvate **************** Structure ---------------- Formula: C58 H43 Cl6 La N12 O14 Mr = 1483.65 Cell: monoclinic P 21/c a = 17.1527(3) alpha = 90.00 b = 28.5415(6) beta = 112.9840(10) c = 13.5331(2) gamma = 90.00 V = 6099.34(19) Z = 4 Radiation: MoK\a mu = 1.040 T = 110(2) Crystal size: 0.25 x 0.20 x 0.10 Data collection ---------------- Device type: Nonius KappaCCD area-detector Absorption correction: multi-scan / (Blessing, 1995) Tmin = 0.7979 Tmax = 0.9113 Measured reflections: 36533 Independent reflections: 10767 Reflections with I>2\s(I): 6137 Rint = 0.0910 Refinement ---------------- R1 = 0.0625 wR2 = 0.1478 S = 0.942 Reflections: 10767 Parameters: 748 Restraints: 0 H treatment: mixed Delta(rho)(max) = 0.833 Delta(rho)(min) = -0.772 Geometry ---------------- TABLE [Atoms] ---------------- [NO.] [atom] [x] [y] [z] [Uiso or Ueq] [ADP type] [calc. flag] [refinement type] [occ.] [disorder assembly] [disorder group] ---------------- 1 La1 0.96484(2) 0.756793(13) 0.32933(3) 0.02382(13) Uani d . 1 . . 2 C1 0.6931(4) 0.9992(2) -0.2023(5) 0.0315(17) Uani d . 1 . . 3 C2 0.7806(4) 0.9892(2) -0.1356(5) 0.0302(16) Uani d . 1 . . 4 H2 0.8282 1.0083 -0.1266 0.036 Uiso calc R 1 . . 5 C3 0.7811(4) 0.9475(2) -0.0887(5) 0.0318(16) Uani d . 1 . . 6 H3 0.8294 0.9311 -0.0412 0.038 Uiso calc R 1 . . 7 C4 0.6927(4) 0.9325(2) -0.1251(5) 0.0263(15) Uani d . 1 . . 8 C5 0.6669(4) 0.8901(2) -0.0909(5) 0.0304(16) Uani d . 1 . . 9 C6 0.5843(4) 0.8735(2) -0.1270(5) 0.0274(15) Uani d . 1 . . 10 C7 0.5562(4) 0.8323(2) -0.0911(5) 0.0290(16) Uani d . 1 . . 11 H7 0.5913 0.8105 -0.0400 0.035 Uiso calc R 1 . . 12 C8 0.4699(4) 0.8295(2) -0.1427(5) 0.0311(16) Uani d . 1 . . 13 H8 0.4349 0.8052 -0.1349 0.037 Uiso calc R 1 . . 14 C9 0.4420(4) 0.8699(2) -0.2109(5) 0.0269(16) Uani d . 1 . . 15 C10 0.3577(4) 0.8822(2) -0.2744(5) 0.0263(15) Uani d . 1 . . 16 C11 0.3310(4) 0.9235(2) -0.3345(5) 0.0298(16) Uani d . 1 . . 17 C12 0.2440(4) 0.9352(2) -0.3940(5) 0.0332(17) Uani d . 1 . . 18 H12 0.1959 0.9171 -0.3997 0.040 Uiso calc R 1 . . 19 C13 0.2437(4) 0.9773(2) -0.4408(5) 0.0358(18) Uani d . 1 . . 20 H13 0.1954 0.9947 -0.4847 0.043 Uiso calc R 1 . . 21 C14 0.3310(4) 0.9905(2) -0.4107(5) 0.0305(16) Uani d . 1 . . 22 C15 0.3563(4) 1.0312(2) -0.4475(5) 0.0278(16) Uani d . 1 . . 23 C16 0.4414(4) 1.0450(2) -0.4221(5) 0.0283(16) Uani d . 1 . . 24 C17 0.4694(5) 1.0875(2) -0.4535(6) 0.0403(18) Uani d . 1 . . 25 H17 0.4339 1.1105 -0.5005 0.048 Uiso calc R 1 . . 26 C18 0.5541(5) 1.0898(2) -0.4057(5) 0.0368(18) Uani d . 1 . . 27 H18 0.5890 1.1141 -0.4137 0.044 Uiso calc R 1 . . 28 C19 0.5827(4) 1.0485(2) -0.3400(5) 0.0310(16) Uani d . 1 . . 29 C20 0.6649(4) 1.0385(2) -0.2702(5) 0.0249(15) Uani d . 1 . . 30 N21 0.6414(3) 0.96361(18) -0.1954(4) 0.0272(13) Uani d . 1 . . 31 H21 0.5861 0.9616 -0.2297 0.033 Uiso calc PR 0.50 . . 32 N22 0.5131(3) 0.89485(18) -0.2010(4) 0.0257(12) Uani d . 1 . . 33 H22 0.5133 0.9207 -0.2364 0.031 Uiso calc PR 0.50 . . 34 N23 0.3832(3) 0.95724(18) -0.3455(4) 0.0283(13) Uani d . 1 . . 35 H23 0.4389 0.9575 -0.3167 0.034 Uiso calc PR 0.50 . . 36 N24 0.5112(3) 1.02204(18) -0.3552(4) 0.0251(13) Uani d . 1 . . 37 H24 0.5111 0.9945 -0.3259 0.030 Uiso calc PR 0.50 . . 38 C25 0.7346(4) 0.8620(2) -0.0057(5) 0.0245(15) Uani d . 1 . . 39 C26 0.7812(4) 0.8812(2) 0.0936(5) 0.0312(16) Uani d . 1 . . 40 H26 0.7719 0.9128 0.1084 0.037 Uiso calc R 1 . . 41 C27 0.8415(4) 0.8545(2) 0.1713(5) 0.0306(16) Uani d . 1 . . 42 H27 0.8741 0.8690 0.2379 0.037 Uiso calc R 1 . . 43 N28 0.8567(3) 0.80923(18) 0.1582(4) 0.0229(12) Uani d . 1 . . 44 C29 0.8109(4) 0.7906(2) 0.0612(5) 0.0257(15) Uani d . 1 . . 45 H29 0.8207 0.7587 0.0492 0.031 Uiso calc R 1 . . 46 C30 0.7503(4) 0.8151(2) -0.0220(5) 0.0292(16) Uani d . 1 . . 47 H30 0.7200 0.8002 -0.0890 0.035 Uiso calc R 1 . . 48 C31 0.2919(4) 0.8492(2) -0.2720(5) 0.0298(16) Uani d . 1 . . 49 C32 0.2894(4) 0.8034(2) -0.3048(5) 0.0330(17) Uani d . 1 . . 50 H32 0.3301 0.7923 -0.3307 0.040 Uiso calc R 1 . . 51 C33 0.2273(4) 0.7732(2) -0.2999(5) 0.0328(17) Uani d . 1 . . 52 H33 0.2274 0.7412 -0.3189 0.039 Uiso calc R 1 . . 53 N34 0.1678(4) 0.7892(2) -0.2685(4) 0.0337(14) Uani d . 1 . . 54 H34 0.124(4) 0.769(2) -0.265(5) 0.040 Uiso d . 1 . . 55 C35 0.1678(4) 0.8342(3) -0.2368(5) 0.0390(18) Uani d . 1 . . 56 H35 0.1240 0.8449 -0.2161 0.047 Uiso calc R 1 . . 57 C36 0.2308(4) 0.8643(3) -0.2345(5) 0.0349(17) Uani d . 1 . . 58 H36 0.2329 0.8952 -0.2076 0.042 Uiso calc R 1 . . 59 C37 0.2895(4) 1.0649(2) -0.5100(5) 0.0276(15) Uani d . 1 . . 60 C38 0.2398(4) 1.0856(2) -0.4621(5) 0.0395(19) Uani d . 1 . . 61 H38 0.2482 1.0782 -0.3903 0.047 Uiso calc R 1 . . 62 C39 0.1777(5) 1.1173(3) -0.5209(6) 0.045(2) Uani d . 1 . . 63 H39 0.1426 1.1302 -0.4882 0.054 Uiso calc R 1 . . 64 N40 0.1641(3) 1.13114(19) -0.6231(4) 0.0343(14) Uani d . 1 . . 65 C41 0.2127(5) 1.1116(3) -0.6668(5) 0.0403(19) Uani d . 1 . . 66 H41 0.2044 1.1203 -0.7379 0.048 Uiso calc R 1 . . 67 C42 0.2747(5) 1.0794(2) -0.6147(6) 0.0393(18) Uani d . 1 . . 68 H42 0.3080 1.0667 -0.6502 0.047 Uiso calc R 1 . . 69 C43 0.7291(4) 1.0756(2) -0.2613(5) 0.0277(15) Uani d . 1 . . 70 C44 0.7486(4) 1.0882(2) -0.3487(5) 0.0387(19) Uani d . 1 . . 71 H44 0.7217 1.0728 -0.4157 0.046 Uiso calc R 1 . . 72 C45 0.8079(5) 1.1235(3) -0.3372(6) 0.047(2) Uani d . 1 . . 73 H45 0.8204 1.1316 -0.3976 0.057 Uiso calc R 1 . . 74 N46 0.8480(3) 1.14660(18) -0.2450(4) 0.0330(14) Uani d . 1 . . 75 C47 0.8298(4) 1.1342(2) -0.1615(5) 0.0318(17) Uani d . 1 . . 76 H47 0.8577 1.1503 -0.0956 0.038 Uiso calc R 1 . . 77 C48 0.7730(4) 1.0995(2) -0.1648(5) 0.0309(16) Uani d . 1 . . 78 H48 0.7637 1.0917 -0.1021 0.037 Uiso calc R 1 . . 79 O49 0.9432(3) 0.70262(14) 0.1751(3) 0.0306(11) Uani d . 1 . . 80 H49A 0.9211 0.6782 0.1833 0.046 Uiso d R 1 . . 81 H49B 0.9601 0.7028 0.1259 0.046 Uiso d R 1 . . 82 O50 1.0480(3) 0.78081(14) 0.2141(3) 0.0258(10) Uani d . 1 . . 83 H50A 1.0224 0.7826 0.1486 0.039 Uiso d R 1 . . 84 H50B 1.0798 0.8035 0.2241 0.039 Uiso d R 1 . . 85 N51 1.1563(4) 0.7302(2) 0.4536(4) 0.0349(15) Uani d . 1 . . 86 O52 1.1402(3) 0.77285(19) 0.4364(4) 0.0444(13) Uani d . 1 . . 87 O53 1.0945(3) 0.70162(17) 0.4164(4) 0.0397(12) Uani d . 1 . . 88 O54 1.2283(3) 0.71593(18) 0.5071(4) 0.0482(13) Uani d . 1 . . 89 N55 0.9465(3) 0.6708(2) 0.4579(4) 0.0302(13) Uani d . 1 . . 90 O56 0.9616(3) 0.71280(15) 0.4953(3) 0.0289(10) Uani d . 1 . . 91 O57 0.9306(3) 0.66620(15) 0.3602(3) 0.0325(11) Uani d . 1 . . 92 O58 0.9498(3) 0.63734(16) 0.5159(4) 0.0363(12) Uani d . 1 . . 93 N59 0.7864(4) 0.7722(2) 0.3193(5) 0.0384(15) Uani d . 1 . . 94 O60 0.8031(3) 0.73672(16) 0.2765(4) 0.0347(11) Uani d . 1 . . 95 O61 0.8476(3) 0.79993(17) 0.3710(3) 0.0384(12) Uani d . 1 . . 96 O62 0.7142(3) 0.78075(19) 0.3121(5) 0.0586(15) Uani d . 1 . . 97 N63 1.0287(4) 0.8411(2) 0.4778(5) 0.0372(15) Uani d . 1 . . 98 O64 1.0108(3) 0.84371(16) 0.3791(3) 0.0338(11) Uani d . 1 . . 99 O65 1.0160(3) 0.80242(16) 0.5148(3) 0.0356(12) Uani d . 1 . . 100 O66 1.0573(3) 0.87437(19) 0.5371(4) 0.0550(15) Uani d . 1 . . 101 Cl1 0.42251(15) 0.70342(8) -0.22617(16) 0.0626(6) Uani d . 1 . . 102 Cl2 0.35825(13) 0.71216(8) -0.03930(17) 0.0607(6) Uani d . 1 . . 103 C67 0.4937(5) 0.7063(2) -0.0949(6) 0.0441(19) Uani d . 1 . . 104 C68 0.5817(6) 0.7047(3) -0.0686(10) 0.069(3) Uani d . 1 . . 105 H68 0.6029 0.7031 -0.1237 0.082 Uiso calc R 1 . . 106 C69 0.6377(6) 0.7054(3) 0.0394(10) 0.077(3) Uani d . 1 . . 107 H69 0.6971 0.7045 0.0579 0.092 Uiso calc R 1 . . 108 C70 0.6070(7) 0.7076(3) 0.1164(9) 0.078(3) Uani d . 1 . . 109 H70 0.6462 0.7074 0.1891 0.093 Uiso calc R 1 . . 110 C71 0.5237(6) 0.7100(3) 0.0968(7) 0.066(3) Uani d . 1 . . 111 H71 0.5047 0.7117 0.1539 0.079 Uiso calc R 1 . . 112 C72 0.4654(5) 0.7098(3) -0.0120(7) 0.048(2) Uani d . 1 . . 113 Cl3 0.36970(14) 0.84834(9) 0.03135(17) 0.0676(7) Uani d . 1 . . 114 Cl4 0.35418(17) 0.95703(9) -0.00892(19) 0.0787(8) Uani d . 1 . . 115 C73 0.4599(6) 0.8831(4) 0.0853(6) 0.057(2) Uani d . 1 . . 116 C74 0.5388(7) 0.8645(4) 0.1437(7) 0.078(3) Uani d . 1 . . 117 H74 0.5447 0.8315 0.1527 0.094 Uiso calc R 1 . . 118 C75 0.6076(6) 0.8918(5) 0.1880(6) 0.088(4) Uani d . 1 . . 119 H75 0.6606 0.8781 0.2304 0.105 Uiso calc R 1 . . 120 C76 0.6010(6) 0.9427(4) 0.1711(7) 0.068(3) Uani d . 1 . . 121 H76 0.6490 0.9627 0.1996 0.081 Uiso calc R 1 . . 122 C77 0.5230(7) 0.9595(4) 0.1131(7) 0.073(3) Uani d . 1 . . 123 H77 0.5169 0.9924 0.1019 0.087 Uiso calc R 1 . . 124 C78 0.4517(5) 0.9322(4) 0.0690(6) 0.067(3) Uani d . 1 . . ---------------- TABLE [Selected Bonds] ---------------- [NO.] [bond] [distance] ---------------- 1 La1-O49(.) 2.506(4) 2 La1-O50(.) 2.583(4) 3 La1-O56(.) 2.593(4) 4 La1-O61(.) 2.601(4) 5 La1-O53(.) 2.602(5) 6 La1-O64(.) 2.611(4) 7 La1-O60(.) 2.643(4) 8 La1-O65(.) 2.654(4) 9 La1-O57(.) 2.720(4) 10 La1-N28(.) 2.773(5) 11 La1-O52(.) 2.820(5) ---------------- TABLE [Selected Angles] ---------------- [NO.] [bonds] [angle] ---------------- ----------------