#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060519.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060519 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_formula_moiety 'C15 H30 I N3 O0.50' _chemical_formula_sum 'C15 H30 I N3 O0.5' _[local]_cod_chemical_formula_sum_orig 'C15 H30 I N3 O0.50' _chemical_formula_weight 387.32 _symmetry_cell_setting Monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.939(2) _cell_length_b 7.6231(8) _cell_length_c 24.024(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.851(2) _cell_angle_gamma 90.00 _cell_volume 3780.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.361 _diffrn_ambient_temperature 150(2) loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.929631(12) 0.25655(3) 0.599436(12) 0.02973(8) Uani 1 1 d . . . I2 I 0.721804(13) 0.48389(3) 0.289240(13) 0.03332(8) Uani 1 1 d . . . N1 N 0.76395(18) 0.1853(5) 0.46825(17) 0.0370(8) Uani 1 1 d . . . H1N H 0.801(3) 0.215(7) 0.506(3) 0.068(17) Uiso 1 1 d . . . N2 N 0.80927(16) -0.0094(4) 0.38696(16) 0.0324(7) Uani 1 1 d . . . N3 N 0.89673(15) 0.1205(4) 0.39456(15) 0.0254(7) Uani 1 1 d . . . C1 C 0.83886(19) 0.1447(5) 0.39463(19) 0.0316(9) Uani 1 1 d . . . H1 H 0.8218 0.2542 0.3994 0.038 Uiso 1 1 calc R . . C2 C 0.84841(19) -0.1347(5) 0.3804(2) 0.0330(9) Uani 1 1 d . . . H2 H 0.8392 -0.2566 0.3743 0.040 Uiso 1 1 calc R . . C3 C 0.9023(2) -0.0547(5) 0.3841(2) 0.0345(10) Uani 1 1 d . . . H3 H 0.9376 -0.1091 0.3802 0.041 Uiso 1 1 calc R . . C4 C 0.94560(18) 0.2587(5) 0.40120(18) 0.0269(8) Uani 1 1 d . . . C5 C 0.9203(2) 0.4356(5) 0.4097(3) 0.0451(12) Uani 1 1 d . . . H5A H 0.8806 0.4640 0.3727 0.068 Uiso 1 1 calc R . . H5B H 0.9530 0.5259 0.4162 0.068 Uiso 1 1 calc R . . H5C H 0.9108 0.4311 0.4457 0.068 Uiso 1 1 calc R . . C6 C 0.9556(2) 0.2574(6) 0.3422(2) 0.0447(11) Uani 1 1 d . . . H6A H 0.9723 0.1426 0.3376 0.067 Uiso 1 1 calc R . . H6B H 0.9868 0.3489 0.3449 0.067 Uiso 1 1 calc R . . H6C H 0.9142 0.2798 0.3063 0.067 Uiso 1 1 calc R . . C7 C 1.0082(2) 0.2133(6) 0.4568(2) 0.0400(10) Uani 1 1 d . . . H7A H 1.0007 0.2109 0.4940 0.060 Uiso 1 1 calc R . . H7B H 1.0411 0.3019 0.4618 0.060 Uiso 1 1 calc R . . H7C H 1.0233 0.0979 0.4507 0.060 Uiso 1 1 calc R . . C8 C 0.7472(2) -0.0396(6) 0.3904(2) 0.0367(10) Uani 1 1 d . . . H8A H 0.7333 -0.1628 0.3793 0.044 Uiso 1 1 calc R . . H8B H 0.7133 0.0376 0.3605 0.044 Uiso 1 1 calc R . . C9 C 0.7543(2) -0.0027(6) 0.4546(2) 0.0423(11) Uani 1 1 d . . . H9A H 0.7149 -0.0423 0.4581 0.051 Uiso 1 1 calc R . . H9B H 0.7917 -0.0689 0.4851 0.051 Uiso 1 1 calc R . . C10 C 0.7111(2) 0.2851(6) 0.4720(2) 0.0400(10) Uani 1 1 d . . . C11 C 0.7345(3) 0.4741(6) 0.4822(3) 0.0593(14) Uani 1 1 d . . . H11A H 0.7769 0.4804 0.5181 0.089 Uiso 1 1 calc R . . H11B H 0.7034 0.5471 0.4896 0.089 Uiso 1 1 calc R . . H11C H 0.7383 0.5168 0.4454 0.089 Uiso 1 1 calc R . . C12 C 0.6496(2) 0.2729(7) 0.4109(2) 0.0508(12) Uani 1 1 d . . . H12A H 0.6589 0.3128 0.3769 0.076 Uiso 1 1 calc R . . H12B H 0.6158 0.3471 0.4132 0.076 Uiso 1 1 calc R . . H12C H 0.6346 0.1509 0.4037 0.076 Uiso 1 1 calc R . . C13 C 0.6973(3) 0.2220(8) 0.5254(3) 0.0720(18) Uani 1 1 d . . . H13A H 0.6862 0.0970 0.5201 0.108 Uiso 1 1 calc R . . H13B H 0.6609 0.2887 0.5258 0.108 Uiso 1 1 calc R . . H13C H 0.7358 0.2398 0.5646 0.108 Uiso 1 1 calc R . . N4 N 0.63210(17) 0.7808(5) 0.14610(17) 0.0376(8) Uani 1 1 d . . . H4N H 0.632(2) 0.706(6) 0.176(2) 0.046(14) Uiso 1 1 d . . . N5 N 0.74866(15) 0.9813(4) 0.21306(14) 0.0272(7) Uani 1 1 d . . . N6 N 0.82183(15) 0.8614(4) 0.19158(14) 0.0261(7) Uani 1 1 d . . . C14 C 0.77501(19) 0.8293(5) 0.20862(18) 0.0281(8) Uani 1 1 d . . . H14 H 0.7624 0.7166 0.2164 0.034 Uiso 1 1 calc R . . C15 C 0.7791(2) 1.1145(5) 0.19792(19) 0.0352(10) Uani 1 1 d . . . H15 H 0.7697 1.2362 0.1970 0.042 Uiso 1 1 calc R . . C16 C 0.8251(2) 1.0405(5) 0.18460(19) 0.0342(9) Uani 1 1 d . . . H16 H 0.8542 1.1003 0.1727 0.041 Uiso 1 1 calc R . . C17 C 0.86381(19) 0.7254(5) 0.18157(18) 0.0296(8) Uani 1 1 d . . . C18 C 0.8568(2) 0.7463(5) 0.11603(18) 0.0362(9) Uani 1 1 d . . . H18A H 0.8109 0.7377 0.0867 0.054 Uiso 1 1 calc R . . H18B H 0.8812 0.6535 0.1073 0.054 Uiso 1 1 calc R . . H18C H 0.8736 0.8611 0.1118 0.054 Uiso 1 1 calc R . . C19 C 0.9326(2) 0.7592(9) 0.2283(2) 0.0670(18) Uani 1 1 d . . . H19A H 0.9464 0.8749 0.2207 0.101 Uiso 1 1 calc R . . H19B H 0.9610 0.6689 0.2244 0.101 Uiso 1 1 calc R . . H19C H 0.9352 0.7559 0.2700 0.101 Uiso 1 1 calc R . . C20 C 0.8408(3) 0.5441(6) 0.1895(3) 0.0641(17) Uani 1 1 d . . . H20A H 0.8417 0.5351 0.2305 0.096 Uiso 1 1 calc R . . H20B H 0.8694 0.4549 0.1853 0.096 Uiso 1 1 calc R . . H20C H 0.7964 0.5255 0.1577 0.096 Uiso 1 1 calc R . . C21 C 0.6906(2) 0.9959(5) 0.22393(19) 0.0339(9) Uani 1 1 d . . . H21A H 0.6882 1.1154 0.2390 0.041 Uiso 1 1 calc R . . H21B H 0.6936 0.9113 0.2563 0.041 Uiso 1 1 calc R . . C22 C 0.6299(2) 0.9598(6) 0.1656(2) 0.0404(10) Uani 1 1 d . . . H22A H 0.5913 0.9763 0.1734 0.049 Uiso 1 1 calc R . . H22B H 0.6269 1.0424 0.1327 0.049 Uiso 1 1 calc R . . C23 C 0.5802(2) 0.7217(8) 0.0866(2) 0.0556(14) Uani 1 1 d . . . C24 C 0.5894(4) 0.8067(12) 0.0351(3) 0.107(3) Uani 1 1 d . . . H24A H 0.5811 0.9329 0.0349 0.160 Uiso 1 1 calc R . . H24B H 0.5591 0.7554 -0.0044 0.160 Uiso 1 1 calc R . . H24C H 0.6339 0.7879 0.0409 0.160 Uiso 1 1 calc R . . C25 C 0.5124(2) 0.7625(9) 0.0813(3) 0.079(2) Uani 1 1 d . . . H25A H 0.5084 0.7151 0.1174 0.119 Uiso 1 1 calc R . . H25B H 0.4796 0.7087 0.0436 0.119 Uiso 1 1 calc R . . H25C H 0.5059 0.8899 0.0795 0.119 Uiso 1 1 calc R . . C26 C 0.5888(3) 0.5228(8) 0.0851(3) 0.082(2) Uani 1 1 d . . . H26A H 0.6331 0.4967 0.0914 0.124 Uiso 1 1 calc R . . H26B H 0.5580 0.4767 0.0449 0.124 Uiso 1 1 calc R . . H26C H 0.5808 0.4678 0.1180 0.124 Uiso 1 1 calc R . . O1 O 0.5060(4) 0.7290(11) 0.3392(4) 0.160(3) Uani 1 1 d . . . C27 C 0.5714(5) 0.7623(12) 0.3515(4) 0.127(4) Uani 1 1 d . . . H27A H 0.5972 0.6536 0.3664 0.152 Uiso 1 1 calc R . . H27B H 0.5899 0.8524 0.3843 0.152 Uiso 1 1 calc R . . C28 C 0.5747(3) 0.8218(12) 0.2967(4) 0.099(2) Uani 1 1 d . . . H28A H 0.6055 0.7491 0.2879 0.119 Uiso 1 1 calc R . . H28B H 0.5894 0.9454 0.3014 0.119 Uiso 1 1 calc R . . C29 C 0.5104(4) 0.8062(9) 0.2471(3) 0.0785(19) Uani 1 1 d . . . H29A H 0.5055 0.6955 0.2240 0.094 Uiso 1 1 calc R . . H29B H 0.5004 0.9061 0.2181 0.094 Uiso 1 1 calc R . . C30 C 0.4683(4) 0.8075(12) 0.2788(5) 0.127(4) Uani 1 1 d . . . H30A H 0.4558 0.9290 0.2833 0.152 Uiso 1 1 calc R . . H30B H 0.4285 0.7384 0.2552 0.152 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02475(13) 0.02540(14) 0.03991(15) -0.00345(11) 0.01489(11) 0.00070(10) I2 0.04242(16) 0.02153(13) 0.04200(15) -0.00041(11) 0.02397(13) -0.00474(11) N1 0.030(2) 0.042(2) 0.040(2) -0.0087(17) 0.0162(17) -0.0096(16) N2 0.0318(18) 0.0218(17) 0.0442(19) -0.0061(14) 0.0172(16) -0.0021(14) N3 0.0239(17) 0.0169(15) 0.0386(18) -0.0035(13) 0.0165(15) -0.0006(12) C1 0.031(2) 0.023(2) 0.046(2) -0.0020(17) 0.021(2) 0.0016(16) C2 0.030(2) 0.0153(18) 0.049(2) -0.0074(17) 0.0125(19) 0.0014(15) C3 0.029(2) 0.021(2) 0.052(3) -0.0109(18) 0.016(2) 0.0018(16) C4 0.0253(19) 0.0174(18) 0.041(2) -0.0012(16) 0.0171(17) -0.0019(15) C5 0.038(3) 0.019(2) 0.086(4) -0.007(2) 0.033(3) -0.0044(18) C6 0.049(3) 0.046(3) 0.045(3) 0.001(2) 0.026(2) -0.011(2) C7 0.034(2) 0.035(2) 0.043(2) -0.0093(19) 0.010(2) -0.0061(19) C8 0.030(2) 0.033(2) 0.049(3) -0.0041(19) 0.018(2) -0.0095(18) C9 0.043(3) 0.041(3) 0.048(3) 0.006(2) 0.024(2) -0.006(2) C10 0.038(2) 0.048(3) 0.039(2) -0.008(2) 0.022(2) -0.006(2) C11 0.063(3) 0.049(3) 0.076(4) -0.025(3) 0.041(3) -0.010(3) C12 0.032(2) 0.060(3) 0.060(3) -0.002(3) 0.019(2) -0.001(2) C13 0.097(5) 0.086(5) 0.058(3) -0.006(3) 0.056(4) -0.006(4) N4 0.0310(19) 0.046(2) 0.0355(19) -0.0119(17) 0.0144(16) -0.0057(17) N5 0.0326(18) 0.0200(16) 0.0318(17) -0.0014(13) 0.0168(14) -0.0032(13) N6 0.0277(17) 0.0222(16) 0.0308(17) 0.0014(13) 0.0152(14) 0.0000(13) C14 0.032(2) 0.0224(19) 0.033(2) 0.0010(16) 0.0172(17) -0.0022(16) C15 0.051(3) 0.0178(19) 0.043(2) -0.0012(17) 0.026(2) -0.0058(18) C16 0.043(2) 0.026(2) 0.042(2) -0.0032(17) 0.027(2) -0.0079(18) C17 0.034(2) 0.026(2) 0.035(2) 0.0050(16) 0.0210(18) 0.0064(16) C18 0.050(3) 0.027(2) 0.033(2) -0.0011(17) 0.0196(19) 0.0045(19) C19 0.035(3) 0.117(5) 0.041(3) -0.011(3) 0.009(2) 0.020(3) C20 0.094(4) 0.027(3) 0.105(5) 0.025(3) 0.076(4) 0.018(3) C21 0.040(2) 0.028(2) 0.043(2) -0.0087(18) 0.026(2) -0.0040(18) C22 0.030(2) 0.043(3) 0.053(3) -0.005(2) 0.022(2) 0.0026(19) C23 0.036(3) 0.086(4) 0.039(3) -0.026(3) 0.012(2) -0.005(3) C24 0.088(5) 0.187(9) 0.041(3) -0.010(4) 0.024(4) -0.017(6) C25 0.032(3) 0.113(6) 0.083(4) -0.042(4) 0.016(3) -0.007(3) C26 0.052(3) 0.099(5) 0.085(4) -0.065(4) 0.019(3) -0.014(3) O1 0.163(7) 0.197(8) 0.127(6) 0.028(5) 0.069(5) -0.016(6) C27 0.094(7) 0.109(7) 0.118(7) 0.029(6) -0.008(6) -0.027(5) C28 0.064(5) 0.110(6) 0.136(7) 0.024(6) 0.054(5) 0.015(4) C29 0.098(5) 0.063(4) 0.060(4) 0.002(3) 0.021(4) -0.006(4) C30 0.069(5) 0.097(6) 0.203(11) 0.071(7) 0.048(6) 0.018(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C9 1.465(5) . ? N1 C10 1.466(6) . ? N2 C1 1.328(5) . ? N2 C2 1.367(5) . ? N2 C8 1.481(5) . ? N3 C1 1.341(5) . ? N3 C3 1.375(5) . ? N3 C4 1.495(5) . ? C2 C3 1.346(6) . ? C4 C7 1.515(6) . ? C4 C5 1.517(5) . ? C4 C6 1.533(6) . ? C8 C9 1.505(6) . ? C10 C11 1.520(6) . ? C10 C13 1.529(7) . ? C10 C12 1.532(6) . ? N4 C22 1.450(5) . ? N4 C23 1.477(6) . ? N5 C14 1.333(5) . ? N5 C15 1.369(5) . ? N5 C21 1.470(5) . ? N6 C14 1.328(5) . ? N6 C16 1.381(5) . ? N6 C17 1.504(5) . ? C15 C16 1.351(6) . ? C17 C19 1.507(6) . ? C17 C18 1.520(5) . ? C17 C20 1.521(6) . ? C21 C22 1.508(6) . ? C23 C24 1.491(9) . ? C23 C26 1.531(8) . ? C23 C25 1.536(7) . ? O1 C27 1.420(11) . ? O1 C30 1.455(10) . ? C27 C28 1.426(11) . ? C28 C29 1.441(9) . ? C29 C30 1.465(11) . ? _cod_database_code 4060519