# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2179 data_struc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H69 I3 N17 U' _chemical_formula_weight 1755.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.598(4) _cell_length_b 22.296(5) _cell_length_c 27.992(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13480(5) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6824 _exptl_absorpt_coefficient_mu 3.838 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85248 _diffrn_reflns_av_R_equivalents 0.1116 _diffrn_reflns_av_sigmaI/netI 0.1262 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.16 _reflns_number_total 16728 _reflns_number_gt 9116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16728 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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 U U 0.640914(11) 0.283181(12) 0.315842(8) 0.01494(7) Uani 1 1 d . . . I1 I 0.62958(3) 0.55305(3) 0.37854(2) 0.05008(18) Uani 1 1 d . . . I2 I 0.38526(2) 0.35681(2) 0.264196(18) 0.02864(13) Uani 1 1 d . . . I3 I 0.72512(2) 0.13278(2) 0.126474(16) 0.02994(13) Uani 1 1 d . . . N1 N 0.7317(2) 0.2178(3) 0.27073(18) 0.0179(12) Uani 1 1 d . . . N2 N 0.5589(2) 0.3509(3) 0.36859(18) 0.0172(12) Uani 1 1 d . . . N11 N 0.6382(2) 0.2806(2) 0.22505(18) 0.0179(12) Uani 1 1 d . . . N12 N 0.6939(3) 0.3049(3) 0.16087(19) 0.0200(13) Uani 1 1 d . . . N21 N 0.7529(3) 0.3156(3) 0.32956(18) 0.0193(13) Uani 1 1 d . . . N22 N 0.8433(2) 0.2818(3) 0.35868(18) 0.0211(13) Uani 1 1 d . . . N31 N 0.6384(3) 0.1686(3) 0.32760(18) 0.0208(13) Uani 1 1 d . . . N32 N 0.6496(3) 0.0765(3) 0.2992(2) 0.0236(14) Uani 1 1 d . . . N41 N 0.6521(2) 0.2824(3) 0.40672(19) 0.0200(13) Uani 1 1 d . . . N42 N 0.6786(3) 0.3465(3) 0.46428(19) 0.0231(14) Uani 1 1 d . . . N51 N 0.6322(2) 0.3932(3) 0.29543(18) 0.0171(12) Uani 1 1 d . . . N52 N 0.5630(2) 0.4585(2) 0.2668(2) 0.0205(13) Uani 1 1 d . . . N61 N 0.5256(2) 0.2567(3) 0.31072(18) 0.0182(12) Uani 1 1 d . . . N62 N 0.4402(3) 0.2327(3) 0.3517(2) 0.0224(14) Uani 1 1 d . . . C11 C 0.7494(3) 0.2505(3) 0.2267(2) 0.0190(15) Uani 1 1 d . . . H11A H 0.7691 0.2232 0.2044 0.023 Uiso 1 1 calc R . . H11B H 0.7788 0.2820 0.2345 0.023 Uiso 1 1 calc R . . C12 C 0.6926(3) 0.2776(3) 0.2041(2) 0.0189(15) Uani 1 1 d . . . C13 C 0.6015(3) 0.3128(3) 0.1932(2) 0.0189(15) Uani 1 1 d . . . C14 C 0.5385(3) 0.3303(3) 0.1966(2) 0.0239(17) Uani 1 1 d . . . H14 H 0.5146 0.3201 0.2230 0.029 Uiso 1 1 calc R . . C15 C 0.5143(3) 0.3629(3) 0.1594(3) 0.0265(17) Uani 1 1 d . . . H15 H 0.4733 0.3753 0.1609 0.032 Uiso 1 1 calc R . . C16 C 0.5493(4) 0.3778(3) 0.1200(3) 0.0322(19) Uani 1 1 d . . . H16 H 0.5309 0.3996 0.0955 0.039 Uiso 1 1 calc R . . C17 C 0.6109(4) 0.3613(3) 0.1156(3) 0.0287(18) Uani 1 1 d . . . H17 H 0.6345 0.3717 0.0891 0.034 Uiso 1 1 calc R . . C18 C 0.6348(3) 0.3285(3) 0.1528(2) 0.0222(16) Uani 1 1 d . . . C19 C 0.7470(4) 0.3100(4) 0.1293(3) 0.0329(19) Uani 1 1 d . . . H19A H 0.7818 0.2898 0.1433 0.049 Uiso 1 1 calc R . . H19B H 0.7569 0.3516 0.1246 0.049 Uiso 1 1 calc R . . H19C H 0.7373 0.2919 0.0990 0.049 Uiso 1 1 calc R . . C21 C 0.7866(3) 0.2136(3) 0.3033(2) 0.0218(16) Uani 1 1 d . . . H21A H 0.7808 0.1809 0.3256 0.026 Uiso 1 1 calc R . . H21B H 0.8235 0.2056 0.2847 0.026 Uiso 1 1 calc R . . C22 C 0.7941(3) 0.2708(3) 0.3298(2) 0.0201(16) Uani 1 1 d . . . C23 C 0.7787(3) 0.3593(3) 0.3599(2) 0.0193(15) Uani 1 1 d . . . C24 C 0.7572(3) 0.4162(3) 0.3721(2) 0.0252(17) Uani 1 1 d . . . H24 H 0.7205 0.4308 0.3592 0.030 Uiso 1 1 calc R . . C25 C 0.7910(4) 0.4500(4) 0.4031(3) 0.0321(19) Uani 1 1 d . . . H25 H 0.7774 0.4882 0.4113 0.039 Uiso 1 1 calc R . . C26 C 0.8468(4) 0.4275(4) 0.4230(3) 0.036(2) Uani 1 1 d . . . H26 H 0.8686 0.4508 0.4448 0.043 Uiso 1 1 calc R . . C27 C 0.8695(3) 0.3713(4) 0.4107(3) 0.0300(19) Uani 1 1 d . . . H27 H 0.9064 0.3567 0.4232 0.036 Uiso 1 1 calc R . . C28 C 0.8343(3) 0.3379(3) 0.3784(2) 0.0215(16) Uani 1 1 d . . . C29 C 0.8970(3) 0.2415(4) 0.3656(3) 0.034(2) Uani 1 1 d . . . H29A H 0.8909 0.2054 0.3476 0.051 Uiso 1 1 calc R . . H29B H 0.9009 0.2318 0.3989 0.051 Uiso 1 1 calc R . . H29C H 0.9339 0.2612 0.3549 0.051 Uiso 1 1 calc R . . C31 C 0.7097(3) 0.1571(3) 0.2588(2) 0.0215(16) Uani 1 1 d . . . H31A H 0.7449 0.1303 0.2557 0.026 Uiso 1 1 calc R . . H31B H 0.6881 0.1580 0.2284 0.026 Uiso 1 1 calc R . . C32 C 0.6675(3) 0.1343(3) 0.2965(2) 0.0185(15) Uani 1 1 d . . . C33 C 0.5986(3) 0.1303(3) 0.3524(2) 0.0186(15) Uani 1 1 d . . . C34 C 0.5566(3) 0.1422(4) 0.3890(3) 0.0273(17) Uani 1 1 d . . . H34 H 0.5530 0.1804 0.4021 0.033 Uiso 1 1 calc R . . C35 C 0.5207(3) 0.0956(4) 0.4050(3) 0.0302(19) Uani 1 1 d . . . H35 H 0.4917 0.1027 0.4290 0.036 Uiso 1 1 calc R . . C36 C 0.5263(4) 0.0386(4) 0.3867(3) 0.037(2) Uani 1 1 d . . . H36 H 0.5008 0.0082 0.3982 0.044 Uiso 1 1 calc R . . C37 C 0.5693(4) 0.0255(4) 0.3513(3) 0.0333(19) Uani 1 1 d . . . H37 H 0.5741 -0.0131 0.3393 0.040 Uiso 1 1 calc R . . C38 C 0.6045(3) 0.0727(3) 0.3350(2) 0.0241(17) Uani 1 1 d . . . C39 C 0.6747(4) 0.0272(3) 0.2712(3) 0.040(2) Uani 1 1 d . . . H39A H 0.7050 0.0424 0.2492 0.060 Uiso 1 1 calc R . . H39B H 0.6419 0.0080 0.2538 0.060 Uiso 1 1 calc R . . H39C H 0.6939 -0.0014 0.2921 0.060 Uiso 1 1 calc R . . C41 C 0.5940(3) 0.3789(3) 0.4082(2) 0.0197(16) Uani 1 1 d . . . H41A H 0.5658 0.3902 0.4336 0.024 Uiso 1 1 calc R . . H41B H 0.6146 0.4148 0.3968 0.024 Uiso 1 1 calc R . . C42 C 0.6411(3) 0.3350(3) 0.4268(2) 0.0201(15) Uani 1 1 d . . . C43 C 0.7003(3) 0.2575(3) 0.4335(2) 0.0201(15) Uani 1 1 d . . . C44 C 0.7310(3) 0.2029(3) 0.4288(2) 0.0258(17) Uani 1 1 d . . . H44 H 0.7203 0.1759 0.4049 0.031 Uiso 1 1 calc R . . C45 C 0.7773(3) 0.1901(4) 0.4602(3) 0.035(2) Uani 1 1 d . . . H45 H 0.7986 0.1540 0.4578 0.042 Uiso 1 1 calc R . . C46 C 0.7931(4) 0.2307(4) 0.4961(3) 0.038(2) Uani 1 1 d . . . H46 H 0.8251 0.2208 0.5168 0.045 Uiso 1 1 calc R . . C47 C 0.7637(3) 0.2847(4) 0.5024(2) 0.0326(19) Uani 1 1 d . . . H47 H 0.7742 0.3110 0.5269 0.039 Uiso 1 1 calc R . . C48 C 0.7169(3) 0.2974(4) 0.4695(2) 0.0259(18) Uani 1 1 d . . . C49 C 0.6809(4) 0.4020(4) 0.4925(3) 0.037(2) Uani 1 1 d . . . H49A H 0.6493 0.4290 0.4817 0.055 Uiso 1 1 calc R . . H49B H 0.7208 0.4205 0.4887 0.055 Uiso 1 1 calc R . . H49C H 0.6744 0.3928 0.5256 0.055 Uiso 1 1 calc R . . C51 C 0.5317(3) 0.3987(3) 0.3377(2) 0.0198(15) Uani 1 1 d . . . H51A H 0.4942 0.3837 0.3228 0.024 Uiso 1 1 calc R . . H51B H 0.5207 0.4330 0.3572 0.024 Uiso 1 1 calc R . . C52 C 0.5760(3) 0.4173(3) 0.3005(2) 0.0175(15) Uani 1 1 d . . . C53 C 0.6582(3) 0.4236(3) 0.2567(2) 0.0209(16) Uani 1 1 d . . . C54 C 0.7175(3) 0.4176(3) 0.2363(2) 0.0232(16) Uani 1 1 d . . . H54 H 0.7471 0.3916 0.2486 0.028 Uiso 1 1 calc R . . C55 C 0.7290(4) 0.4532(4) 0.1966(3) 0.0315(19) Uani 1 1 d . . . H55 H 0.7678 0.4513 0.1822 0.038 Uiso 1 1 calc R . . C56 C 0.6849(4) 0.4913(3) 0.1777(2) 0.0300(18) Uani 1 1 d . . . H56 H 0.6949 0.5135 0.1507 0.036 Uiso 1 1 calc R . . C57 C 0.6261(4) 0.4977(3) 0.1974(2) 0.0269(18) Uani 1 1 d . . . H57 H 0.5966 0.5234 0.1844 0.032 Uiso 1 1 calc R . . C58 C 0.6142(3) 0.4634(3) 0.2377(2) 0.0216(16) Uani 1 1 d . . . C59 C 0.5051(3) 0.4927(3) 0.2631(3) 0.0327(19) Uani 1 1 d . . . H59A H 0.4773 0.4803 0.2879 0.049 Uiso 1 1 calc R . . H59B H 0.4865 0.4853 0.2325 0.049 Uiso 1 1 calc R . . H59C H 0.5138 0.5347 0.2664 0.049 Uiso 1 1 calc R . . C61 C 0.5101(3) 0.3114(3) 0.3870(2) 0.0202(16) Uani 1 1 d . . . H61A H 0.4745 0.3351 0.3965 0.024 Uiso 1 1 calc R . . H61B H 0.5250 0.2899 0.4148 0.024 Uiso 1 1 calc R . . C62 C 0.4918(3) 0.2678(3) 0.3491(2) 0.0209(16) Uani 1 1 d . . . C63 C 0.4929(3) 0.2128(3) 0.2858(2) 0.0197(15) Uani 1 1 d . . . C64 C 0.5059(3) 0.1865(3) 0.2419(2) 0.0225(16) Uani 1 1 d . . . H64 H 0.5414 0.1962 0.2247 0.027 Uiso 1 1 calc R . . C65 C 0.4637(3) 0.1455(3) 0.2252(2) 0.0241(17) Uani 1 1 d . . . H65 H 0.4706 0.1275 0.1957 0.029 Uiso 1 1 calc R . . C66 C 0.4109(4) 0.1299(3) 0.2510(3) 0.0302(19) Uani 1 1 d . . . H66 H 0.3837 0.1019 0.2381 0.036 Uiso 1 1 calc R . . C67 C 0.3976(3) 0.1547(3) 0.2951(3) 0.0246(17) Uani 1 1 d . . . H67 H 0.3630 0.1436 0.3128 0.029 Uiso 1 1 calc R . . C68 C 0.4398(3) 0.1975(3) 0.3109(2) 0.0205(15) Uani 1 1 d . . . C69 C 0.3957(3) 0.2316(4) 0.3918(3) 0.0307(19) Uani 1 1 d . . . H69A H 0.4074 0.2609 0.4152 0.046 Uiso 1 1 calc R . . H69B H 0.3957 0.1925 0.4062 0.046 Uiso 1 1 calc R . . H69C H 0.3549 0.2405 0.3801 0.046 Uiso 1 1 calc R . . N71 N 0.8539(5) 0.4747(4) 0.5546(3) 0.076(3) Uani 1 1 d . . . C71 C 0.7979(4) 0.5037(4) 0.5446(3) 0.042(2) Uani 1 1 d . . . H71 H 0.7611 0.4911 0.5586 0.051 Uiso 1 1 calc R . . C72 C 0.7987(5) 0.5512(4) 0.5134(3) 0.048(2) Uani 1 1 d . . . H72 H 0.7623 0.5706 0.5046 0.058 Uiso 1 1 calc R . . C73 C 0.8556(5) 0.5692(4) 0.4953(3) 0.046(2) Uani 1 1 d . . . H73 H 0.8585 0.6018 0.4747 0.055 Uiso 1 1 calc R . . C74 C 0.9069(4) 0.5383(5) 0.5085(3) 0.050(3) Uani 1 1 d . . . H74 H 0.9447 0.5507 0.4961 0.060 Uiso 1 1 calc R . . C75 C 0.9070(4) 0.4928(4) 0.5371(2) 0.031(2) Uani 1 1 d . . . H75 H 0.9438 0.4734 0.5450 0.037 Uiso 1 1 calc R . . N81 N 0.3699(4) 0.3951(5) 0.4367(4) 0.077(3) Uani 1 1 d . . . C81 C 0.3917(5) 0.4200(7) 0.4746(4) 0.073(4) Uani 1 1 d . . . H81 H 0.3879 0.3994 0.5033 0.088 Uiso 1 1 calc R . . C82 C 0.4198(7) 0.4746(7) 0.4753(5) 0.092(4) Uani 1 1 d . . . H82 H 0.4362 0.4904 0.5033 0.111 Uiso 1 1 calc R . . C83 C 0.4229(8) 0.5056(6) 0.4323(6) 0.120(6) Uani 1 1 d . . . H83 H 0.4428 0.5426 0.4306 0.144 Uiso 1 1 calc R . . C84 C 0.3958(6) 0.4806(6) 0.3919(4) 0.080(4) Uani 1 1 d . . . H84 H 0.3938 0.5005 0.3628 0.096 Uiso 1 1 calc R . . C85 C 0.3729(4) 0.4259(6) 0.3982(4) 0.059(3) Uani 1 1 d . . . H85 H 0.3569 0.4075 0.3711 0.071 Uiso 1 1 calc R . . N91 N 0.9819(5) 0.2109(6) 0.4850(4) 0.100(4) Uani 1 1 d . . . C91 C 1.0022(5) 0.1747(5) 0.4454(4) 0.056(3) Uani 1 1 d . . . H91 H 0.9765 0.1455 0.4323 0.067 Uiso 1 1 calc R . . C92 C 1.0611(5) 0.1846(5) 0.4271(4) 0.057(3) Uani 1 1 d . . . H92 H 1.0764 0.1622 0.4017 0.068 Uiso 1 1 calc R . . C93 C 1.0947(5) 0.2276(5) 0.4476(4) 0.060(3) Uani 1 1 d . . . H93 H 1.1342 0.2358 0.4361 0.072 Uiso 1 1 calc R . . C94 C 1.0722(5) 0.2596(5) 0.4849(3) 0.056(3) Uani 1 1 d . . . H94 H 1.0977 0.2885 0.4985 0.067 Uiso 1 1 calc R . . C95 C 1.0178(4) 0.2527(5) 0.5028(3) 0.045(2) Uani 1 1 d . . . H95 H 1.0043 0.2768 0.5278 0.054 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 U 0.01250(11) 0.01654(13) 0.01579(11) -0.00129(11) 0.00103(10) -0.00075(11) I1 0.0765(5) 0.0280(3) 0.0457(3) -0.0023(3) -0.0184(3) 0.0104(3) I2 0.0139(2) 0.0305(3) 0.0415(3) 0.0025(2) -0.0043(2) -0.0028(2) I3 0.0385(3) 0.0294(3) 0.0219(2) -0.0031(2) -0.0056(2) 0.0035(2) N1 0.017(3) 0.018(3) 0.018(3) -0.003(3) 0.002(2) -0.002(3) N2 0.014(3) 0.021(3) 0.017(3) -0.001(2) 0.001(2) -0.003(2) N11 0.017(3) 0.018(3) 0.019(3) -0.001(2) 0.002(2) -0.005(3) N12 0.017(3) 0.025(4) 0.018(3) -0.002(3) 0.007(2) 0.001(3) N21 0.015(3) 0.024(4) 0.018(3) -0.003(2) 0.004(2) -0.002(3) N22 0.012(3) 0.033(4) 0.018(3) -0.001(3) -0.004(2) 0.001(3) N31 0.020(3) 0.026(4) 0.017(3) 0.003(2) 0.001(2) -0.002(3) N32 0.027(4) 0.018(3) 0.025(3) -0.002(3) 0.002(3) -0.002(3) N41 0.018(3) 0.021(3) 0.021(3) -0.001(3) 0.001(2) -0.002(3) N42 0.022(3) 0.029(4) 0.018(3) 0.000(3) -0.005(2) -0.002(3) N51 0.015(3) 0.019(3) 0.017(3) -0.002(2) -0.002(2) -0.001(2) N52 0.015(3) 0.014(3) 0.032(3) 0.004(3) -0.004(2) -0.001(2) N61 0.013(3) 0.020(3) 0.022(3) -0.003(3) 0.000(2) 0.000(2) N62 0.014(3) 0.028(4) 0.026(3) 0.002(3) 0.001(2) -0.003(3) C11 0.016(3) 0.022(4) 0.019(3) -0.002(3) 0.005(3) -0.004(3) C12 0.017(3) 0.022(4) 0.017(3) -0.002(3) 0.003(3) -0.002(3) C13 0.020(4) 0.020(4) 0.017(4) 0.003(3) 0.000(3) -0.002(3) C14 0.018(4) 0.026(4) 0.027(4) -0.001(3) -0.001(3) -0.005(3) C15 0.023(4) 0.023(4) 0.034(4) 0.000(4) -0.009(3) 0.001(3) C16 0.033(5) 0.030(5) 0.033(4) 0.010(4) -0.009(4) 0.000(4) C17 0.039(5) 0.024(4) 0.023(4) 0.001(3) -0.001(3) -0.003(4) C18 0.026(4) 0.018(4) 0.023(4) -0.007(3) 0.001(3) -0.003(3) C19 0.033(5) 0.036(5) 0.030(4) 0.011(4) 0.012(4) 0.006(4) C21 0.015(3) 0.029(4) 0.022(3) 0.002(3) -0.001(3) 0.001(3) C22 0.018(4) 0.028(5) 0.014(3) 0.003(3) -0.001(3) -0.004(3) C23 0.017(4) 0.023(4) 0.017(3) -0.004(3) 0.002(3) -0.005(3) C24 0.025(4) 0.024(4) 0.027(4) -0.006(3) 0.003(3) 0.002(3) C25 0.034(5) 0.031(5) 0.031(4) -0.009(4) 0.007(3) -0.008(4) C26 0.032(5) 0.038(5) 0.038(5) -0.016(4) -0.005(4) -0.009(4) C27 0.023(4) 0.039(5) 0.028(4) 0.001(4) -0.005(3) -0.010(4) C28 0.014(3) 0.030(5) 0.020(4) 0.007(3) -0.001(3) -0.004(3) C29 0.017(4) 0.041(5) 0.044(5) -0.004(4) -0.013(3) 0.007(4) C31 0.023(4) 0.018(4) 0.024(4) -0.002(3) -0.002(3) 0.001(3) C32 0.021(4) 0.020(4) 0.014(3) 0.001(3) -0.004(3) 0.002(3) C33 0.016(4) 0.018(4) 0.021(3) 0.004(3) -0.003(3) -0.006(3) C34 0.022(4) 0.027(5) 0.033(4) 0.010(4) 0.002(3) 0.005(3) C35 0.017(4) 0.042(6) 0.032(4) 0.011(4) -0.003(3) -0.001(4) C36 0.031(5) 0.037(6) 0.043(5) 0.013(4) -0.005(4) -0.011(4) C37 0.045(5) 0.019(5) 0.035(4) 0.003(4) -0.001(4) -0.014(4) C38 0.027(4) 0.022(4) 0.023(4) 0.003(3) -0.003(3) -0.001(3) C39 0.060(6) 0.016(4) 0.044(5) -0.009(4) 0.009(4) -0.003(4) C41 0.021(4) 0.022(4) 0.016(3) -0.003(3) -0.001(3) 0.001(3) C42 0.017(3) 0.025(4) 0.018(3) -0.002(3) 0.001(3) -0.005(3) C43 0.016(3) 0.023(4) 0.021(4) 0.006(3) 0.002(3) 0.004(3) C44 0.023(4) 0.034(5) 0.020(4) 0.002(3) 0.000(3) 0.001(3) C45 0.025(4) 0.049(6) 0.030(4) 0.010(4) 0.004(3) 0.017(4) C46 0.029(5) 0.060(7) 0.024(4) 0.006(4) -0.006(3) 0.008(4) C47 0.030(4) 0.044(5) 0.023(4) 0.001(4) -0.009(3) -0.002(4) C48 0.021(4) 0.041(5) 0.016(3) 0.005(3) -0.002(3) 0.000(4) C49 0.048(5) 0.036(5) 0.026(4) -0.014(4) -0.006(4) -0.002(4) C51 0.011(3) 0.018(4) 0.030(4) 0.000(3) 0.000(3) -0.003(3) C52 0.017(4) 0.015(4) 0.020(3) 0.000(3) -0.003(3) -0.002(3) C53 0.025(4) 0.021(4) 0.017(3) -0.003(3) 0.002(3) -0.004(3) C54 0.024(4) 0.019(4) 0.026(4) -0.001(3) 0.007(3) -0.002(3) C55 0.031(4) 0.030(5) 0.034(4) -0.008(4) 0.008(3) -0.009(4) C56 0.040(5) 0.027(5) 0.023(4) 0.004(3) -0.001(3) -0.014(4) C57 0.038(5) 0.016(4) 0.026(4) 0.006(3) -0.004(3) -0.003(3) C58 0.021(4) 0.017(4) 0.027(4) -0.002(3) -0.004(3) -0.002(3) C59 0.019(4) 0.026(5) 0.053(5) 0.010(4) -0.005(4) 0.002(3) C61 0.021(4) 0.019(4) 0.021(4) 0.002(3) 0.002(3) -0.001(3) C62 0.018(4) 0.022(4) 0.023(4) 0.004(3) -0.001(3) 0.000(3) C63 0.018(4) 0.020(4) 0.021(3) 0.001(3) -0.001(3) 0.000(3) C64 0.018(4) 0.019(4) 0.030(4) 0.002(3) -0.001(3) -0.005(3) C65 0.030(4) 0.019(4) 0.023(4) -0.004(3) -0.006(3) 0.000(3) C66 0.031(4) 0.017(4) 0.042(5) 0.000(4) -0.013(4) -0.002(3) C67 0.022(4) 0.017(4) 0.034(4) 0.007(3) -0.001(3) 0.000(3) C68 0.012(3) 0.020(4) 0.029(4) 0.005(3) -0.003(3) 0.002(3) C69 0.014(4) 0.039(5) 0.039(4) 0.003(4) 0.005(3) -0.008(3) N71 0.107(9) 0.076(7) 0.046(5) -0.011(5) -0.025(5) -0.002(6) C71 0.038(5) 0.054(7) 0.035(5) 0.000(5) -0.008(4) -0.010(5) C72 0.054(6) 0.051(7) 0.039(5) -0.001(5) -0.012(4) 0.003(5) C73 0.071(7) 0.038(6) 0.029(4) 0.003(4) 0.001(5) -0.017(5) C74 0.043(6) 0.069(8) 0.038(5) -0.019(5) -0.001(4) -0.023(5) C75 0.020(4) 0.056(6) 0.017(4) 0.008(4) -0.004(3) -0.003(4) N81 0.061(7) 0.097(9) 0.072(7) 0.023(6) -0.014(5) -0.013(5) C81 0.055(7) 0.105(11) 0.061(8) 0.030(8) 0.002(6) 0.012(7) C82 0.128(13) 0.081(11) 0.068(9) -0.033(8) 0.006(8) 0.015(9) C83 0.188(17) 0.044(9) 0.127(13) -0.014(9) 0.075(13) -0.015(9) C84 0.103(10) 0.074(10) 0.063(8) 0.015(7) 0.040(7) 0.033(8) C85 0.029(6) 0.092(10) 0.056(7) 0.013(6) -0.003(4) 0.002(6) N91 0.091(9) 0.142(12) 0.066(7) 0.024(7) 0.004(6) 0.020(8) C91 0.058(7) 0.047(7) 0.063(7) 0.009(5) -0.015(5) -0.002(5) C92 0.049(7) 0.043(7) 0.078(7) 0.012(6) 0.011(6) 0.011(5) C93 0.043(6) 0.060(8) 0.076(7) 0.029(6) 0.015(5) 0.006(6) C94 0.050(7) 0.068(8) 0.051(6) 0.018(6) -0.016(5) -0.005(6) C95 0.046(6) 0.069(7) 0.021(4) -0.008(4) -0.005(4) -0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 U N51 2.527(6) . ? U N11 2.543(5) . ? U N21 2.554(6) . ? U N41 2.555(5) . ? U N61 2.562(5) . ? U N31 2.576(6) . ? U N1 2.750(5) . ? U N2 2.756(5) . ? N1 C31 1.474(8) . ? N1 C11 1.483(8) . ? N1 C21 1.498(8) . ? N2 C61 1.469(8) . ? N2 C41 1.479(8) . ? N2 C51 1.492(8) . ? N11 C12 1.314(8) . ? N11 C13 1.392(8) . ? N12 C12 1.355(8) . ? N12 C18 1.399(9) . ? N12 C19 1.452(8) . ? N21 C22 1.338(9) . ? N21 C23 1.408(8) . ? N22 C22 1.356(8) . ? N22 C28 1.382(9) . ? N22 C29 1.479(9) . ? N31 C32 1.320(8) . ? N31 C33 1.398(8) . ? N32 C32 1.348(9) . ? N32 C38 1.398(9) . ? N32 C39 1.457(9) . ? N41 C42 1.323(8) . ? N41 C43 1.396(8) . ? N42 C42 1.350(8) . ? N42 C48 1.380(9) . ? N42 C49 1.469(9) . ? N51 C52 1.335(8) . ? N51 C53 1.396(8) . ? N52 C52 1.347(8) . ? N52 C58 1.379(8) . ? N52 C59 1.466(8) . ? N61 C62 1.324(8) . ? N61 C63 1.396(8) . ? N62 C62 1.364(8) . ? N62 C68 1.385(9) . ? N62 C69 1.480(8) . ? C11 C12 1.508(9) . ? C13 C18 1.385(9) . ? C13 C14 1.418(9) . ? C14 C15 1.372(9) . ? C15 C16 1.377(10) . ? C16 C17 1.386(10) . ? C17 C18 1.375(10) . ? C21 C22 1.485(10) . ? C23 C28 1.392(9) . ? C23 C24 1.392(10) . ? C24 C25 1.362(10) . ? C25 C26 1.419(11) . ? C26 C27 1.389(11) . ? C27 C28 1.396(10) . ? C31 C32 1.483(9) . ? C33 C38 1.379(10) . ? C33 C34 1.393(9) . ? C34 C35 1.373(10) . ? C35 C36 1.377(11) . ? C36 C37 1.390(11) . ? C37 C38 1.377(10) . ? C41 C42 1.505(9) . ? C43 C48 1.392(10) . ? C43 C44 1.393(10) . ? C44 C45 1.362(10) . ? C45 C46 1.394(11) . ? C46 C47 1.372(11) . ? C47 C48 1.396(9) . ? C51 C52 1.473(9) . ? C53 C58 1.404(10) . ? C53 C54 1.410(9) . ? C54 C55 1.387(10) . ? C55 C56 1.382(11) . ? C56 C57 1.392(10) . ? C57 C58 1.387(9) . ? C61 C62 1.491(9) . ? C63 C68 1.388(9) . ? C63 C64 1.389(9) . ? C64 C65 1.374(9) . ? C65 C66 1.393(10) . ? C66 C67 1.382(10) . ? C67 C68 1.392(9) . ? N71 C75 1.312(11) . ? N71 C71 1.400(12) . ? C71 C72 1.372(12) . ? C72 C73 1.389(12) . ? C73 C74 1.356(13) . ? C74 C75 1.292(12) . ? N81 C85 1.278(12) . ? N81 C81 1.287(14) . ? C81 C82 1.361(17) . ? C82 C83 1.391(17) . ? C83 C84 1.390(18) . ? C84 C85 1.328(15) . ? N91 C95 1.311(13) . ? N91 C91 1.440(14) . ? C91 C92 1.389(13) . ? C92 C93 1.332(14) . ? C93 C94 1.355(13) . ? C94 C95 1.285(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N51 U N11 78.12(17) . . ? N51 U N21 80.19(18) . . ? N11 U N21 100.27(16) . . ? N51 U N41 103.82(18) . . ? N11 U N41 175.53(17) . . ? N21 U N41 76.26(16) . . ? N51 U N61 97.96(17) . . ? N11 U N61 85.23(16) . . ? N21 U N61 173.64(17) . . ? N41 U N61 98.40(16) . . ? N51 U N31 172.06(16) . . ? N11 U N31 96.02(17) . . ? N21 U N31 106.33(18) . . ? N41 U N31 82.41(17) . . ? N61 U N31 76.04(18) . . ? N51 U N1 117.65(16) . . ? N11 U N1 62.96(16) . . ? N21 U N1 62.85(16) . . ? N41 U N1 112.69(16) . . ? N61 U N1 123.03(16) . . ? N31 U N1 63.13(17) . . ? N51 U N2 62.69(16) . . ? N11 U N2 122.22(16) . . ? N21 U N2 111.90(16) . . ? N41 U N2 62.05(16) . . ? N61 U N2 62.09(16) . . ? N31 U N2 117.48(16) . . ? N1 U N2 173.94(15) . . ? C31 N1 C11 110.3(5) . . ? C31 N1 C21 109.6(5) . . ? C11 N1 C21 109.4(5) . . ? C31 N1 U 111.2(4) . . ? C11 N1 U 107.8(4) . . ? C21 N1 U 108.5(4) . . ? C61 N2 C41 111.0(5) . . ? C61 N2 C51 110.4(5) . . ? C41 N2 C51 109.5(5) . . ? C61 N2 U 108.7(4) . . ? C41 N2 U 107.7(4) . . ? C51 N2 U 109.5(4) . . ? C12 N11 C13 104.4(5) . . ? C12 N11 U 115.3(4) . . ? C13 N11 U 129.9(4) . . ? C12 N12 C18 107.0(5) . . ? C12 N12 C19 126.6(6) . . ? C18 N12 C19 126.4(6) . . ? C22 N21 C23 104.5(6) . . ? C22 N21 U 114.8(4) . . ? C23 N21 U 131.4(4) . . ? C22 N22 C28 106.9(6) . . ? C22 N22 C29 125.6(6) . . ? C28 N22 C29 127.4(6) . . ? C32 N31 C33 105.5(6) . . ? C32 N31 U 118.8(4) . . ? C33 N31 U 133.0(4) . . ? C32 N32 C38 107.4(6) . . ? C32 N32 C39 125.6(6) . . ? C38 N32 C39 126.9(6) . . ? C42 N41 C43 105.0(6) . . ? C42 N41 U 113.5(4) . . ? C43 N41 U 127.4(4) . . ? C42 N42 C48 107.0(6) . . ? C42 N42 C49 126.8(6) . . ? C48 N42 C49 126.2(6) . . ? C52 N51 C53 104.8(6) . . ? C52 N51 U 115.7(4) . . ? C53 N51 U 128.0(4) . . ? C52 N52 C58 107.5(5) . . ? C52 N52 C59 125.6(6) . . ? C58 N52 C59 126.9(6) . . ? C62 N61 C63 104.9(5) . . ? C62 N61 U 116.7(4) . . ? C63 N61 U 133.0(4) . . ? C62 N62 C68 106.7(5) . . ? C62 N62 C69 125.5(6) . . ? C68 N62 C69 127.8(6) . . ? N1 C11 C12 109.6(5) . . ? N11 C12 N12 113.3(6) . . ? N11 C12 C11 124.1(6) . . ? N12 C12 C11 122.5(6) . . ? C18 C13 N11 110.9(6) . . ? C18 C13 C14 118.8(6) . . ? N11 C13 C14 130.3(6) . . ? C15 C14 C13 117.5(6) . . ? C14 C15 C16 121.8(7) . . ? C15 C16 C17 122.2(7) . . ? C18 C17 C16 115.7(7) . . ? C17 C18 C13 124.0(7) . . ? C17 C18 N12 131.7(7) . . ? C13 C18 N12 104.3(6) . . ? C22 C21 N1 109.7(6) . . ? N21 C22 N22 112.9(6) . . ? N21 C22 C21 124.4(6) . . ? N22 C22 C21 122.6(6) . . ? C28 C23 C24 120.6(6) . . ? C28 C23 N21 109.1(6) . . ? C24 C23 N21 130.3(6) . . ? C25 C24 C23 118.8(7) . . ? C24 C25 C26 120.6(8) . . ? C27 C26 C25 121.5(7) . . ? C26 C27 C28 116.6(7) . . ? N22 C28 C23 106.5(6) . . ? N22 C28 C27 131.6(7) . . ? C23 C28 C27 121.9(7) . . ? N1 C31 C32 110.6(5) . . ? N31 C32 N32 112.3(6) . . ? N31 C32 C31 124.3(6) . . ? N32 C32 C31 123.1(6) . . ? C38 C33 C34 119.9(7) . . ? C38 C33 N31 109.6(6) . . ? C34 C33 N31 130.5(7) . . ? C35 C34 C33 117.6(7) . . ? C34 C35 C36 121.8(7) . . ? C35 C36 C37 121.3(7) . . ? C38 C37 C36 116.4(8) . . ? C37 C38 C33 122.9(7) . . ? C37 C38 N32 131.9(7) . . ? C33 C38 N32 105.2(6) . . ? N2 C41 C42 109.3(5) . . ? N41 C42 N42 113.0(6) . . ? N41 C42 C41 123.5(6) . . ? N42 C42 C41 123.5(6) . . ? C48 C43 C44 120.2(7) . . ? C48 C43 N41 109.1(6) . . ? C44 C43 N41 130.7(7) . . ? C45 C44 C43 118.2(7) . . ? C44 C45 C46 120.6(8) . . ? C47 C46 C45 123.3(7) . . ? C46 C47 C48 115.3(7) . . ? N42 C48 C43 106.0(6) . . ? N42 C48 C47 131.7(7) . . ? C43 C48 C47 122.4(7) . . ? C52 C51 N2 110.7(5) . . ? N51 C52 N52 112.9(6) . . ? N51 C52 C51 123.6(6) . . ? N52 C52 C51 123.5(6) . . ? N51 C53 C58 109.1(6) . . ? N51 C53 C54 129.5(7) . . ? C58 C53 C54 121.4(6) . . ? C55 C54 C53 115.7(7) . . ? C56 C55 C54 122.3(7) . . ? C55 C56 C57 122.7(7) . . ? C58 C57 C56 115.7(7) . . ? N52 C58 C57 132.2(7) . . ? N52 C58 C53 105.7(6) . . ? C57 C58 C53 122.1(7) . . ? N2 C61 C62 109.4(5) . . ? N61 C62 N62 112.8(6) . . ? N61 C62 C61 123.5(6) . . ? N62 C62 C61 123.6(6) . . ? C68 C63 C64 120.8(6) . . ? C68 C63 N61 109.7(6) . . ? C64 C63 N61 129.5(6) . . ? C65 C64 C63 116.6(7) . . ? C64 C65 C66 122.1(7) . . ? C67 C66 C65 122.3(7) . . ? C66 C67 C68 114.9(7) . . ? N62 C68 C63 105.9(6) . . ? N62 C68 C67 130.9(6) . . ? C63 C68 C67 123.3(7) . . ? C75 N71 C71 122.7(9) . . ? C72 C71 N71 118.2(9) . . ? C71 C72 C73 117.8(9) . . ? C74 C73 C72 118.5(9) . . ? C75 C74 C73 124.7(9) . . ? C74 C75 N71 118.1(9) . . ? C85 N81 C81 116.4(11) . . ? N81 C81 C82 124.1(12) . . ? C81 C82 C83 117.0(12) . . ? C84 C83 C82 118.9(13) . . ? C85 C84 C83 114.7(11) . . ? N81 C85 C84 128.6(12) . . ? C95 N91 C91 120.7(10) . . ? C92 C91 N91 118.2(10) . . ? C93 C92 C91 117.1(10) . . ? C92 C93 C94 120.9(10) . . ? C95 C94 C93 124.5(11) . . ? C94 C95 N91 118.5(10) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.999 _refine_diff_density_min -2.108 _refine_diff_density_rms 0.237 #===END data_struc2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H23 I3 N5 U' _chemical_formula_weight 988.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6979(6) _cell_length_b 15.3561(9) _cell_length_c 9.9489(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.8940(10) _cell_angle_gamma 90.00 _cell_volume 1332.86(14) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour noir _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 9.583 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8613 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.93 _reflns_number_total 5730 _reflns_number_gt 5532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(6) _refine_ls_number_reflns 5730 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 U U 0.77085(3) 0.75346(2) -0.14848(3) 0.01447(9) Uani 1 1 d . . . I1 I 0.84006(8) 0.58430(4) -0.30768(7) 0.02504(15) Uani 1 1 d . . . I2 I 0.55830(8) 0.81514(5) 0.01764(7) 0.02691(15) Uani 1 1 d . . . I3 I 1.09798(7) 0.80372(5) 0.11099(6) 0.02259(14) Uani 1 1 d . . . N1 N 0.9071(9) 0.8022(6) -0.3163(9) 0.0186(15) Uani 1 1 d . . . N2 N 0.7201(10) 0.9246(6) -0.1789(9) 0.0246(17) Uani 1 1 d . . . N3 N 0.5057(9) 0.6743(6) -0.2903(10) 0.0242(18) Uani 1 1 d . . . N4 N 0.5868(9) 0.8153(6) -0.4179(8) 0.0181(15) Uani 1 1 d . . . N5 N 0.8118(10) 0.6250(6) 0.0516(9) 0.0227(17) Uani 1 1 d . . . C1 C 0.6625(11) 0.8607(8) -0.5004(11) 0.027(2) Uani 1 1 d . . . H1A H 0.6631 0.9241 -0.4819 0.032 Uiso 1 1 calc R . . H1B H 0.6011 0.8510 -0.6088 0.032 Uiso 1 1 calc R . . C2 C 0.8252(10) 0.8310(7) -0.4568(10) 0.0197(19) Uani 1 1 d . . . C3 C 0.8867(12) 0.8385(7) -0.5588(11) 0.024(2) Uani 1 1 d . . . H3A H 0.8258 0.8587 -0.6575 0.029 Uiso 1 1 calc R . . C4 C 1.0399(12) 0.8157(9) -0.5134(12) 0.029(2) Uani 1 1 d . . . H4A H 1.0855 0.8213 -0.5802 0.035 Uiso 1 1 calc R . . C5 C 1.1252(11) 0.7847(7) -0.3686(12) 0.025(2) Uani 1 1 d . . . H5A H 1.2288 0.7671 -0.3358 0.030 Uiso 1 1 calc R . . C6 C 1.0551(11) 0.7803(7) -0.2744(11) 0.022(2) Uani 1 1 d . . . H6A H 1.1140 0.7609 -0.1748 0.027 Uiso 1 1 calc R . . C7 C 0.4838(10) 0.8786(7) -0.3914(10) 0.0208(19) Uani 1 1 d . . . H7A H 0.4208 0.8476 -0.3507 0.025 Uiso 1 1 calc R . . H7B H 0.4139 0.9062 -0.4870 0.025 Uiso 1 1 calc R . . C8 C 0.5792(11) 0.9473(6) -0.2828(11) 0.0198(18) Uani 1 1 d . . . C9 C 0.5159(12) 1.0289(7) -0.2856(12) 0.025(2) Uani 1 1 d . . . H9A H 0.4167 1.0433 -0.3602 0.030 Uiso 1 1 calc R . . C10 C 0.6027(14) 1.0890(8) -0.1755(13) 0.031(2) Uani 1 1 d . . . H10A H 0.5624 1.1450 -0.1724 0.038 Uiso 1 1 calc R . . C11 C 0.7490(13) 1.0656(7) -0.0706(13) 0.030(2) Uani 1 1 d . . . H11A H 0.8110 1.1056 0.0041 0.035 Uiso 1 1 calc R . . C12 C 0.8026(12) 0.9829(8) -0.0770(12) 0.026(2) Uani 1 1 d . . . H12A H 0.9026 0.9673 -0.0055 0.032 Uiso 1 1 calc R . . C13 C 0.4962(11) 0.7422(7) -0.5145(10) 0.024(2) Uani 1 1 d . . . H13A H 0.5633 0.7079 -0.5462 0.029 Uiso 1 1 calc R . . H13B H 0.4123 0.7667 -0.6055 0.029 Uiso 1 1 calc R . . C14 C 0.4279(11) 0.6819(7) -0.4394(11) 0.0218(19) Uani 1 1 d . . . C15 C 0.2960(11) 0.6363(7) -0.5192(12) 0.025(2) Uani 1 1 d . . . H15A H 0.2426 0.6444 -0.6241 0.030 Uiso 1 1 calc R . . C16 C 0.2392(12) 0.5783(8) -0.4491(13) 0.030(2) Uani 1 1 d . . . H16A H 0.1488 0.5456 -0.5045 0.036 Uiso 1 1 calc R . . C17 C 0.3178(12) 0.5697(8) -0.2970(13) 0.030(2) Uani 1 1 d . . . H17A H 0.2818 0.5308 -0.2451 0.036 Uiso 1 1 calc R . . C18 C 0.4498(12) 0.6178(8) -0.2191(14) 0.031(2) Uani 1 1 d . . . H18A H 0.5030 0.6116 -0.1137 0.037 Uiso 1 1 calc R . . C21 C 0.8455(11) 0.6548(7) 0.1889(10) 0.0217(19) Uani 1 1 d . . . H21A H 0.8631 0.7154 0.2081 0.026 Uiso 1 1 calc R . . C22 C 0.8555(13) 0.5997(8) 0.3054(12) 0.027(2) Uani 1 1 d . . . H22A H 0.8791 0.6229 0.4016 0.033 Uiso 1 1 calc R . . C23 C 0.8313(14) 0.5137(8) 0.2795(13) 0.033(2) Uani 1 1 d . . . H23A H 0.8391 0.4752 0.3572 0.040 Uiso 1 1 calc R . . C24 C 0.7939(13) 0.4817(7) 0.1339(13) 0.030(2) Uani 1 1 d . . . H24A H 0.7738 0.4215 0.1117 0.036 Uiso 1 1 calc R . . C25 C 0.7874(13) 0.5387(7) 0.0263(12) 0.028(2) Uani 1 1 d . . . H25A H 0.7647 0.5168 -0.0704 0.033 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 U 0.01700(14) 0.01419(16) 0.01277(14) 0.00193(12) 0.00701(11) 0.00037(12) I1 0.0353(3) 0.0218(3) 0.0202(3) -0.0014(2) 0.0141(3) 0.0018(3) I2 0.0288(3) 0.0308(4) 0.0260(3) 0.0011(3) 0.0164(3) 0.0048(3) I3 0.0213(3) 0.0265(4) 0.0171(3) 0.0018(2) 0.0058(2) -0.0013(2) N1 0.026(4) 0.018(4) 0.020(4) 0.003(3) 0.018(3) -0.003(3) N2 0.027(4) 0.023(5) 0.022(4) 0.001(3) 0.009(3) -0.002(4) N3 0.021(4) 0.026(5) 0.026(4) 0.003(3) 0.011(3) -0.005(3) N4 0.022(4) 0.015(4) 0.017(3) 0.002(3) 0.008(3) 0.002(3) N5 0.038(5) 0.016(4) 0.017(4) 0.003(3) 0.015(4) -0.003(3) C1 0.026(5) 0.035(6) 0.021(4) 0.015(4) 0.012(4) 0.004(4) C2 0.019(4) 0.025(5) 0.016(4) 0.004(3) 0.009(3) -0.004(3) C3 0.035(5) 0.025(5) 0.019(4) -0.002(4) 0.016(4) -0.003(4) C4 0.034(5) 0.036(6) 0.025(5) -0.005(5) 0.021(4) 0.004(5) C5 0.021(4) 0.025(5) 0.031(5) -0.002(4) 0.013(4) -0.001(4) C6 0.029(5) 0.022(5) 0.020(4) -0.001(3) 0.015(4) 0.003(3) C7 0.021(4) 0.025(5) 0.019(4) 0.007(4) 0.010(4) 0.012(4) C8 0.024(4) 0.015(5) 0.023(4) 0.008(3) 0.011(4) 0.003(3) C9 0.033(5) 0.018(5) 0.029(5) 0.000(4) 0.018(4) 0.011(4) C10 0.046(6) 0.016(5) 0.034(5) 0.003(4) 0.019(5) 0.008(5) C11 0.033(5) 0.015(5) 0.031(5) -0.001(4) 0.006(4) 0.001(4) C12 0.025(5) 0.028(6) 0.026(5) 0.005(4) 0.011(4) 0.004(4) C13 0.030(5) 0.027(6) 0.013(4) -0.009(4) 0.007(3) -0.002(4) C14 0.025(4) 0.018(5) 0.028(5) -0.005(4) 0.017(4) 0.002(4) C15 0.024(5) 0.022(5) 0.026(5) -0.005(4) 0.009(4) 0.004(4) C16 0.030(5) 0.021(5) 0.042(6) -0.007(5) 0.018(5) -0.006(4) C17 0.025(5) 0.021(6) 0.039(6) 0.001(4) 0.010(4) -0.006(4) C18 0.026(5) 0.031(6) 0.038(6) -0.002(5) 0.016(5) -0.009(4) C21 0.033(5) 0.017(5) 0.015(4) 0.002(3) 0.011(4) 0.001(4) C22 0.038(6) 0.025(6) 0.023(5) 0.005(4) 0.018(4) 0.006(4) C23 0.040(6) 0.030(6) 0.037(6) 0.011(5) 0.022(5) 0.002(5) C24 0.041(6) 0.017(5) 0.036(6) -0.002(4) 0.020(5) -0.007(4) C25 0.040(6) 0.011(5) 0.028(5) 0.001(4) 0.013(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 U N3 2.629(8) . ? U N1 2.650(7) . ? U N4 2.663(7) . ? U N2 2.666(10) . ? U N5 2.706(8) . ? U I3 3.1893(7) . ? U I1 3.2612(7) . ? U I2 3.2944(7) . ? N1 C2 1.345(12) . ? N1 C6 1.351(12) . ? N2 C12 1.327(15) . ? N2 C8 1.350(13) . ? N3 C14 1.343(13) . ? N3 C18 1.372(14) . ? N4 C13 1.489(12) . ? N4 C1 1.492(12) . ? N4 C7 1.498(12) . ? N5 C21 1.339(12) . ? N5 C25 1.351(14) . ? C1 C2 1.513(13) . ? C2 C3 1.389(13) . ? C3 C4 1.395(14) . ? C4 C5 1.395(15) . ? C5 C6 1.379(14) . ? C7 C8 1.504(14) . ? C8 C9 1.390(14) . ? C9 C10 1.398(16) . ? C10 C11 1.393(16) . ? C11 C12 1.383(16) . ? C13 C14 1.512(15) . ? C14 C15 1.368(14) . ? C15 C16 1.384(17) . ? C16 C17 1.371(17) . ? C17 C18 1.385(15) . ? C21 C22 1.404(14) . ? C22 C23 1.347(18) . ? C23 C24 1.419(17) . ? C24 C25 1.362(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U N1 115.6(3) . . ? N3 U N4 63.7(3) . . ? N1 U N4 64.2(2) . . ? N3 U N2 107.8(3) . . ? N1 U N2 76.6(3) . . ? N4 U N2 61.7(3) . . ? N3 U N5 81.5(3) . . ? N1 U N5 135.7(3) . . ? N4 U N5 145.0(3) . . ? N2 U N5 139.7(3) . . ? N3 U I3 160.11(19) . . ? N1 U I3 81.27(18) . . ? N4 U I3 136.13(18) . . ? N2 U I3 85.55(18) . . ? N5 U I3 78.83(19) . . ? N3 U I1 74.4(2) . . ? N1 U I1 69.75(19) . . ? N4 U I1 89.11(18) . . ? N2 U I1 142.84(19) . . ? N5 U I1 77.37(19) . . ? I3 U I1 104.057(19) . . ? N3 U I2 73.9(2) . . ? N1 U I2 145.93(19) . . ? N4 U I2 96.40(17) . . ? N2 U I2 69.4(2) . . ? N5 U I2 76.32(19) . . ? I3 U I2 98.252(19) . . ? I1 U I2 141.19(2) . . ? C2 N1 C6 117.9(8) . . ? C2 N1 U 121.1(6) . . ? C6 N1 U 119.4(6) . . ? C12 N2 C8 118.8(10) . . ? C12 N2 U 124.0(7) . . ? C8 N2 U 114.6(7) . . ? C14 N3 C18 117.9(9) . . ? C14 N3 U 119.9(7) . . ? C18 N3 U 122.0(7) . . ? C13 N4 C1 106.9(8) . . ? C13 N4 C7 110.6(8) . . ? C1 N4 C7 108.6(8) . . ? C13 N4 U 109.2(6) . . ? C1 N4 U 116.5(5) . . ? C7 N4 U 105.0(5) . . ? C21 N5 C25 118.1(9) . . ? C21 N5 U 113.2(7) . . ? C25 N5 U 128.4(7) . . ? N4 C1 C2 113.8(8) . . ? N1 C2 C3 122.6(9) . . ? N1 C2 C1 117.8(8) . . ? C3 C2 C1 119.5(9) . . ? C2 C3 C4 118.6(10) . . ? C5 C4 C3 119.2(9) . . ? C6 C5 C4 118.2(9) . . ? N1 C6 C5 123.4(9) . . ? N4 C7 C8 109.5(7) . . ? N2 C8 C9 122.6(10) . . ? N2 C8 C7 117.9(9) . . ? C9 C8 C7 119.3(9) . . ? C8 C9 C10 118.1(10) . . ? C11 C10 C9 118.9(10) . . ? C12 C11 C10 118.9(10) . . ? N2 C12 C11 122.8(10) . . ? N4 C13 C14 113.9(7) . . ? N3 C14 C15 121.8(10) . . ? N3 C14 C13 116.3(8) . . ? C15 C14 C13 121.8(9) . . ? C14 C15 C16 120.9(10) . . ? C17 C16 C15 117.8(10) . . ? C16 C17 C18 119.9(11) . . ? N3 C18 C17 121.7(11) . . ? N5 C21 C22 122.3(10) . . ? C23 C22 C21 119.3(10) . . ? C22 C23 C24 118.7(11) . . ? C25 C24 C23 118.9(11) . . ? N5 C25 C24 122.7(10) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 2.185 _refine_diff_density_min -3.525 _refine_diff_density_rms 0.300 #===END data_struc3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H23 I3 La N5' _chemical_formula_weight 889.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7180(5) _cell_length_b 15.3889(8) _cell_length_c 9.9741(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.8260(10) _cell_angle_gamma 90.00 _cell_volume 1342.64(12) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 5.060 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8639 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.89 _reflns_number_total 6035 _reflns_number_gt 5890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 6035 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 La La 0.77299(4) 0.75358(2) -0.14709(3) 0.01642(9) Uani 1 1 d . . . I1 I 0.84260(5) 0.58312(3) -0.30677(5) 0.02780(11) Uani 1 1 d . . . I2 I 0.55776(5) 0.81470(3) 0.01884(5) 0.03037(12) Uani 1 1 d . . . I3 I 1.10165(5) 0.80510(3) 0.11132(4) 0.02521(11) Uani 1 1 d . . . N1 N 0.9089(6) 0.8041(4) -0.3162(6) 0.0194(10) Uani 1 1 d . . . N2 N 0.7177(7) 0.9245(4) -0.1791(6) 0.0240(11) Uani 1 1 d . . . N3 N 0.5034(6) 0.6741(4) -0.2927(6) 0.0228(11) Uani 1 1 d . . . N4 N 0.5871(6) 0.8167(4) -0.4205(6) 0.0196(10) Uani 1 1 d . . . N5 N 0.8143(7) 0.6246(4) 0.0534(7) 0.0258(12) Uani 1 1 d . . . C1 C 0.6665(7) 0.8630(5) -0.4974(7) 0.0247(13) Uani 1 1 d . . . H1A H 0.6702 0.9256 -0.4737 0.030 Uiso 1 1 calc R . . H1B H 0.6050 0.8565 -0.6063 0.030 Uiso 1 1 calc R . . C2 C 0.8260(8) 0.8323(5) -0.4579(8) 0.0231(13) Uani 1 1 d . . . C3 C 0.8869(9) 0.8400(5) -0.5591(8) 0.0278(15) Uani 1 1 d . . . H3 H 0.8259 0.8605 -0.6572 0.033 Uiso 1 1 calc R . . C4 C 1.0397(8) 0.8173(6) -0.5151(8) 0.0306(15) Uani 1 1 d . . . H4 H 1.0845 0.8230 -0.5823 0.037 Uiso 1 1 calc R . . C5 C 1.1245(9) 0.7863(5) -0.3726(9) 0.0289(16) Uani 1 1 d . . . H5 H 1.2284 0.7700 -0.3403 0.035 Uiso 1 1 calc R . . C6 C 1.0551(8) 0.7797(5) -0.2778(8) 0.0262(14) Uani 1 1 d . . . H6 H 1.1130 0.7568 -0.1808 0.031 Uiso 1 1 calc R . . C7 C 0.4860(7) 0.8782(5) -0.3923(7) 0.0227(13) Uani 1 1 d . . . H7A H 0.4244 0.8462 -0.3513 0.027 Uiso 1 1 calc R . . H7B H 0.4148 0.9053 -0.4874 0.027 Uiso 1 1 calc R . . C8 C 0.5765(8) 0.9479(4) -0.2847(7) 0.0213(12) Uani 1 1 d . . . C9 C 0.5165(8) 1.0297(5) -0.2855(8) 0.0275(14) Uani 1 1 d . . . H9 H 0.4184 1.0447 -0.3608 0.033 Uiso 1 1 calc R . . C10 C 0.5993(9) 1.0893(5) -0.1770(9) 0.0308(15) Uani 1 1 d . . . H10 H 0.5582 1.1451 -0.1753 0.037 Uiso 1 1 calc R . . C11 C 0.7436(9) 1.0663(5) -0.0702(9) 0.0315(16) Uani 1 1 d . . . H11 H 0.8030 1.1060 0.0061 0.038 Uiso 1 1 calc R . . C12 C 0.7992(9) 0.9845(5) -0.0770(8) 0.0278(14) Uani 1 1 d . . . H12 H 0.8997 0.9700 -0.0063 0.033 Uiso 1 1 calc R . . C13 C 0.4976(7) 0.7423(5) -0.5168(7) 0.0219(12) Uani 1 1 d . . . H13A H 0.5659 0.7075 -0.5460 0.026 Uiso 1 1 calc R . . H13B H 0.4146 0.7659 -0.6089 0.026 Uiso 1 1 calc R . . C14 C 0.4283(8) 0.6832(5) -0.4400(7) 0.0220(12) Uani 1 1 d . . . C15 C 0.2956(8) 0.6376(5) -0.5244(8) 0.0278(15) Uani 1 1 d . . . H15 H 0.2437 0.6457 -0.6291 0.033 Uiso 1 1 calc R . . C16 C 0.2405(9) 0.5803(6) -0.4538(9) 0.0344(16) Uani 1 1 d . . . H16 H 0.1505 0.5477 -0.5094 0.041 Uiso 1 1 calc R . . C17 C 0.3179(8) 0.5707(6) -0.2998(9) 0.0320(16) Uani 1 1 d . . . H17 H 0.2832 0.5311 -0.2481 0.038 Uiso 1 1 calc R . . C18 C 0.4459(9) 0.6204(5) -0.2256(9) 0.0307(15) Uani 1 1 d . . . H18 H 0.4966 0.6162 -0.1201 0.037 Uiso 1 1 calc R . . C21 C 0.8473(8) 0.6535(5) 0.1926(8) 0.0268(14) Uani 1 1 d . . . H21 H 0.8638 0.7140 0.2118 0.032 Uiso 1 1 calc R . . C22 C 0.8583(9) 0.6001(6) 0.3080(8) 0.0313(16) Uani 1 1 d . . . H22 H 0.8856 0.6228 0.4049 0.038 Uiso 1 1 calc R . . C23 C 0.8284(9) 0.5124(6) 0.2785(8) 0.0324(16) Uani 1 1 d . . . H23 H 0.8298 0.4740 0.3537 0.039 Uiso 1 1 calc R . . C24 C 0.7966(10) 0.4818(6) 0.1381(9) 0.0357(17) Uani 1 1 d . . . H24 H 0.7788 0.4216 0.1163 0.043 Uiso 1 1 calc R . . C25 C 0.7906(8) 0.5392(5) 0.0292(8) 0.0262(14) Uani 1 1 d . . . H25 H 0.7688 0.5171 -0.0669 0.031 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 La 0.01204(15) 0.02055(16) 0.01342(15) 0.00203(12) 0.00252(12) 0.00015(12) I1 0.0313(2) 0.0289(2) 0.0213(2) -0.00167(17) 0.00978(18) 0.00208(18) I2 0.0251(2) 0.0396(3) 0.0279(2) 0.0019(2) 0.01288(18) 0.0054(2) I3 0.01681(19) 0.0334(2) 0.01844(19) 0.00228(16) 0.00116(15) -0.00135(17) N1 0.014(2) 0.026(3) 0.016(2) 0.004(2) 0.0049(19) 0.000(2) N2 0.020(3) 0.022(3) 0.024(3) 0.001(2) 0.005(2) 0.004(2) N3 0.014(2) 0.029(3) 0.019(3) -0.004(2) 0.002(2) -0.005(2) N4 0.013(2) 0.023(3) 0.017(2) -0.001(2) 0.0012(19) 0.001(2) N5 0.027(3) 0.027(3) 0.020(3) 0.008(2) 0.007(2) 0.003(2) C1 0.015(3) 0.036(4) 0.018(3) 0.008(3) 0.003(2) 0.001(3) C2 0.021(3) 0.023(3) 0.023(3) -0.002(2) 0.008(3) -0.002(2) C3 0.030(4) 0.034(4) 0.020(3) 0.003(3) 0.011(3) -0.001(3) C4 0.029(4) 0.041(4) 0.028(3) -0.011(3) 0.018(3) -0.006(3) C5 0.023(3) 0.032(4) 0.034(4) -0.010(3) 0.015(3) -0.008(3) C6 0.023(3) 0.030(3) 0.023(3) -0.003(2) 0.007(3) -0.002(3) C7 0.015(3) 0.026(3) 0.022(3) 0.003(3) 0.003(2) 0.001(2) C8 0.018(3) 0.026(3) 0.019(3) -0.001(2) 0.008(2) -0.001(2) C9 0.025(3) 0.032(4) 0.023(3) 0.005(3) 0.008(3) 0.006(3) C10 0.032(4) 0.025(3) 0.033(4) 0.002(3) 0.012(3) 0.007(3) C11 0.033(4) 0.026(4) 0.027(3) -0.004(3) 0.006(3) 0.000(3) C12 0.027(4) 0.023(3) 0.026(3) 0.003(3) 0.005(3) -0.002(3) C13 0.014(3) 0.029(3) 0.015(3) 0.000(2) 0.000(2) -0.002(3) C14 0.015(3) 0.027(3) 0.020(3) 0.001(2) 0.004(2) 0.001(2) C15 0.018(3) 0.028(3) 0.027(3) -0.011(3) 0.001(3) 0.003(3) C16 0.021(3) 0.033(4) 0.042(4) -0.012(4) 0.007(3) -0.006(3) C17 0.018(3) 0.036(4) 0.040(4) -0.003(3) 0.011(3) -0.003(3) C18 0.024(3) 0.037(4) 0.027(3) 0.002(3) 0.007(3) -0.008(3) C21 0.025(3) 0.030(4) 0.022(3) 0.006(3) 0.007(3) 0.001(3) C22 0.027(4) 0.042(4) 0.024(3) 0.006(3) 0.010(3) 0.000(3) C23 0.034(4) 0.035(4) 0.029(4) 0.013(3) 0.014(3) 0.000(3) C24 0.033(4) 0.029(4) 0.038(4) 0.008(3) 0.009(3) 0.003(3) C25 0.023(3) 0.029(3) 0.022(3) -0.003(3) 0.006(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 La N1 2.670(5) . ? La N3 2.675(6) . ? La N2 2.676(6) . ? La N4 2.712(5) . ? La N5 2.720(6) . ? La I3 3.2095(5) . ? La I1 3.2885(6) . ? La I2 3.3189(5) . ? N1 C6 1.353(9) . ? N1 C2 1.358(9) . ? N2 C12 1.347(9) . ? N2 C8 1.365(9) . ? N3 C18 1.330(10) . ? N3 C14 1.333(9) . ? N4 C7 1.477(8) . ? N4 C1 1.485(8) . ? N4 C13 1.503(8) . ? N5 C25 1.339(10) . ? N5 C21 1.356(9) . ? C1 C2 1.500(9) . ? C2 C3 1.379(10) . ? C3 C4 1.397(10) . ? C4 C5 1.380(11) . ? C5 C6 1.385(10) . ? C7 C8 1.501(9) . ? C8 C9 1.385(10) . ? C9 C10 1.380(11) . ? C10 C11 1.387(11) . ? C11 C12 1.383(11) . ? C13 C14 1.522(9) . ? C14 C15 1.385(10) . ? C15 C16 1.374(13) . ? C16 C17 1.393(12) . ? C17 C18 1.370(11) . ? C21 C22 1.380(10) . ? C22 C23 1.385(13) . ? C23 C24 1.379(12) . ? C24 C25 1.381(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 La N3 115.29(17) . . ? N1 La N2 76.56(19) . . ? N3 La N2 106.63(19) . . ? N1 La N4 63.69(16) . . ? N3 La N4 63.37(18) . . ? N2 La N4 61.10(18) . . ? N1 La N5 136.16(19) . . ? N3 La N5 82.04(19) . . ? N2 La N5 139.69(19) . . ? N4 La N5 145.18(18) . . ? N1 La I3 80.93(11) . . ? N3 La I3 161.03(13) . . ? N2 La I3 86.03(12) . . ? N4 La I3 135.50(12) . . ? N5 La I3 79.25(13) . . ? N1 La I1 70.34(13) . . ? N3 La I1 74.46(13) . . ? N2 La I1 143.07(13) . . ? N4 La I1 89.20(13) . . ? N5 La I1 77.20(14) . . ? I3 La I1 104.081(15) . . ? N1 La I2 145.58(13) . . ? N3 La I2 73.68(13) . . ? N2 La I2 69.11(13) . . ? N4 La I2 96.40(12) . . ? N5 La I2 76.31(14) . . ? I3 La I2 98.766(15) . . ? I1 La I2 140.796(17) . . ? C6 N1 C2 117.1(6) . . ? C6 N1 La 119.2(4) . . ? C2 N1 La 121.2(4) . . ? C12 N2 C8 117.7(6) . . ? C12 N2 La 124.2(5) . . ? C8 N2 La 115.7(4) . . ? C18 N3 C14 118.2(6) . . ? C18 N3 La 122.5(5) . . ? C14 N3 La 119.1(5) . . ? C7 N4 C1 109.2(6) . . ? C7 N4 C13 111.2(5) . . ? C1 N4 C13 108.7(5) . . ? C7 N4 La 104.2(4) . . ? C1 N4 La 115.0(4) . . ? C13 N4 La 108.4(4) . . ? C25 N5 C21 116.9(6) . . ? C25 N5 La 128.7(5) . . ? C21 N5 La 114.0(5) . . ? N4 C1 C2 115.1(6) . . ? N1 C2 C3 122.7(6) . . ? N1 C2 C1 116.7(6) . . ? C3 C2 C1 120.3(6) . . ? C2 C3 C4 119.0(7) . . ? C5 C4 C3 119.1(6) . . ? C4 C5 C6 118.6(7) . . ? N1 C6 C5 123.4(7) . . ? N4 C7 C8 111.3(5) . . ? N2 C8 C9 121.6(6) . . ? N2 C8 C7 116.2(6) . . ? C9 C8 C7 122.0(6) . . ? C10 C9 C8 120.0(7) . . ? C9 C10 C11 118.8(7) . . ? C12 C11 C10 118.7(7) . . ? N2 C12 C11 123.2(7) . . ? N4 C13 C14 113.1(5) . . ? N3 C14 C15 122.3(7) . . ? N3 C14 C13 117.9(6) . . ? C15 C14 C13 119.7(6) . . ? C16 C15 C14 118.8(7) . . ? C15 C16 C17 119.3(7) . . ? C18 C17 C16 117.6(8) . . ? N3 C18 C17 123.8(7) . . ? N5 C21 C22 123.8(7) . . ? C21 C22 C23 118.1(7) . . ? C24 C23 C22 118.8(7) . . ? C23 C24 C25 119.6(8) . . ? N5 C25 C24 122.7(7) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 2.497 _refine_diff_density_min -2.407 _refine_diff_density_rms 0.225 #===END