Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Marinella Mazzanti' 'Christelle Gateau' 'Clement Hill' 'Lydia Karmazin' 'Jacques Pecaut' _publ_contact_author_name 'Dr Marinella Mazzanti' _publ_contact_author_address ; Dr Marinella Mazzanti Departement de Recherche Fondamentale sur la Matiere Condensee CEA-Grenoble Laboratoire de Reconnaissance Ioniq Grenoble 38054 FRANCE ; _publ_contact_author_email 'MAZZANTI@DRFMC.CENG.CEA.FR' _publ_section_title ; ; data_struc_1a _database_code_CSD 191654 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 I3 La N10' _chemical_formula_weight 962.15 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.6347(11) _cell_length_b 9.9451(6) _cell_length_c 17.9814(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.9970(10) _cell_angle_gamma 90.00 _cell_volume 2944.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(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 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 4.628 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 18324 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 28.93 _reflns_number_total 7003 _reflns_number_gt 4785 _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^)+(0.0494P)^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 7003 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.008 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 -0.051783(12) 1.48276(2) 0.750871(12) 0.01905(5) Uani 1 1 d . . . I1 I -0.067020(17) 1.35557(3) 0.902376(16) 0.03848(8) Uani 1 1 d . . . I2 I -0.172300(16) 1.73142(3) 0.696017(16) 0.03488(8) Uani 1 1 d . . . I3 I 0.124002(17) 1.12968(3) 0.539303(18) 0.03901(8) Uani 1 1 d . . . N1 N -0.04377(18) 1.2126(3) 0.71318(18) 0.0259(9) Uani 1 1 d . . . N2 N 0.11051(18) 1.4317(3) 0.83156(17) 0.0245(8) Uani 1 1 d . . . N3 N -0.0759(2) 1.4262(4) 0.59838(18) 0.0327(10) Uani 1 1 d . . . N4 N -0.19875(18) 1.3545(3) 0.66742(19) 0.0272(9) Uani 1 1 d . . . N5 N 0.05264(18) 1.6413(3) 0.70856(18) 0.0248(8) Uani 1 1 d . . . N6 N 0.02903(19) 1.6721(3) 0.86357(18) 0.0271(9) Uani 1 1 d . . . N7 N -0.1489(3) 1.3599(4) 0.4370(2) 0.0625(15) Uani 1 1 d . . . N8 N -0.3290(2) 1.2049(4) 0.5639(2) 0.0451(12) Uani 1 1 d . . . N9 N 0.1714(2) 1.8355(4) 0.7204(2) 0.0442(11) Uani 1 1 d . . . N10 N 0.1312(2) 1.8712(4) 0.9602(2) 0.0426(11) Uani 1 1 d . . . C1 C -0.0377(3) 1.1933(5) 0.6334(2) 0.0351(12) Uani 1 1 d . . . H1A H -0.0611 1.1057 0.6125 0.042 Uiso 1 1 calc R . . H1B H 0.0199 1.1911 0.6399 0.042 Uiso 1 1 calc R . . C2 C -0.0793(2) 1.2997(4) 0.5733(2) 0.0296(11) Uani 1 1 d . . . C3 C -0.1159(3) 1.2683(5) 0.4943(3) 0.0490(15) Uani 1 1 d . . . H3A H -0.1180 1.1774 0.4794 0.059 Uiso 1 1 calc R . . C4 C -0.1443(3) 1.4858(5) 0.4626(3) 0.0539(16) Uani 1 1 d . . . H4A H -0.1655 1.5549 0.4252 0.065 Uiso 1 1 calc R . . C5 C -0.1099(3) 1.5188(5) 0.5415(2) 0.0525(15) Uani 1 1 d . . . H5A H -0.1099 1.6093 0.5565 0.063 Uiso 1 1 calc R . . C6 C -0.1196(2) 1.1513(4) 0.7144(2) 0.0330(11) Uani 1 1 d . . . H6A H -0.1186 1.1523 0.7692 0.040 Uiso 1 1 calc R . . H6B H -0.1214 1.0571 0.6978 0.040 Uiso 1 1 calc R . . C7 C -0.1958(2) 1.2204(4) 0.6615(2) 0.0279(10) Uani 1 1 d . . . C8 C -0.2606(3) 1.1482(5) 0.6108(3) 0.0434(14) Uani 1 1 d . . . H8A H -0.2559 1.0542 0.6094 0.052 Uiso 1 1 calc R . . C9 C -0.3317(3) 1.3361(5) 0.5714(3) 0.0432(14) Uani 1 1 d . . . H9A H -0.3796 1.3810 0.5408 0.052 Uiso 1 1 calc R . . C10 C -0.2684(3) 1.4119(5) 0.6214(3) 0.0420(14) Uani 1 1 d . . . H10A H -0.2743 1.5057 0.6232 0.050 Uiso 1 1 calc R . . C11 C 0.1565(2) 1.4776(5) 0.7825(2) 0.0351(11) Uani 1 1 d . . . H11A H 0.1484 1.4134 0.7389 0.042 Uiso 1 1 calc R . . H11B H 0.2145 1.4783 0.8151 0.042 Uiso 1 1 calc R . . C12 C 0.1317(2) 1.6166(4) 0.7475(2) 0.0268(10) Uani 1 1 d . . . C13 C 0.1898(2) 1.7153(5) 0.7547(2) 0.0411(13) Uani 1 1 d . . . H13A H 0.2444 1.6963 0.7851 0.049 Uiso 1 1 calc R . . C14 C 0.0936(3) 1.8536(5) 0.6774(3) 0.0423(13) Uani 1 1 d . . . H14A H 0.0781 1.9345 0.6489 0.051 Uiso 1 1 calc R . . C15 C 0.0346(2) 1.7610(4) 0.6722(2) 0.0315(11) Uani 1 1 d . . . H15A H -0.0199 1.7817 0.6424 0.038 Uiso 1 1 calc R . . C16 C 0.1383(2) 1.5064(4) 0.9080(2) 0.0319(12) Uani 1 1 d . . . H16A H 0.1978 1.5090 0.9283 0.038 Uiso 1 1 calc R . . H16B H 0.1219 1.4554 0.9465 0.038 Uiso 1 1 calc R . . C17 C 0.1075(2) 1.6482(4) 0.9054(2) 0.0266(10) Uani 1 1 d . . . C18 C 0.1570(3) 1.7501(5) 0.9521(2) 0.0376(13) Uani 1 1 d . . . H18A H 0.2122 1.7304 0.9793 0.045 Uiso 1 1 calc R . . C19 C 0.0516(3) 1.8923(4) 0.9224(2) 0.0418(13) Uani 1 1 d . . . H19A H 0.0289 1.9748 0.9293 0.050 Uiso 1 1 calc R . . C20 C 0.0016(3) 1.7947(4) 0.8731(2) 0.0360(12) Uani 1 1 d . . . H20A H -0.0534 1.8154 0.8455 0.043 Uiso 1 1 calc R . . C21 C 0.0228(2) 1.1319(4) 0.7727(2) 0.0338(12) Uani 1 1 d . . . H21A H 0.0198 1.0396 0.7527 0.041 Uiso 1 1 calc R . . H21B H 0.0121 1.1283 0.8225 0.041 Uiso 1 1 calc R . . C22 C 0.1090(2) 1.1824(5) 0.7917(3) 0.0367(12) Uani 1 1 d . . . H22A H 0.1136 1.2187 0.7428 0.044 Uiso 1 1 calc R . . H22B H 0.1461 1.1056 0.8084 0.044 Uiso 1 1 calc R . . C23 C 0.1368(2) 1.2898(4) 0.8562(2) 0.0338(12) Uani 1 1 d . . . H23A H 0.1171 1.2649 0.8988 0.041 Uiso 1 1 calc R . . H23B H 0.1963 1.2882 0.8789 0.041 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 0.02239(10) 0.01405(10) 0.02012(9) 0.00057(9) 0.00691(8) -0.00009(9) I1 0.04829(15) 0.04317(18) 0.02819(13) 0.00357(12) 0.01882(11) -0.00666(14) I2 0.03525(14) 0.02428(14) 0.04029(15) -0.00105(12) 0.00769(12) 0.00744(12) I3 0.03661(14) 0.03092(16) 0.04740(16) 0.01530(13) 0.01251(12) 0.00077(13) N1 0.0321(16) 0.0203(17) 0.0232(15) 0.0024(14) 0.0074(13) 0.0032(15) N2 0.0280(16) 0.0211(17) 0.0234(15) 0.0042(14) 0.0081(13) 0.0048(14) N3 0.050(2) 0.0236(19) 0.0242(16) -0.0007(15) 0.0133(14) -0.0081(17) N4 0.0295(16) 0.0191(18) 0.0334(17) 0.0023(14) 0.0116(13) -0.0038(14) N5 0.0312(16) 0.0183(17) 0.0276(16) 0.0010(14) 0.0136(13) 0.0013(14) N6 0.0342(17) 0.0237(18) 0.0235(15) 0.0022(14) 0.0105(13) -0.0007(15) N7 0.119(4) 0.030(2) 0.0261(19) -0.0052(17) 0.011(2) -0.001(2) N8 0.044(2) 0.044(3) 0.037(2) 0.0029(19) 0.0023(17) -0.009(2) N9 0.049(2) 0.035(2) 0.058(2) -0.0019(19) 0.0305(17) -0.0151(18) N10 0.059(2) 0.027(2) 0.042(2) -0.0097(17) 0.0191(17) -0.0137(19) C1 0.042(2) 0.030(2) 0.034(2) -0.0050(19) 0.0138(18) 0.010(2) C2 0.045(2) 0.023(2) 0.0252(18) -0.0042(17) 0.0174(16) -0.0016(19) C3 0.085(3) 0.024(2) 0.031(2) -0.005(2) 0.013(2) 0.008(3) C4 0.099(4) 0.028(3) 0.029(2) 0.006(2) 0.015(2) -0.001(3) C5 0.108(4) 0.018(2) 0.031(2) 0.0011(19) 0.025(2) 0.000(3) C6 0.042(2) 0.021(2) 0.037(2) -0.0015(18) 0.0146(18) -0.0057(19) C7 0.035(2) 0.022(2) 0.0254(18) 0.0009(17) 0.0093(16) -0.0060(18) C8 0.051(3) 0.032(3) 0.042(2) -0.003(2) 0.009(2) -0.012(2) C9 0.031(2) 0.046(3) 0.041(2) 0.012(2) -0.001(2) -0.003(2) C10 0.038(2) 0.024(2) 0.054(3) 0.010(2) 0.004(2) 0.000(2) C11 0.037(2) 0.034(3) 0.041(2) 0.009(2) 0.0221(17) 0.010(2) C12 0.0318(19) 0.029(2) 0.0245(17) 0.0023(17) 0.0158(15) 0.0008(18) C13 0.029(2) 0.062(3) 0.033(2) -0.003(2) 0.0119(17) -0.009(2) C14 0.063(3) 0.029(3) 0.049(2) 0.002(2) 0.036(2) -0.005(2) C15 0.034(2) 0.029(2) 0.033(2) 0.0089(18) 0.0146(17) 0.0049(19) C16 0.029(2) 0.023(2) 0.036(2) 0.0035(18) 0.0028(18) 0.0035(18) C17 0.034(2) 0.019(2) 0.0270(19) 0.0024(16) 0.0116(16) -0.0038(18) C18 0.035(2) 0.043(3) 0.032(2) -0.009(2) 0.0091(17) -0.016(2) C19 0.079(3) 0.019(2) 0.024(2) 0.0017(18) 0.015(2) 0.002(2) C20 0.045(2) 0.028(2) 0.028(2) -0.0033(19) 0.0058(18) 0.003(2) C21 0.046(2) 0.015(2) 0.034(2) 0.0060(18) 0.0077(19) 0.0104(19) C22 0.038(2) 0.027(2) 0.040(2) 0.0035(19) 0.0081(19) 0.017(2) C23 0.036(2) 0.024(2) 0.035(2) 0.0061(19) 0.0052(18) 0.0091(19) _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 N3 2.680(3) . ? La N5 2.731(3) . ? La N2 2.753(3) . ? La N6 2.759(3) . ? La N1 2.787(3) . ? La N4 2.794(3) . ? La I1 3.1014(4) . ? La I2 3.1786(4) . ? N1 C6 1.477(5) . ? N1 C1 1.488(5) . ? N1 C21 1.506(5) . ? N2 C11 1.469(5) . ? N2 C16 1.483(5) . ? N2 C23 1.502(5) . ? N3 C2 1.332(5) . ? N3 C5 1.347(5) . ? N4 C10 1.338(5) . ? N4 C7 1.340(5) . ? N5 C12 1.339(5) . ? N5 C15 1.341(5) . ? N6 C17 1.339(5) . ? N6 C20 1.345(6) . ? N7 C4 1.327(6) . ? N7 C3 1.342(6) . ? N8 C9 1.315(6) . ? N8 C8 1.324(5) . ? N9 C14 1.323(5) . ? N9 C13 1.331(6) . ? N10 C18 1.314(6) . ? N10 C19 1.339(6) . ? C1 C2 1.503(6) . ? C2 C3 1.368(6) . ? C4 C5 1.368(6) . ? C6 C7 1.506(5) . ? C7 C8 1.380(5) . ? C9 C10 1.380(6) . ? C11 C12 1.517(6) . ? C12 C13 1.391(6) . ? C14 C15 1.368(6) . ? C16 C17 1.506(6) . ? C17 C18 1.402(6) . ? C19 C20 1.395(6) . ? C21 C22 1.519(6) . ? C22 C23 1.523(6) . ? 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 La N5 73.23(10) . . ? N3 La N2 104.74(10) . . ? N5 La N2 64.90(9) . . ? N3 La N6 138.20(11) . . ? N5 La N6 65.69(10) . . ? N2 La N6 64.71(10) . . ? N3 La N1 63.40(10) . . ? N5 La N1 113.00(10) . . ? N2 La N1 79.44(9) . . ? N6 La N1 141.13(9) . . ? N3 La N4 65.06(11) . . ? N5 La N4 134.59(9) . . ? N2 La N4 141.99(10) . . ? N6 La N4 147.30(10) . . ? N1 La N4 63.09(9) . . ? N3 La I1 141.39(8) . . ? N5 La I1 139.41(6) . . ? N2 La I1 82.11(7) . . ? N6 La I1 79.49(7) . . ? N1 La I1 81.27(7) . . ? N4 La I1 85.98(7) . . ? N3 La I2 90.14(8) . . ? N5 La I2 84.67(7) . . ? N2 La I2 139.49(7) . . ? N6 La I2 78.99(7) . . ? N1 La I2 139.57(6) . . ? N4 La I2 78.47(7) . . ? I1 La I2 109.339(11) . . ? C6 N1 C1 109.8(3) . . ? C6 N1 C21 104.5(3) . . ? C1 N1 C21 108.0(3) . . ? C6 N1 La 105.6(2) . . ? C1 N1 La 112.7(2) . . ? C21 N1 La 115.8(2) . . ? C11 N2 C16 109.4(3) . . ? C11 N2 C23 106.9(3) . . ? C16 N2 C23 103.4(3) . . ? C11 N2 La 108.6(2) . . ? C16 N2 La 109.4(2) . . ? C23 N2 La 118.8(2) . . ? C2 N3 C5 115.8(3) . . ? C2 N3 La 121.1(3) . . ? C5 N3 La 119.9(3) . . ? C10 N4 C7 115.3(3) . . ? C10 N4 La 127.3(3) . . ? C7 N4 La 116.3(2) . . ? C12 N5 C15 116.0(3) . . ? C12 N5 La 115.3(2) . . ? C15 N5 La 125.6(3) . . ? C17 N6 C20 115.8(3) . . ? C17 N6 La 116.8(3) . . ? C20 N6 La 126.7(2) . . ? C4 N7 C3 114.8(4) . . ? C9 N8 C8 114.6(4) . . ? C14 N9 C13 115.0(4) . . ? C18 N10 C19 115.5(4) . . ? N1 C1 C2 114.7(4) . . ? N3 C2 C3 121.0(4) . . ? N3 C2 C1 118.0(3) . . ? C3 C2 C1 120.9(4) . . ? N7 C3 C2 123.8(4) . . ? N7 C4 C5 122.3(4) . . ? N3 C5 C4 122.4(4) . . ? N1 C6 C7 114.2(3) . . ? N4 C7 C8 121.6(4) . . ? N4 C7 C6 117.1(3) . . ? C8 C7 C6 121.3(4) . . ? N8 C8 C7 123.3(4) . . ? N8 C9 C10 123.9(4) . . ? N4 C10 C9 121.2(4) . . ? N2 C11 C12 113.1(3) . . ? N5 C12 C13 120.9(4) . . ? N5 C12 C11 118.4(4) . . ? C13 C12 C11 120.7(4) . . ? N9 C13 C12 122.7(4) . . ? N9 C14 C15 123.5(4) . . ? N5 C15 C14 121.5(4) . . ? N2 C16 C17 116.4(3) . . ? N6 C17 C18 120.3(4) . . ? N6 C17 C16 118.1(3) . . ? C18 C17 C16 121.2(3) . . ? N10 C18 C17 124.2(4) . . ? N10 C19 C20 121.4(4) . . ? N6 C20 C19 122.6(4) . . ? N1 C21 C22 116.6(3) . . ? C21 C22 C23 115.3(4) . . ? N2 C23 C22 117.0(3) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 2.000 _refine_diff_density_min -1.910 _refine_diff_density_rms 0.208 #======END data_struc_1b _database_code_CSD 191655 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.33 H29.50 I3 La N11.17' _chemical_formula_weight 1010.04 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 Rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 33.6224(11) _cell_length_b 33.6224(11) _cell_length_c 15.2549(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14934.7(10) _cell_formula_units_Z 18 _cell_measurement_temperature 193(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 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8562 _exptl_absorpt_coefficient_mu 4.112 _exptl_absorpt_correction_type SADABS _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 24602 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.99 _reflns_number_total 6472 _reflns_number_gt 5857 _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^)+(0.0287P)^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 -0.009(13) _refine_ls_number_reflns 6472 _refine_ls_number_parameters 478 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0475 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.017 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 0.479757(4) 0.107483(4) 0.620224(10) 0.01899(3) Uani 1 1 d . . . I1 I 0.552866(6) 0.159080(7) 0.770087(14) 0.03852(5) Uani 1 1 d . . . I2 I 0.434728(6) 0.017972(6) 0.742924(13) 0.03774(5) Uani 1 1 d . . . N1 N 0.46786(7) 0.16965(7) 0.52866(16) 0.0269(6) Uani 1 1 d . . . N2 N 0.46593(6) 0.06794(7) 0.45845(14) 0.0239(5) Uani 1 1 d . . . N3 N 0.55552(7) 0.17376(7) 0.53884(16) 0.0272(6) Uani 1 1 d . . . N4 N 0.43780(7) 0.14448(7) 0.70901(17) 0.0313(6) Uani 1 1 d . . . N5 N 0.52910(7) 0.06852(7) 0.58364(16) 0.0290(6) Uani 1 1 d . . . N6 N 0.39336(7) 0.05114(7) 0.56916(15) 0.0243(5) Uani 1 1 d . . . N7 N 0.63162(8) 0.25251(8) 0.47170(19) 0.0408(7) Uani 1 1 d . . . N8 N 0.41095(9) 0.19877(9) 0.8001(2) 0.0560(9) Uani 1 1 d . . . N9 N 0.57000(8) 0.01664(8) 0.5502(2) 0.0484(7) Uani 1 1 d . . . N10 N 0.30668(8) -0.02634(8) 0.54731(18) 0.0382(7) Uani 1 1 d . . . C1 C 0.51168(9) 0.21332(8) 0.5509(2) 0.0326(8) Uani 1 1 d . . . H1A H 0.5054(13) 0.2371(13) 0.513(3) 0.082(14) Uiso 1 1 d . . . H1B H 0.5134(8) 0.2172(8) 0.6209(18) 0.018(7) Uiso 1 1 d . . . C2 C 0.55448(8) 0.21266(8) 0.52390(19) 0.0267(7) Uani 1 1 d . . . C3 C 0.59230(9) 0.25141(9) 0.4912(2) 0.0348(8) Uani 1 1 d . . . H3 H 0.5918(9) 0.2789(10) 0.4808(19) 0.031(8) Uiso 1 1 d . . . C4 C 0.63244(9) 0.21377(10) 0.4866(2) 0.0351(8) Uani 1 1 d . . . H4 H 0.6633(9) 0.2140(9) 0.4702(17) 0.025(7) Uiso 1 1 d . . . C5 C 0.59504(8) 0.17483(9) 0.5205(2) 0.0305(7) Uani 1 1 d . . . H5 H 0.5923(9) 0.1437(10) 0.529(2) 0.039(9) Uiso 1 1 d . . . C6 C 0.42930(8) 0.17374(9) 0.5678(2) 0.0323(7) Uani 1 1 d . . . H6A H 0.4331(9) 0.2035(10) 0.543(2) 0.035(8) Uiso 1 1 d . . . H6B H 0.4010(9) 0.1447(9) 0.5481(19) 0.032(8) Uiso 1 1 d . . . C7 C 0.42852(8) 0.17361(9) 0.6661(2) 0.0323(8) Uani 1 1 d . . . C8 C 0.41585(10) 0.20147(10) 0.7131(3) 0.0431(9) Uani 1 1 d . . . H8 H 0.4111(13) 0.2212(13) 0.668(3) 0.080(14) Uiso 1 1 d . . . C9 C 0.41927(11) 0.16883(12) 0.8405(2) 0.0507(10) Uani 1 1 d . . . H9 H 0.4187(13) 0.1694(13) 0.906(3) 0.082(14) Uiso 1 1 d . . . C10 C 0.43351(10) 0.14231(10) 0.7948(2) 0.0380(8) Uani 1 1 d . . . H10 H 0.4367(12) 0.1232(13) 0.826(3) 0.064(12) Uiso 1 1 d . . . C11 C 0.50772(9) 0.06743(9) 0.42974(19) 0.0299(7) Uani 1 1 d . . . H11A H 0.5275(7) 0.0987(7) 0.4098(16) 0.009(6) Uiso 1 1 d . . . H11B H 0.4983(9) 0.0462(9) 0.3808(19) 0.028(8) Uiso 1 1 d . . . C12 C 0.52962(8) 0.05422(8) 0.5023(2) 0.0268(7) Uani 1 1 d . . . C13 C 0.55063(10) 0.02819(10) 0.4883(2) 0.0410(8) Uani 1 1 d . . . H13 H 0.5479(9) 0.0207(9) 0.436(2) 0.028(8) Uiso 1 1 d . . . C14 C 0.57009(9) 0.03179(9) 0.6292(2) 0.0363(8) Uani 1 1 d . . . H14 H 0.5821(10) 0.0192(10) 0.672(2) 0.040(9) Uiso 1 1 d . . . C15 C 0.54982(9) 0.05801(9) 0.6466(2) 0.0318(7) Uani 1 1 d . . . H15 H 0.5444(14) 0.0699(13) 0.708(3) 0.092(15) Uiso 1 1 d . . . C16 C 0.42875(9) 0.01983(9) 0.4722(2) 0.0295(7) Uani 1 1 d . . . H16A H 0.4389(12) 0.0043(12) 0.519(2) 0.057(11) Uiso 1 1 d . . . H16B H 0.4186(11) -0.0041(11) 0.416(3) 0.055(11) Uiso 1 1 d . . . C17 C 0.38693(8) 0.01668(8) 0.51498(19) 0.0253(7) Uani 1 1 d . . . C18 C 0.34377(10) -0.02115(9) 0.5053(2) 0.0355(8) Uani 1 1 d . . . H18 H 0.3430(10) -0.0364(9) 0.470(2) 0.037(10) Uiso 1 1 d . . . C19 C 0.31336(9) 0.00826(10) 0.5995(2) 0.0329(8) Uani 1 1 d . . . H19 H 0.2867(11) 0.0034(11) 0.630(2) 0.048(10) Uiso 1 1 d . . . C20 C 0.35613(8) 0.04652(9) 0.61012(19) 0.0264(7) Uani 1 1 d . . . H20 H 0.3590(9) 0.0700(9) 0.6437(18) 0.024(7) Uiso 1 1 d . . . C21 C 0.46019(9) 0.16577(10) 0.4322(2) 0.0350(8) Uani 1 1 d . . . H21A H 0.4719(8) 0.1999(8) 0.4040(17) 0.013(6) Uiso 1 1 d . . . H21B H 0.4361(14) 0.1623(14) 0.418(3) 0.082(15) Uiso 1 1 d . . . C22 C 0.47856(9) 0.14055(10) 0.3779(2) 0.0308(7) Uani 1 1 d . . . H22A H 0.5104(9) 0.1509(9) 0.3863(19) 0.031(8) Uiso 1 1 d . . . H22B H 0.4736(10) 0.1480(10) 0.316(2) 0.037(9) Uiso 1 1 d . . . C23 C 0.45140(9) 0.08780(10) 0.3862(2) 0.0332(8) Uani 1 1 d . . . H23A H 0.4209(14) 0.0813(15) 0.386(3) 0.091(14) Uiso 1 1 d . . . H23B H 0.4517(9) 0.0706(9) 0.334(2) 0.033(8) Uiso 1 1 d . . . I3 I 0.452905(7) 0.310498(8) 0.56769(2) 0.05677(7) Uani 1 1 d . . . N31 N 0.53284(15) 0.26334(17) 0.8292(3) 0.1044(16) Uani 1 1 d . . . C31 C 0.5599(3) 0.3149(2) 0.6966(5) 0.134(3) Uani 1 1 d . . . H31A H 0.5914 0.3402 0.7047 0.201 Uiso 1 1 calc R . . H31B H 0.5393 0.3273 0.6874 0.201 Uiso 1 1 calc R . . H31C H 0.5587 0.2967 0.6454 0.201 Uiso 1 1 calc R . . C32 C 0.54605(17) 0.28703(15) 0.7708(3) 0.0761(14) Uani 1 1 d . . . N41 N 0.6667 0.3333 0.1473(11) 0.135(8) Uani 0.50 3 d SP . . C41 C 0.6667 0.3333 0.2187(10) 0.064(4) Uani 0.50 3 d SP . . C42 C 0.6667 0.3333 0.3167(10) 0.062(4) Uani 0.50 3 d SP . . H42 H 0.6753(19) 0.3077(19) 0.357(4) 0.039(18) Uiso 0.50 1 d P . . 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 0.02043(5) 0.01697(5) 0.02235(7) -0.00081(5) 0.00022(6) 0.01144(4) I1 0.03785(8) 0.04395(9) 0.03337(10) -0.00973(8) -0.01124(8) 0.02017(7) I2 0.04296(9) 0.03118(8) 0.03710(11) 0.01294(8) 0.00525(8) 0.01707(7) N1 0.0236(8) 0.0197(8) 0.0385(14) -0.0007(9) -0.0032(10) 0.0117(7) N2 0.0262(9) 0.0213(9) 0.0232(12) -0.0017(8) 0.0019(9) 0.0113(7) N3 0.0235(9) 0.0242(9) 0.0335(13) 0.0009(9) -0.0023(9) 0.0117(7) N4 0.0271(9) 0.0294(10) 0.0390(15) -0.0094(10) 0.0029(10) 0.0153(8) N5 0.0331(9) 0.0296(9) 0.0326(14) 0.0024(9) 0.0040(10) 0.0218(7) N6 0.0237(8) 0.0200(8) 0.0301(13) -0.0059(8) -0.0037(9) 0.0116(7) N7 0.0250(10) 0.0293(11) 0.0592(18) 0.0039(11) 0.0056(12) 0.0070(9) N8 0.0556(12) 0.0450(12) 0.078(2) -0.0185(13) 0.0043(15) 0.0333(10) N9 0.0563(11) 0.0556(11) 0.058(2) -0.0027(12) 0.0060(13) 0.0465(9) N10 0.0252(10) 0.0289(11) 0.0503(17) -0.0038(11) 0.0029(11) 0.0059(9) C1 0.0264(11) 0.0149(10) 0.057(2) -0.0029(11) -0.0039(13) 0.0110(8) C2 0.0229(10) 0.0204(10) 0.0335(16) -0.0027(11) -0.0022(11) 0.0083(9) C3 0.0329(12) 0.0203(11) 0.0481(19) 0.0036(12) 0.0014(13) 0.0111(9) C4 0.0262(11) 0.0355(13) 0.0406(18) -0.0036(13) 0.0021(12) 0.0131(10) C5 0.0249(11) 0.0302(12) 0.0342(16) -0.0009(12) -0.0027(12) 0.0121(9) C6 0.0221(10) 0.0241(10) 0.055(2) 0.0009(12) -0.0044(12) 0.0148(8) C7 0.0230(10) 0.0212(10) 0.055(2) -0.0076(12) -0.0005(12) 0.0124(8) C8 0.0376(12) 0.0330(13) 0.065(2) -0.0049(14) 0.0079(15) 0.0221(10) C9 0.0453(15) 0.0590(17) 0.045(2) -0.0242(16) 0.0021(15) 0.0239(14) C10 0.0372(13) 0.0385(14) 0.0380(19) -0.0062(13) 0.0049(13) 0.0189(11) C11 0.0331(11) 0.0323(12) 0.0245(15) 0.0016(11) 0.0114(12) 0.0166(10) C12 0.0245(10) 0.0227(10) 0.0344(16) 0.0023(10) 0.0112(11) 0.0128(8) C13 0.0490(13) 0.0451(13) 0.0410(19) -0.0045(13) 0.0112(14) 0.0326(11) C14 0.0310(11) 0.0356(12) 0.052(2) 0.0013(13) 0.0011(13) 0.0240(9) C15 0.0351(11) 0.0333(11) 0.0363(17) -0.0028(11) -0.0031(12) 0.0241(9) C16 0.0328(12) 0.0202(10) 0.0331(16) -0.0044(11) 0.0063(12) 0.0114(9) C17 0.0271(10) 0.0205(10) 0.0289(15) -0.0031(10) 0.0013(11) 0.0122(8) C18 0.0353(13) 0.0240(12) 0.0395(18) -0.0095(12) 0.0022(13) 0.0091(10) C19 0.0255(11) 0.0314(12) 0.0398(18) -0.0012(12) 0.0025(12) 0.0128(10) C20 0.0242(10) 0.0241(11) 0.0308(16) -0.0031(11) 0.0003(11) 0.0120(9) C21 0.0326(12) 0.0335(12) 0.0428(19) 0.0057(12) -0.0051(13) 0.0195(10) C22 0.0282(11) 0.0369(13) 0.0263(15) 0.0067(11) -0.0021(12) 0.0154(10) C23 0.0288(12) 0.0352(13) 0.0281(16) -0.0013(12) -0.0012(12) 0.0104(11) I3 0.04024(9) 0.04497(10) 0.0891(2) 0.00898(11) 0.01605(11) 0.02431(8) N31 0.100(3) 0.114(3) 0.105(3) 0.002(3) 0.017(3) 0.059(2) C31 0.186(6) 0.084(3) 0.124(6) -0.013(4) -0.018(5) 0.061(4) C32 0.096(3) 0.066(2) 0.072(3) -0.017(2) -0.001(3) 0.044(2) N41 0.179(11) 0.179(11) 0.046(9) 0.000 0.000 0.090(6) C41 0.066(5) 0.066(5) 0.060(10) 0.000 0.000 0.033(3) C42 0.060(5) 0.060(5) 0.065(10) 0.000 0.000 0.030(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 N5 2.637(2) . ? La N4 2.670(3) . ? La N6 2.6704(19) . ? La N1 2.705(2) . ? La N3 2.705(2) . ? La N2 2.731(2) . ? La I1 3.1645(3) . ? La I2 3.2089(2) . ? N1 C21 1.489(4) . ? N1 C6 1.495(4) . ? N1 C1 1.509(3) . ? N2 C11 1.480(4) . ? N2 C16 1.484(3) . ? N2 C23 1.492(4) . ? N3 C5 1.341(4) . ? N3 C2 1.345(4) . ? N4 C10 1.315(4) . ? N4 C7 1.338(4) . ? N5 C12 1.334(4) . ? N5 C15 1.334(4) . ? N6 C20 1.337(3) . ? N6 C17 1.350(3) . ? N7 C4 1.336(4) . ? N7 C3 1.338(4) . ? N8 C9 1.324(5) . ? N8 C8 1.335(5) . ? N9 C14 1.308(5) . ? N9 C13 1.311(5) . ? N10 C19 1.333(4) . ? N10 C18 1.333(4) . ? C1 C2 1.508(4) . ? C2 C3 1.381(3) . ? C4 C5 1.384(4) . ? C6 C7 1.499(5) . ? C7 C8 1.404(5) . ? C9 C10 1.392(5) . ? C11 C12 1.514(4) . ? C12 C13 1.389(4) . ? C14 C15 1.383(5) . ? C16 C17 1.505(4) . ? C17 C18 1.378(3) . ? C19 C20 1.378(3) . ? C21 C22 1.519(5) . ? C22 C23 1.541(4) . ? N31 C32 1.128(7) . ? C31 C32 1.393(8) . ? N41 C41 1.09(2) . ? C41 C42 1.50(2) . ? 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 N5 La N4 161.65(8) . . ? N5 La N6 108.50(7) . . ? N4 La N6 80.66(7) . . ? N5 La N1 130.35(7) . . ? N4 La N1 65.49(8) . . ? N6 La N1 82.46(6) . . ? N5 La N3 75.22(7) . . ? N4 La N3 110.39(7) . . ? N6 La N3 133.85(7) . . ? N1 La N3 64.45(7) . . ? N5 La N2 64.09(7) . . ? N4 La N2 133.19(7) . . ? N6 La N2 62.03(6) . . ? N1 La N2 81.64(7) . . ? N3 La N2 81.22(6) . . ? N5 La I1 85.18(5) . . ? N4 La I1 79.90(5) . . ? N6 La I1 150.57(5) . . ? N1 La I1 108.90(4) . . ? N3 La I1 74.13(5) . . ? N2 La I1 144.72(4) . . ? N5 La I2 77.08(5) . . ? N4 La I2 91.70(5) . . ? N6 La I2 70.68(5) . . ? N1 La I2 147.49(4) . . ? N3 La I2 148.05(5) . . ? N2 La I2 100.65(4) . . ? I1 La I2 88.032(7) . . ? C21 N1 C6 106.4(2) . . ? C21 N1 C1 110.5(2) . . ? C6 N1 C1 106.9(2) . . ? C21 N1 La 121.94(17) . . ? C6 N1 La 109.55(16) . . ? C1 N1 La 100.72(16) . . ? C11 N2 C16 108.5(2) . . ? C11 N2 C23 108.2(2) . . ? C16 N2 C23 107.9(2) . . ? C11 N2 La 109.98(15) . . ? C16 N2 La 104.38(16) . . ? C23 N2 La 117.62(18) . . ? C5 N3 C2 116.5(2) . . ? C5 N3 La 129.09(18) . . ? C2 N3 La 114.02(17) . . ? C10 N4 C7 118.0(3) . . ? C10 N4 La 123.2(2) . . ? C7 N4 La 117.6(2) . . ? C12 N5 C15 118.1(3) . . ? C12 N5 La 120.05(19) . . ? C15 N5 La 121.4(2) . . ? C20 N6 C17 116.6(2) . . ? C20 N6 La 124.70(17) . . ? C17 N6 La 115.99(16) . . ? C4 N7 C3 115.9(2) . . ? C9 N8 C8 116.6(3) . . ? C14 N9 C13 116.9(3) . . ? C19 N10 C18 115.7(2) . . ? C2 C1 N1 113.5(2) . . ? N3 C2 C3 121.3(3) . . ? N3 C2 C1 117.2(2) . . ? C3 C2 C1 121.3(3) . . ? N7 C3 C2 122.5(3) . . ? N7 C4 C5 122.3(3) . . ? N3 C5 C4 121.5(3) . . ? N1 C6 C7 114.5(2) . . ? N4 C7 C8 119.8(3) . . ? N4 C7 C6 118.8(3) . . ? C8 C7 C6 121.3(3) . . ? N8 C8 C7 122.1(3) . . ? N8 C9 C10 121.7(3) . . ? N4 C10 C9 121.7(3) . . ? N2 C11 C12 113.0(2) . . ? N5 C12 C13 118.2(3) . . ? N5 C12 C11 118.6(3) . . ? C13 C12 C11 123.2(3) . . ? N9 C13 C12 124.1(3) . . ? N9 C14 C15 121.3(3) . . ? N5 C15 C14 121.3(3) . . ? N2 C16 C17 112.7(2) . . ? N6 C17 C18 120.0(3) . . ? N6 C17 C16 117.5(2) . . ? C18 C17 C16 122.3(3) . . ? N10 C18 C17 123.6(3) . . ? N10 C19 C20 121.8(3) . . ? N6 C20 C19 122.2(3) . . ? N1 C21 C22 119.1(3) . . ? C21 C22 C23 115.2(2) . . ? N2 C23 C22 115.9(2) . . ? N31 C32 C31 176.7(6) . . ? N41 C41 C42 180.000(7) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.135 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.088 #======END data_struc_2 _database_code_CSD 191656 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 I3 La N14' _chemical_formula_weight 1112.34 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4266(16) _cell_length_b 14.839(2) _cell_length_c 22.916(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.065(3) _cell_angle_gamma 90.00 _cell_volume 3880.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(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 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 3.529 _exptl_absorpt_correction_type SADABS _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 '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 24524 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.95 _reflns_number_total 9297 _reflns_number_gt 7066 _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. We are unable to calculate the positions of the hydrogen atoms of the four acetonitrile groups due to the value of the N-C-C angle very close to 180 degrees ; _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^)+(0.0531P)^2^+2.7265P] 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 9297 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 La La 0.22934(2) 0.245368(15) 0.371515(10) 0.01764(7) Uani 1 1 d . . . I1 I 0.18219(3) 0.08287(2) 0.278926(14) 0.03700(9) Uani 1 1 d . . . N1 N 0.2238(3) 0.2928(2) 0.48660(15) 0.0217(7) Uani 1 1 d . . . N2 N 0.1259(3) 0.4068(2) 0.38565(15) 0.0222(7) Uani 1 1 d . . . N3 N 0.1606(3) 0.1117(2) 0.44528(16) 0.0249(8) Uani 1 1 d . . . N4 N 0.4015(3) 0.1798(2) 0.44191(16) 0.0261(8) Uani 1 1 d . . . N5 N 0.3763(3) 0.3862(3) 0.39094(16) 0.0258(8) Uani 1 1 d . . . N6 N -0.0075(3) 0.2513(2) 0.36570(16) 0.0235(8) Uani 1 1 d . . . N7 N 0.1402(4) -0.0144(3) 0.5353(2) 0.0379(10) Uani 1 1 d . . . N8 N 0.5718(4) 0.1029(3) 0.5188(2) 0.0419(11) Uani 1 1 d . . . N9 N 0.5127(4) 0.5376(3) 0.4190(2) 0.0432(11) Uani 1 1 d . . . N10 N -0.2511(4) 0.2639(3) 0.3428(2) 0.0404(11) Uani 1 1 d . . . C1 C 0.1303(4) 0.2366(3) 0.5122(2) 0.0262(9) Uani 1 1 d . . . H1A H 0.1315 0.2469 0.5541 0.031 Uiso 1 1 calc R . . H1B H 0.0543 0.2556 0.4957 0.031 Uiso 1 1 calc R . . C2 C 0.1451(4) 0.1379(3) 0.50115(19) 0.0249(9) Uani 1 1 d . . . C3 C 0.1362(4) 0.0745(3) 0.5450(2) 0.0323(11) Uani 1 1 d . . . H3A H 0.1271 0.0946 0.5829 0.039 Uiso 1 1 calc R . . C4 C 0.1532(4) -0.0395(3) 0.4805(2) 0.0334(11) Uani 1 1 d . . . H4A H 0.1544 -0.1006 0.4716 0.040 Uiso 1 1 calc R . . C5 C 0.1652(4) 0.0226(3) 0.4360(2) 0.0307(10) Uani 1 1 d . . . H5A H 0.1767 0.0017 0.3985 0.037 Uiso 1 1 calc R . . C6 C 0.3372(4) 0.2789(4) 0.5203(2) 0.0314(10) Uani 1 1 d . . . H6A H 0.3213 0.2669 0.5608 0.038 Uiso 1 1 calc R . . H6B H 0.3822 0.3343 0.5195 0.038 Uiso 1 1 calc R . . C7 C 0.4113(4) 0.2029(3) 0.49836(19) 0.0243(9) Uani 1 1 d . . . C8 C 0.4940(4) 0.1627(4) 0.5362(2) 0.0357(11) Uani 1 1 d . . . H8A H 0.4954 0.1782 0.5756 0.043 Uiso 1 1 calc R . . C9 C 0.5642(4) 0.0815(3) 0.4623(2) 0.0364(12) Uani 1 1 d . . . H9A H 0.6180 0.0410 0.4482 0.044 Uiso 1 1 calc R . . C10 C 0.4793(4) 0.1172(3) 0.4242(2) 0.0326(11) Uani 1 1 d . . . H10A H 0.4750 0.0981 0.3855 0.039 Uiso 1 1 calc R . . C11 C 0.2039(4) 0.4817(3) 0.3681(2) 0.0276(10) Uani 1 1 d . . . H11A H 0.1752 0.5379 0.3836 0.033 Uiso 1 1 calc R . . H11B H 0.1992 0.4865 0.3258 0.033 Uiso 1 1 calc R . . C12 C 0.3307(4) 0.4698(3) 0.3887(2) 0.0263(9) Uani 1 1 d . . . C13 C 0.4008(4) 0.5440(3) 0.4024(2) 0.0381(12) Uani 1 1 d . . . H13A H 0.3672 0.6011 0.3997 0.046 Uiso 1 1 calc R . . C14 C 0.5585(4) 0.4543(4) 0.4202(2) 0.0369(12) Uani 1 1 d . . . H14A H 0.6377 0.4469 0.4305 0.044 Uiso 1 1 calc R . . C15 C 0.4909(4) 0.3794(3) 0.4065(2) 0.0295(10) Uani 1 1 d . . . H15A H 0.5257 0.3228 0.4080 0.035 Uiso 1 1 calc R . . C16 C 0.0158(4) 0.4134(3) 0.3489(2) 0.0254(9) Uani 1 1 d . . . H16A H 0.0346 0.4220 0.3085 0.030 Uiso 1 1 calc R . . H16B H -0.0279 0.4657 0.3608 0.030 Uiso 1 1 calc R . . C17 C -0.0594(4) 0.3305(3) 0.35339(18) 0.0237(9) Uani 1 1 d . . . C18 C -0.1800(4) 0.3361(3) 0.3425(2) 0.0317(10) Uani 1 1 d . . . H18A H -0.2130 0.3924 0.3345 0.038 Uiso 1 1 calc R . . C19 C -0.1979(4) 0.1851(3) 0.3564(2) 0.0349(11) Uani 1 1 d . . . H19A H -0.2429 0.1330 0.3577 0.042 Uiso 1 1 calc R . . C20 C -0.0785(4) 0.1797(3) 0.3684(2) 0.0290(10) Uani 1 1 d . . . H20A H -0.0460 0.1241 0.3788 0.035 Uiso 1 1 calc R . . C21 C 0.1898(4) 0.3900(3) 0.49245(19) 0.0247(9) Uani 1 1 d . . . H21A H 0.2581 0.4275 0.4876 0.030 Uiso 1 1 calc R . . H21B H 0.1637 0.4002 0.5315 0.030 Uiso 1 1 calc R . . C22 C 0.0940(4) 0.4180(3) 0.44854(19) 0.0253(9) Uani 1 1 d . . . H22A H 0.0748 0.4807 0.4552 0.030 Uiso 1 1 calc R . . H22B H 0.0245 0.3825 0.4549 0.030 Uiso 1 1 calc R . . N11 N 0.2013(4) 0.3272(3) 0.26892(19) 0.0394(10) Uani 1 1 d . . . C31 C 0.2004(4) 0.3344(3) 0.2196(2) 0.0286(10) Uani 1 1 d . . . C32 C 0.2003(5) 0.3406(4) 0.1566(2) 0.0471(14) Uani 1 1 d . . . N12 N 0.4203(4) 0.2290(3) 0.31042(19) 0.0357(10) Uani 1 1 d . . . C33 C 0.4729(5) 0.2000(4) 0.2752(2) 0.0432(13) Uani 1 1 d . . . C34 C 0.5440(8) 0.1606(5) 0.2293(3) 0.085(3) Uani 1 1 d . . . I2 I 0.19813(3) 0.68537(2) 0.486786(17) 0.04147(10) Uani 1 1 d . . . I3 I 0.87862(4) 0.43882(3) 0.181590(17) 0.05008(11) Uani 1 1 d . . . N41 N 0.7260(5) 0.0781(4) 0.1453(2) 0.0581(14) Uani 1 1 d . . . C41 C 0.7973(6) 0.1204(4) 0.1683(2) 0.0449(14) Uani 1 1 d . . . C42 C 0.8884(7) 0.1758(5) 0.1965(3) 0.077(2) Uani 1 1 d . . . N42 N 0.4905(6) 0.3583(5) 0.1604(3) 0.081(2) Uani 1 1 d . . . C44 C 0.5806(6) 0.4276(5) 0.2575(3) 0.0631(18) Uani 1 1 d . . . C43 C 0.5287(6) 0.3895(5) 0.2034(3) 0.0556(16) Uani 1 1 d . . . 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 0.01749(12) 0.01842(12) 0.01698(12) -0.00110(9) 0.00075(8) 0.00023(9) I1 0.0449(2) 0.03308(18) 0.03283(18) -0.01321(13) 0.00005(14) -0.00363(14) N1 0.0174(18) 0.0254(19) 0.0223(18) -0.0005(14) 0.0003(14) -0.0031(15) N2 0.0257(19) 0.0183(17) 0.0230(18) 0.0001(14) 0.0051(15) -0.0016(15) N3 0.0238(19) 0.0232(19) 0.027(2) 0.0025(15) -0.0001(15) -0.0007(15) N4 0.0216(19) 0.028(2) 0.029(2) -0.0012(15) 0.0013(15) 0.0013(15) N5 0.0215(19) 0.0260(19) 0.031(2) -0.0032(16) 0.0067(15) -0.0045(15) N6 0.0208(18) 0.0232(18) 0.0262(19) 0.0014(15) 0.0001(14) -0.0014(15) N7 0.034(2) 0.032(2) 0.048(3) 0.019(2) 0.0031(19) 0.0024(19) N8 0.030(2) 0.048(3) 0.047(3) 0.012(2) -0.0051(19) 0.006(2) N9 0.027(2) 0.036(2) 0.067(3) -0.018(2) 0.015(2) -0.0120(19) N10 0.027(2) 0.039(3) 0.055(3) 0.002(2) -0.0043(19) 0.0004(19) C1 0.025(2) 0.029(2) 0.026(2) 0.0017(18) 0.0069(18) -0.0005(19) C2 0.017(2) 0.030(2) 0.028(2) 0.0043(18) -0.0001(17) 0.0004(18) C3 0.028(3) 0.040(3) 0.029(2) 0.006(2) 0.0018(19) -0.003(2) C4 0.024(2) 0.028(2) 0.048(3) 0.009(2) 0.000(2) 0.000(2) C5 0.029(2) 0.024(2) 0.039(3) 0.003(2) 0.003(2) 0.004(2) C6 0.028(2) 0.042(3) 0.024(2) -0.009(2) -0.0071(18) 0.003(2) C7 0.017(2) 0.026(2) 0.029(2) -0.0001(18) -0.0021(17) -0.0049(18) C8 0.031(3) 0.045(3) 0.030(3) 0.000(2) -0.007(2) 0.002(2) C9 0.027(3) 0.034(3) 0.048(3) 0.004(2) 0.001(2) 0.004(2) C10 0.028(2) 0.032(3) 0.038(3) -0.001(2) 0.002(2) 0.006(2) C11 0.028(2) 0.021(2) 0.035(3) 0.0028(18) 0.0067(19) -0.0036(18) C12 0.023(2) 0.026(2) 0.030(2) -0.0027(18) 0.0092(18) -0.0034(19) C13 0.028(3) 0.025(2) 0.062(4) -0.010(2) 0.015(2) -0.005(2) C14 0.025(3) 0.040(3) 0.046(3) -0.009(2) 0.006(2) -0.009(2) C15 0.021(2) 0.031(2) 0.036(3) -0.002(2) 0.0054(19) -0.0033(19) C16 0.024(2) 0.023(2) 0.029(2) 0.0046(18) 0.0017(18) 0.0021(18) C17 0.022(2) 0.028(2) 0.021(2) 0.0011(17) 0.0012(17) -0.0022(18) C18 0.022(2) 0.032(3) 0.041(3) 0.003(2) -0.002(2) 0.001(2) C19 0.029(3) 0.031(3) 0.044(3) 0.004(2) -0.003(2) -0.008(2) C20 0.029(2) 0.026(2) 0.032(3) 0.0038(19) -0.0019(19) -0.0038(19) C21 0.027(2) 0.025(2) 0.023(2) -0.0071(17) 0.0045(17) -0.0022(18) C22 0.030(2) 0.021(2) 0.026(2) -0.0032(17) 0.0093(18) 0.0018(18) N11 0.052(3) 0.037(2) 0.030(2) 0.0034(18) 0.007(2) 0.007(2) C31 0.033(3) 0.025(2) 0.028(3) 0.0027(18) 0.0001(19) 0.000(2) C32 0.054(4) 0.066(4) 0.021(3) 0.002(2) -0.002(2) -0.001(3) N12 0.028(2) 0.045(3) 0.035(2) -0.0052(19) 0.0065(18) -0.0020(19) C33 0.041(3) 0.049(3) 0.040(3) 0.000(3) 0.010(3) 0.008(3) C34 0.109(7) 0.076(5) 0.074(5) -0.002(4) 0.053(5) 0.038(5) I2 0.0396(2) 0.03441(19) 0.0520(2) -0.00425(15) 0.01753(16) 0.00051(14) I3 0.0519(2) 0.0543(2) 0.0441(2) 0.00745(17) 0.00361(17) 0.00831(18) N41 0.058(4) 0.065(4) 0.053(3) -0.001(3) 0.021(3) -0.006(3) C41 0.055(4) 0.045(3) 0.035(3) 0.004(2) 0.008(3) 0.015(3) C42 0.094(6) 0.063(5) 0.071(5) -0.015(4) -0.031(4) 0.008(4) N42 0.068(4) 0.118(6) 0.057(4) -0.003(4) 0.003(3) -0.023(4) C44 0.068(5) 0.072(5) 0.047(4) -0.005(3) -0.007(3) 0.013(4) C43 0.050(4) 0.066(4) 0.051(4) 0.006(3) 0.007(3) -0.004(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 N11 2.650(4) . ? La N4 2.661(4) . ? La N12 2.666(4) . ? La N2 2.698(3) . ? La N6 2.703(4) . ? La N5 2.704(4) . ? La N1 2.734(3) . ? La N3 2.748(4) . ? La I1 3.2379(5) . ? N1 C6 1.488(6) . ? N1 C1 1.501(5) . ? N1 C21 1.502(6) . ? N2 C16 1.479(6) . ? N2 C11 1.495(5) . ? N2 C22 1.514(5) . ? N3 C5 1.341(6) . ? N3 C2 1.358(6) . ? N4 C7 1.337(6) . ? N4 C10 1.363(6) . ? N5 C15 1.342(6) . ? N5 C12 1.344(6) . ? N6 C20 1.340(6) . ? N6 C17 1.341(5) . ? N7 C4 1.327(7) . ? N7 C3 1.339(6) . ? N8 C9 1.331(7) . ? N8 C8 1.333(7) . ? N9 C13 1.318(7) . ? N9 C14 1.342(7) . ? N10 C18 1.344(6) . ? N10 C19 1.347(6) . ? C1 C2 1.497(6) . ? C2 C3 1.383(6) . ? C4 C5 1.386(7) . ? C6 C7 1.513(6) . ? C7 C8 1.383(6) . ? C9 C10 1.376(7) . ? C11 C12 1.511(6) . ? C12 C13 1.388(6) . ? C14 C15 1.380(7) . ? C16 C17 1.508(6) . ? C17 C18 1.389(6) . ? C19 C20 1.380(7) . ? C21 C22 1.505(6) . ? N11 C31 1.134(6) . ? C31 C32 1.446(7) . ? N12 C33 1.118(6) . ? C33 C34 1.482(8) . ? N41 C41 1.135(8) . ? C41 C42 1.452(10) . ? N42 C43 1.152(8) . ? C44 C43 1.460(9) . ? 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 N11 La N4 139.10(13) . . ? N11 La N12 68.87(14) . . ? N4 La N12 71.68(12) . . ? N11 La N2 70.53(12) . . ? N4 La N2 124.49(11) . . ? N12 La N2 121.36(12) . . ? N11 La N6 82.42(13) . . ? N4 La N6 138.36(11) . . ? N12 La N6 145.31(12) . . ? N2 La N6 62.18(11) . . ? N11 La N5 80.58(13) . . ? N4 La N5 75.53(12) . . ? N12 La N5 68.80(12) . . ? N2 La N5 64.30(11) . . ? N6 La N5 126.47(11) . . ? N11 La N1 136.87(12) . . ? N4 La N1 64.13(11) . . ? N12 La N1 126.30(12) . . ? N2 La N1 67.83(11) . . ? N6 La N1 87.97(10) . . ? N5 La N1 71.84(11) . . ? N11 La N3 148.37(13) . . ? N4 La N3 65.76(11) . . ? N12 La N3 121.74(12) . . ? N2 La N3 115.17(11) . . ? N6 La N3 74.66(11) . . ? N5 La N3 130.72(11) . . ? N1 La N3 64.55(11) . . ? N11 La I1 75.64(10) . . ? N4 La I1 102.52(8) . . ? N12 La I1 72.54(9) . . ? N2 La I1 132.93(8) . . ? N6 La I1 82.00(8) . . ? N5 La I1 139.81(8) . . ? N1 La I1 144.32(8) . . ? N3 La I1 79.78(8) . . ? C6 N1 C1 109.8(4) . . ? C6 N1 C21 108.0(3) . . ? C1 N1 C21 107.8(3) . . ? C6 N1 La 113.7(3) . . ? C1 N1 La 106.7(2) . . ? C21 N1 La 110.7(2) . . ? C16 N2 C11 107.3(3) . . ? C16 N2 C22 107.1(3) . . ? C11 N2 C22 110.6(3) . . ? C16 N2 La 110.8(2) . . ? C11 N2 La 110.9(2) . . ? C22 N2 La 109.9(2) . . ? C5 N3 C2 116.1(4) . . ? C5 N3 La 126.8(3) . . ? C2 N3 La 115.4(3) . . ? C7 N4 C10 116.1(4) . . ? C7 N4 La 121.0(3) . . ? C10 N4 La 122.8(3) . . ? C15 N5 C12 116.7(4) . . ? C15 N5 La 125.0(3) . . ? C12 N5 La 118.1(3) . . ? C20 N6 C17 116.3(4) . . ? C20 N6 La 125.4(3) . . ? C17 N6 La 118.0(3) . . ? C4 N7 C3 116.0(4) . . ? C9 N8 C8 116.1(4) . . ? C13 N9 C14 116.3(4) . . ? C18 N10 C19 115.3(4) . . ? C2 C1 N1 112.8(4) . . ? N3 C2 C3 120.5(4) . . ? N3 C2 C1 117.5(4) . . ? C3 C2 C1 121.9(4) . . ? N7 C3 C2 123.1(5) . . ? N7 C4 C5 122.1(5) . . ? N3 C5 C4 122.2(5) . . ? N1 C6 C7 114.7(4) . . ? N4 C7 C8 121.1(4) . . ? N4 C7 C6 119.6(4) . . ? C8 C7 C6 119.2(4) . . ? N8 C8 C7 122.9(5) . . ? N8 C9 C10 122.2(5) . . ? N4 C10 C9 121.6(5) . . ? N2 C11 C12 113.8(4) . . ? N5 C12 C13 120.4(4) . . ? N5 C12 C11 118.9(4) . . ? C13 C12 C11 120.6(4) . . ? N9 C13 C12 123.2(5) . . ? N9 C14 C15 121.6(5) . . ? N5 C15 C14 121.7(5) . . ? N2 C16 C17 112.1(3) . . ? N6 C17 C18 120.9(4) . . ? N6 C17 C16 118.9(4) . . ? C18 C17 C16 120.2(4) . . ? N10 C18 C17 123.0(4) . . ? N10 C19 C20 121.7(4) . . ? N6 C20 C19 122.7(4) . . ? N1 C21 C22 112.8(3) . . ? C21 C22 N2 113.8(3) . . ? C31 N11 La 157.1(4) . . ? N11 C31 C32 178.2(5) . . ? C33 N12 La 154.3(4) . . ? N12 C33 C34 178.9(7) . . ? N41 C41 C42 178.7(7) . . ? N42 C43 C44 178.2(8) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 2.061 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.137 #======END