Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Harald Krautscheid' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; 'Christine Lode' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; 'Frieder Vielsack' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author 'Dr. Harald Krautscheid' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author_email 'harald@achibm6.chemie.uni-karlsruhe.de' _publ_contact_author_fax 'Int + 721 661921' _publ_contact_author_phone 'Int + 721 608 8097' ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Synthesis and crystal structures of iodoplumbate chains, ribbons and rods with new structural types ; data_vbr2 _database_code_CSD 153703 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H56 I8 P2 Pb3' _chemical_formula_weight 2427.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.334(2) _cell_length_b 13.559(3) _cell_length_c 14.286(4) _cell_angle_alpha 78.06(2) _cell_angle_beta 71.54(2) _cell_angle_gamma 73.02(2) _cell_volume 1627.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.478 _exptl_crystal_density_method ? _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 11.618 _exptl_absorpt_correction_type 'empirical, psi-scans' _exptl_absorpt_correction_T_min 0.1062 _exptl_absorpt_correction_T_max 0.1393 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'omega-scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '+/- 0.8 %' _diffrn_reflns_number 5644 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5257 _reflns_number_observed 4490 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI IV software' _computing_cell_refinement 'STOE STADI IV software' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0378P)^2^+3.3948P] 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 'idealized positions' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_number_reflns 5255 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_obs 0.0255 _refine_ls_wR_factor_all 0.0712 _refine_ls_wR_factor_obs 0.0655 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pb1 Pb 0.5000 0.5000 0.5000 0.04061(11) Uani 1 d S . Pb2 Pb 0.02048(3) 0.61064(2) 0.58959(2) 0.03923(9) Uani 1 d . . I1 I 0.27485(6) 0.49996(3) 0.36858(3) 0.04622(13) Uani 1 d . . I2 I 0.28204(6) 0.73393(3) 0.51987(4) 0.05242(14) Uani 1 d . . I3 I 0.22520(7) 0.43219(4) 0.68583(4) 0.0638(2) Uani 1 d . . I4 I -0.12352(6) 0.70785(4) 0.77460(4) 0.05045(14) Uani 1 d . . P1 P 0.3544(2) 0.86549(12) 0.79339(12) 0.0356(4) Uani 1 d . . C1 C 0.4204(8) 0.7253(5) 0.7930(5) 0.0400(15) Uani 1 d . . H1 H 0.3822(8) 0.7049(5) 0.7444(5) 0.048 Uiso 1 calc R . H2 H 0.5357(8) 0.7052(5) 0.7718(5) 0.048 Uiso 1 calc R . C2 C 0.3630(8) 0.6679(5) 0.8944(5) 0.044(2) Uani 1 d . . C3 C 0.4376(9) 0.6524(5) 0.9684(5) 0.046(2) Uani 1 d . . H3 H 0.5290(9) 0.6765(5) 0.9547(5) 0.055 Uiso 1 calc R . C4 C 0.3812(10) 0.6029(5) 1.0605(5) 0.056(2) Uani 1 d . . H4 H 0.4329(10) 0.5939(5) 1.1104(5) 0.067 Uiso 1 calc R . C5 C 0.2520(11) 0.5663(6) 1.0820(7) 0.065(2) Uani 1 d . . H5 H 0.2134(11) 0.5327(6) 1.1467(7) 0.078 Uiso 1 calc R . C6 C 0.1777(11) 0.5778(7) 1.0107(7) 0.070(2) Uani 1 d . . H6 H 0.0887(11) 0.5508(7) 1.0254(7) 0.084 Uiso 1 calc R . C7 C 0.2324(10) 0.6291(6) 0.9164(7) 0.062(2) Uani 1 d . . H7 H 0.1801(10) 0.6375(6) 0.8669(7) 0.075 Uiso 1 calc R . C8 C 0.1466(8) 0.8958(5) 0.8562(5) 0.047(2) Uani 1 d . . H8 H 0.1045(8) 0.8384(5) 0.8515(5) 0.057 Uiso 1 calc R . H9 H 0.1340(8) 0.8963(5) 0.9275(5) 0.057 Uiso 1 calc R . C9 C 0.0478(7) 0.9966(5) 0.8191(5) 0.0387(14) Uani 1 d . . C10 C 0.0348(9) 1.0902(6) 0.8504(6) 0.057(2) Uani 1 d . . H10 H 0.0952(9) 1.0924(6) 0.8920(6) 0.069 Uiso 1 calc R . C11 C -0.0664(9) 1.1804(6) 0.8209(7) 0.066(2) Uani 1 d . . H11 H -0.0742(9) 1.2442(6) 0.8420(7) 0.079 Uiso 1 calc R . C12 C -0.1553(9) 1.1776(6) 0.7614(6) 0.060(2) Uani 1 d . . H12 H -0.2249(9) 1.2395(6) 0.7419(6) 0.073 Uiso 1 calc R . C13 C -0.1439(8) 1.0860(6) 0.7301(5) 0.051(2) Uani 1 d . . H13 H -0.2064(8) 1.0843(6) 0.6896(5) 0.061 Uiso 1 calc R . C14 C -0.0411(8) 0.9955(6) 0.7576(5) 0.043(2) Uani 1 d . . H14 H -0.0315(8) 0.9326(6) 0.7342(5) 0.052 Uiso 1 calc R . C15 C 0.4641(8) 0.9026(5) 0.8582(5) 0.045(2) Uani 1 d . . H15 H 0.4697(8) 0.8517(5) 0.9183(5) 0.054 Uiso 1 calc R . H16 H 0.5718(8) 0.8968(5) 0.8148(5) 0.054 Uiso 1 calc R . C16 C 0.4034(7) 1.0099(5) 0.8897(5) 0.0361(14) Uani 1 d . . C17 C 0.3140(8) 1.0232(5) 0.9871(5) 0.0411(15) Uani 1 d . . H17 H 0.2902(8) 0.9651(5) 1.0334(5) 0.049 Uiso 1 calc R . C18 C 0.2602(8) 1.1223(6) 1.0156(5) 0.049(2) Uani 1 d . . H18 H 0.1986(8) 1.1314(6) 1.0818(5) 0.059 Uiso 1 calc R . C19 C 0.2940(9) 1.2065(6) 0.9507(6) 0.055(2) Uani 1 d . . H19 H 0.2546(9) 1.2738(6) 0.9713(6) 0.066 Uiso 1 calc R . C20 C 0.3860(10) 1.1939(6) 0.8542(6) 0.057(2) Uani 1 d . . H20 H 0.4121(10) 1.2521(6) 0.8089(6) 0.068 Uiso 1 calc R . C21 C 0.4391(9) 1.0954(6) 0.8251(5) 0.051(2) Uani 1 d . . H21 H 0.5016(9) 1.0866(6) 0.7591(5) 0.061 Uiso 1 calc R . C22 C 0.3840(8) 0.9303(5) 0.6669(5) 0.0406(15) Uani 1 d . . H22 H 0.3172(8) 0.9115(5) 0.6352(5) 0.049 Uiso 1 calc R . H23 H 0.3491(8) 1.0064(5) 0.6690(5) 0.049 Uiso 1 calc R . C23 C 0.5498(8) 0.9051(5) 0.6025(4) 0.0378(14) Uani 1 d . . C24 C 0.6441(8) 0.9739(5) 0.5833(5) 0.043(2) Uani 1 d . . H24 H 0.6050(8) 1.0370(5) 0.6121(5) 0.052 Uiso 1 calc R . C25 C 0.7937(9) 0.9505(6) 0.5226(5) 0.050(2) Uani 1 d . . H25 H 0.8579(9) 0.9972(6) 0.5112(5) 0.060 Uiso 1 calc R . C26 C 0.8519(9) 0.8614(6) 0.4785(5) 0.052(2) Uani 1 d . . H26 H 0.9560(9) 0.8457(6) 0.4375(5) 0.062 Uiso 1 calc R . C27 C 0.7564(8) 0.7935(6) 0.4946(5) 0.049(2) Uani 1 d . . H27 H 0.7936(8) 0.7330(6) 0.4618(5) 0.059 Uiso 1 calc R . C28 C 0.6103(8) 0.8144(5) 0.5571(5) 0.044(2) Uani 1 d . . H28 H 0.5480(8) 0.7662(5) 0.5703(5) 0.053 Uiso 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 Pb1 0.0359(2) 0.0366(2) 0.0521(2) -0.01092(15) -0.0183(2) -0.00249(14) Pb2 0.0362(2) 0.03593(14) 0.04732(15) -0.01313(10) -0.01297(11) -0.00432(10) I1 0.0531(3) 0.0459(2) 0.0470(2) -0.0095(2) -0.0182(2) -0.0157(2) I2 0.0440(3) 0.0353(2) 0.0869(3) -0.0101(2) -0.0296(2) -0.0086(2) I3 0.0642(4) 0.0515(3) 0.0566(3) 0.0033(2) -0.0147(2) 0.0052(2) I4 0.0433(3) 0.0525(3) 0.0573(3) -0.0285(2) -0.0122(2) -0.0011(2) P1 0.0315(9) 0.0317(8) 0.0423(8) -0.0085(6) -0.0139(7) 0.0009(6) C1 0.038(4) 0.034(3) 0.044(3) -0.015(3) -0.009(3) 0.002(3) C2 0.043(4) 0.031(3) 0.052(4) -0.009(3) -0.015(3) 0.005(3) C3 0.047(4) 0.035(3) 0.054(4) -0.010(3) -0.015(3) -0.004(3) C4 0.072(6) 0.040(4) 0.050(4) -0.008(3) -0.022(4) 0.002(4) C5 0.075(6) 0.041(4) 0.065(5) -0.007(4) -0.008(4) -0.006(4) C6 0.062(6) 0.054(5) 0.094(7) -0.011(5) -0.015(5) -0.021(4) C7 0.057(5) 0.052(5) 0.088(6) -0.005(4) -0.036(5) -0.015(4) C8 0.039(4) 0.044(4) 0.048(4) 0.000(3) -0.008(3) -0.002(3) C9 0.025(3) 0.043(4) 0.043(3) -0.008(3) -0.006(3) -0.003(3) C10 0.041(5) 0.053(4) 0.079(5) -0.031(4) -0.018(4) 0.004(3) C11 0.046(5) 0.050(5) 0.096(6) -0.031(4) -0.011(4) 0.003(4) C12 0.037(5) 0.055(5) 0.072(5) 0.000(4) -0.009(4) 0.003(3) C13 0.035(4) 0.067(5) 0.045(4) 0.006(3) -0.014(3) -0.010(3) C14 0.036(4) 0.051(4) 0.043(3) -0.011(3) -0.003(3) -0.016(3) C15 0.045(4) 0.039(4) 0.053(4) -0.011(3) -0.024(3) 0.001(3) C16 0.027(3) 0.041(3) 0.043(3) -0.014(3) -0.013(3) -0.002(3) C17 0.043(4) 0.047(4) 0.039(3) -0.007(3) -0.015(3) -0.015(3) C18 0.036(4) 0.063(5) 0.055(4) -0.029(4) -0.010(3) -0.011(3) C19 0.053(5) 0.048(4) 0.067(5) -0.028(4) -0.021(4) 0.005(3) C20 0.066(5) 0.045(4) 0.064(5) -0.004(3) -0.028(4) -0.012(4) C21 0.053(5) 0.058(4) 0.042(4) -0.011(3) -0.008(3) -0.017(4) C22 0.040(4) 0.037(3) 0.043(3) -0.004(3) -0.016(3) -0.001(3) C23 0.037(4) 0.038(3) 0.037(3) -0.004(3) -0.015(3) -0.002(3) C24 0.053(5) 0.042(4) 0.039(3) -0.002(3) -0.018(3) -0.013(3) C25 0.043(4) 0.060(5) 0.047(4) 0.002(3) -0.009(3) -0.022(3) C26 0.039(4) 0.058(4) 0.046(4) 0.000(3) -0.009(3) -0.002(3) C27 0.043(4) 0.048(4) 0.048(4) -0.015(3) -0.013(3) 0.006(3) C28 0.040(4) 0.041(4) 0.055(4) -0.012(3) -0.021(3) -0.005(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 Pb1 I1 3.2312(8) 2_666 ? Pb1 I1 3.2313(8) . ? Pb1 I2 3.2432(10) . ? Pb1 I2 3.2432(10) 2_666 ? Pb1 I3 3.2446(11) 2_666 ? Pb1 I3 3.2447(11) . ? Pb1 Pb2 4.1432(11) 2_666 ? Pb1 Pb2 4.1432(12) . ? Pb2 I4 2.9474(10) . ? Pb2 I3 2.9971(10) . ? Pb2 I2 3.1468(9) . ? Pb2 I1 3.3475(9) 2_566 ? Pb2 C27 3.350(7) 1_455 ? Pb2 C26 3.575(7) 1_455 ? Pb2 I1 3.6041(12) . ? I1 Pb2 3.3475(9) 2_566 ? P1 C15 1.804(7) . ? P1 C22 1.812(6) . ? P1 C1 1.820(6) . ? P1 C8 1.822(7) . ? C1 C2 1.509(9) . ? C2 C7 1.388(11) . ? C2 C3 1.391(10) . ? C3 C4 1.364(10) . ? C4 C5 1.359(12) . ? C5 C6 1.364(13) . ? C6 C7 1.395(12) . ? C8 C9 1.508(9) . ? C9 C10 1.391(10) . ? C9 C14 1.391(9) . ? C10 C11 1.389(11) . ? C11 C12 1.376(12) . ? C12 C13 1.370(11) . ? C13 C14 1.390(10) . ? C15 C16 1.505(8) . ? C16 C21 1.376(10) . ? C16 C17 1.395(9) . ? C17 C18 1.388(9) . ? C18 C19 1.360(11) . ? C19 C20 1.389(11) . ? C20 C21 1.384(10) . ? C22 C23 1.509(9) . ? C23 C24 1.392(9) . ? C23 C28 1.394(9) . ? C24 C25 1.375(10) . ? C25 C26 1.366(10) . ? C26 C27 1.399(11) . ? C26 Pb2 3.574(7) 1_655 ? C27 C28 1.359(10) . ? C27 Pb2 3.350(7) 1_655 ? 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 I1 Pb1 I1 180.0 2_666 . ? I1 Pb1 I2 98.69(2) 2_666 . ? I1 Pb1 I2 81.31(2) . . ? I1 Pb1 I2 81.31(2) 2_666 2_666 ? I1 Pb1 I2 98.69(2) . 2_666 ? I2 Pb1 I2 180.0 . 2_666 ? I1 Pb1 I3 84.05(2) 2_666 2_666 ? I1 Pb1 I3 95.95(2) . 2_666 ? I2 Pb1 I3 95.31(3) . 2_666 ? I2 Pb1 I3 84.69(3) 2_666 2_666 ? I1 Pb1 I3 95.95(2) 2_666 . ? I1 Pb1 I3 84.05(2) . . ? I2 Pb1 I3 84.69(3) . . ? I2 Pb1 I3 95.31(3) 2_666 . ? I3 Pb1 I3 180.000(2) 2_666 . ? I1 Pb1 Pb2 56.91(2) 2_666 2_666 ? I1 Pb1 Pb2 123.09(2) . 2_666 ? I2 Pb1 Pb2 131.43(2) . 2_666 ? I2 Pb1 Pb2 48.57(2) 2_666 2_666 ? I3 Pb1 Pb2 45.90(2) 2_666 2_666 ? I3 Pb1 Pb2 134.10(2) . 2_666 ? I1 Pb1 Pb2 123.09(2) 2_666 . ? I1 Pb1 Pb2 56.91(2) . . ? I2 Pb1 Pb2 48.57(2) . . ? I2 Pb1 Pb2 131.43(2) 2_666 . ? I3 Pb1 Pb2 134.10(2) 2_666 . ? I3 Pb1 Pb2 45.90(2) . . ? Pb2 Pb1 Pb2 180.0 2_666 . ? I4 Pb2 I3 92.41(3) . . ? I4 Pb2 I2 91.96(2) . . ? I3 Pb2 I2 90.65(3) . . ? I4 Pb2 I1 92.22(2) . 2_566 ? I3 Pb2 I1 97.28(2) . 2_566 ? I2 Pb2 I1 170.87(2) . 2_566 ? I4 Pb2 C27 86.68(12) . 1_455 ? I3 Pb2 C27 172.74(14) . 1_455 ? I2 Pb2 C27 96.58(14) . 1_455 ? I1 Pb2 C27 75.57(14) 2_566 1_455 ? I4 Pb2 C26 83.20(12) . 1_455 ? I3 Pb2 C26 163.82(13) . 1_455 ? I2 Pb2 C26 74.01(13) . 1_455 ? I1 Pb2 C26 98.45(13) 2_566 1_455 ? C27 Pb2 C26 23.0(2) 1_455 1_455 ? I4 Pb2 I1 167.28(2) . . ? I3 Pb2 I1 81.54(3) . . ? I2 Pb2 I1 77.01(2) . . ? I1 Pb2 I1 99.61(2) 2_566 . ? C27 Pb2 I1 100.70(12) 1_455 . ? C26 Pb2 I1 99.52(12) 1_455 . ? I4 Pb2 Pb1 119.12(2) . . ? I3 Pb2 Pb1 51.02(2) . . ? I2 Pb2 Pb1 50.60(2) . . ? I1 Pb2 Pb1 132.84(2) 2_566 . ? C27 Pb2 Pb1 135.22(13) 1_455 . ? C26 Pb2 Pb1 118.20(12) 1_455 . ? I1 Pb2 Pb1 48.69(2) . . ? Pb1 I1 Pb2 133.29(2) . 2_566 ? Pb1 I1 Pb2 74.40(2) . . ? Pb2 I1 Pb2 80.39(2) 2_566 . ? Pb2 I2 Pb1 80.83(2) . . ? Pb2 I3 Pb1 83.08(3) . . ? C15 P1 C22 110.9(3) . . ? C15 P1 C1 107.6(3) . . ? C22 P1 C1 110.0(3) . . ? C15 P1 C8 111.7(3) . . ? C22 P1 C8 108.8(3) . . ? C1 P1 C8 107.6(3) . . ? C2 C1 P1 111.6(4) . . ? C7 C2 C3 118.0(7) . . ? C7 C2 C1 120.3(7) . . ? C3 C2 C1 121.7(7) . . ? C4 C3 C2 120.8(7) . . ? C5 C4 C3 120.9(8) . . ? C4 C5 C6 120.1(8) . . ? C5 C6 C7 119.9(8) . . ? C2 C7 C6 120.2(8) . . ? C9 C8 P1 117.3(5) . . ? C10 C9 C14 118.9(6) . . ? C10 C9 C8 121.5(7) . . ? C14 C9 C8 119.5(6) . . ? C11 C10 C9 120.1(8) . . ? C12 C11 C10 120.3(8) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 120.1(7) . . ? C13 C14 C9 120.4(7) . . ? C16 C15 P1 116.8(5) . . ? C21 C16 C17 118.8(6) . . ? C21 C16 C15 121.3(6) . . ? C17 C16 C15 119.8(6) . . ? C18 C17 C16 119.3(6) . . ? C19 C18 C17 121.3(7) . . ? C18 C19 C20 119.9(7) . . ? C21 C20 C19 119.1(7) . . ? C16 C21 C20 121.5(7) . . ? C23 C22 P1 115.0(4) . . ? C24 C23 C28 118.2(6) . . ? C24 C23 C22 120.9(6) . . ? C28 C23 C22 120.7(6) . . ? C25 C24 C23 120.0(6) . . ? C26 C25 C24 121.3(7) . . ? C25 C26 C27 119.2(7) . . ? C25 C26 Pb2 126.0(5) . 1_655 ? C27 C26 Pb2 69.4(4) . 1_655 ? C28 C27 C26 119.8(7) . . ? C28 C27 Pb2 115.0(5) . 1_655 ? C26 C27 Pb2 87.5(4) . 1_655 ? C27 C28 C23 121.4(7) . . ? _refine_diff_density_max 1.245 _refine_diff_density_min -.843 _refine_diff_density_rms .123 #===END data_385n1 _database_code_CSD 153704 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 I6 N2 Pb2' _chemical_formula_weight 1378.16 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' 'Pb' 'Pb' -3.3944 10.1111 '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/c' #(No. 13) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.676(2) _cell_length_b 9.9403(9) _cell_length_c 22.984(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.029(18) _cell_angle_gamma 90.00 _cell_volume 2851.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 18.287 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3225 _exptl_absorpt_correction_T_max 0.6100 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23926 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4466 _reflns_number_gt 3627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _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^)+(0.0310P)^2^+129.1562P] 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 'idealized positions' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00003(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4466 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 Pb1 Pb 0.0000 0.24285(12) 0.2500 0.0444(3) Uani 1 2 d S . . Pb2 Pb 0.21363(6) 0.25411(8) 0.13620(3) 0.0411(2) Uani 1 1 d . . . Pb3 Pb 0.5000 0.23018(11) 0.2500 0.0406(3) Uani 1 2 d S . . I1 I 0.26502(11) 0.22486(16) 0.29486(6) 0.0505(4) Uani 1 1 d . . . I2 I 0.03261(12) 0.02865(14) 0.15135(6) 0.0490(4) Uani 1 1 d . . . I3 I 0.05283(12) 0.48173(14) 0.16349(6) 0.0489(4) Uani 1 1 d . . . I4 I 0.41177(12) 0.45950(14) 0.15691(6) 0.0497(4) Uani 1 1 d . . . I5 I 0.39914(12) 0.01537(15) 0.15060(7) 0.0515(4) Uani 1 1 d . . . I6 I 0.15559(13) 0.29192(17) 0.00458(6) 0.0553(4) Uani 1 1 d . . . N1 N 0.2047(12) 0.2337(15) 0.5052(7) 0.040(4) Uani 1 1 d . . . N2 N 0.7260(13) 0.2568(15) 0.6871(8) 0.041(4) Uani 1 1 d . . . C1 C 0.3116(19) 0.196(2) 0.4932(11) 0.057(6) Uani 1 1 d . . . H1A H 0.3020 0.1532 0.4547 0.068 Uiso 1 1 calc R . . H1B H 0.3415 0.1290 0.5221 0.068 Uiso 1 1 calc R . . C2 C 0.3925(17) 0.307(3) 0.4940(10) 0.058(6) Uani 1 1 d . . . H2A H 0.4041 0.3500 0.5323 0.070 Uiso 1 1 calc R . . H2B H 0.3651 0.3734 0.4645 0.070 Uiso 1 1 calc R . . C3 C 0.5015(17) 0.251(3) 0.4811(11) 0.062(7) Uani 1 1 d . . . H3A H 0.4872 0.1905 0.4475 0.074 Uiso 1 1 calc R . . H3B H 0.5437 0.3253 0.4704 0.074 Uiso 1 1 calc R . . C4 C 0.5647(18) 0.179(3) 0.5311(9) 0.054(6) Uani 1 1 d . . . H4A H 0.6289 0.1444 0.5188 0.065 Uiso 1 1 calc R . . H4B H 0.5234 0.1016 0.5403 0.065 Uiso 1 1 calc R . . C5 C 0.5979(17) 0.259(2) 0.5874(10) 0.052(5) Uani 1 1 d . . . H5A H 0.5364 0.2724 0.6067 0.062 Uiso 1 1 calc R . . H5B H 0.6232 0.3472 0.5777 0.062 Uiso 1 1 calc R . . C6 C 0.6862(19) 0.187(2) 0.6294(10) 0.053(6) Uani 1 1 d . . . H6A H 0.6600 0.0988 0.6379 0.064 Uiso 1 1 calc R . . H6B H 0.7465 0.1738 0.6092 0.064 Uiso 1 1 calc R . . C7 C 0.200(2) 0.295(3) 0.5605(10) 0.067(7) Uani 1 1 d . . . H7A H 0.1271 0.3146 0.5633 0.100 Uiso 1 1 calc R . . H7B H 0.2407 0.3776 0.5637 0.100 Uiso 1 1 calc R . . H7C H 0.2303 0.2356 0.5919 0.100 Uiso 1 1 calc R . . C8 C 0.1498(18) 0.312(2) 0.4531(11) 0.059(6) Uani 1 1 d . . . H8A H 0.1556 0.2651 0.4174 0.088 Uiso 1 1 calc R . . H8B H 0.1831 0.3992 0.4527 0.088 Uiso 1 1 calc R . . H8C H 0.0756 0.3236 0.4558 0.088 Uiso 1 1 calc R . . C9 C 0.145(2) 0.100(3) 0.5053(12) 0.067(7) Uani 1 1 d . . . H9A H 0.1456 0.0541 0.4686 0.101 Uiso 1 1 calc R . . H9B H 0.0725 0.1166 0.5100 0.101 Uiso 1 1 calc R . . H9C H 0.1800 0.0452 0.5374 0.101 Uiso 1 1 calc R . . C10 C 0.817(3) 0.184(4) 0.7215(16) 0.130(17) Uani 1 1 d . . . H10A H 0.7975 0.0919 0.7260 0.196 Uiso 1 1 calc R . . H10B H 0.8361 0.2249 0.7598 0.196 Uiso 1 1 calc R . . H10C H 0.8771 0.1880 0.7012 0.196 Uiso 1 1 calc R . . C11 C 0.637(3) 0.258(4) 0.7252(12) 0.108(13) Uani 1 1 d . . . H11A H 0.5756 0.3039 0.7045 0.162 Uiso 1 1 calc R . . H11B H 0.6630 0.3029 0.7618 0.162 Uiso 1 1 calc R . . H11C H 0.6184 0.1668 0.7330 0.162 Uiso 1 1 calc R . . C12 C 0.755(4) 0.398(3) 0.6763(16) 0.130(17) Uani 1 1 d . . . H12A H 0.6945 0.4422 0.6530 0.195 Uiso 1 1 calc R . . H12B H 0.8142 0.3991 0.6555 0.195 Uiso 1 1 calc R . . H12C H 0.7742 0.4436 0.7134 0.195 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 Pb1 0.0488(6) 0.0465(7) 0.0412(6) 0.000 0.0172(5) 0.000 Pb2 0.0384(4) 0.0438(5) 0.0416(4) 0.0003(3) 0.0084(3) -0.0002(3) Pb3 0.0386(6) 0.0424(6) 0.0385(6) 0.000 0.0000(4) 0.000 I1 0.0442(8) 0.0619(9) 0.0459(8) -0.0001(7) 0.0090(6) -0.0020(7) I2 0.0545(8) 0.0471(8) 0.0460(8) -0.0045(6) 0.0099(6) -0.0052(6) I3 0.0558(8) 0.0452(8) 0.0475(8) 0.0035(6) 0.0141(6) 0.0050(6) I4 0.0517(8) 0.0457(8) 0.0485(8) 0.0096(6) -0.0003(6) -0.0083(6) I5 0.0522(8) 0.0475(8) 0.0535(8) -0.0136(7) 0.0061(6) 0.0032(6) I6 0.0616(9) 0.0627(10) 0.0432(8) 0.0011(7) 0.0138(7) 0.0011(7) N1 0.039(9) 0.025(8) 0.050(10) 0.004(7) -0.011(7) 0.008(7) N2 0.048(10) 0.028(8) 0.051(10) -0.007(7) 0.017(8) -0.001(7) C1 0.057(14) 0.047(13) 0.071(15) 0.012(12) 0.026(12) -0.004(11) C2 0.040(12) 0.081(17) 0.050(13) -0.001(12) -0.001(10) -0.016(11) C3 0.037(11) 0.078(17) 0.075(16) 0.006(14) 0.024(11) -0.017(12) C4 0.047(13) 0.067(15) 0.048(13) -0.013(11) 0.009(10) 0.005(11) C5 0.048(12) 0.048(13) 0.062(14) 0.003(11) 0.017(10) 0.013(10) C6 0.064(14) 0.042(12) 0.055(13) -0.015(11) 0.015(11) 0.010(11) C7 0.070(16) 0.072(17) 0.054(14) -0.010(13) -0.001(12) 0.004(13) C8 0.046(13) 0.045(13) 0.078(16) 0.005(12) -0.010(11) -0.008(10) C9 0.058(15) 0.068(17) 0.075(17) 0.011(14) 0.011(13) -0.009(13) C10 0.11(3) 0.16(4) 0.10(3) -0.03(3) -0.04(2) 0.08(3) C11 0.09(2) 0.19(4) 0.053(16) -0.01(2) 0.041(16) 0.02(2) C12 0.19(4) 0.07(2) 0.11(3) 0.009(19) -0.04(3) -0.08(2) _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 Pb1 I2 3.1894(16) . ? Pb1 I2 3.1894(16) 2 ? Pb1 I3 3.2410(17) . ? Pb1 I3 3.2410(17) 2 ? Pb1 I1 3.3428(15) 2 ? Pb1 I1 3.3428(15) . ? Pb1 Pb2 4.0808(10) . ? Pb1 Pb2 4.0808(10) 2 ? Pb2 I6 3.0100(17) . ? Pb2 I3 3.1800(16) . ? Pb2 I4 3.2073(16) . ? Pb2 I2 3.2691(16) . ? Pb2 I5 3.3167(17) . ? Pb2 I1 3.6026(17) . ? Pb2 Pb3 4.0949(11) . ? Pb3 I4 3.1924(16) 2_655 ? Pb3 I4 3.1924(16) . ? Pb3 I5 3.2243(16) . ? Pb3 I5 3.2243(16) 2_655 ? Pb3 I1 3.3177(15) 2_655 ? Pb3 I1 3.3177(15) . ? Pb3 Pb2 4.0949(11) 2_655 ? N1 C7 1.42(3) . ? N1 C1 1.48(3) . ? N1 C8 1.50(3) . ? N1 C9 1.53(3) . ? N2 C10 1.47(3) . ? N2 C12 1.48(3) . ? N2 C6 1.50(3) . ? N2 C11 1.54(3) . ? C1 C2 1.50(3) . ? C2 C3 1.56(3) . ? C3 C4 1.47(3) . ? C4 C5 1.52(3) . ? C5 C6 1.53(3) . ? 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 I2 Pb1 I2 96.24(6) . 2 ? I2 Pb1 I3 89.24(4) . . ? I2 Pb1 I3 172.52(4) 2 . ? I2 Pb1 I3 172.52(4) . 2 ? I2 Pb1 I3 89.24(4) 2 2 ? I3 Pb1 I3 85.78(6) . 2 ? I2 Pb1 I1 89.58(4) . 2 ? I2 Pb1 I1 86.32(4) 2 2 ? I3 Pb1 I1 98.85(4) . 2 ? I3 Pb1 I1 85.67(4) 2 2 ? I2 Pb1 I1 86.32(4) . . ? I2 Pb1 I1 89.58(4) 2 . ? I3 Pb1 I1 85.67(4) . . ? I3 Pb1 I1 98.85(4) 2 . ? I1 Pb1 I1 173.87(7) 2 . ? I2 Pb1 Pb2 51.69(3) . . ? I2 Pb1 Pb2 131.04(4) 2 . ? I3 Pb1 Pb2 49.88(3) . . ? I3 Pb1 Pb2 127.17(4) 2 . ? I1 Pb1 Pb2 123.17(3) 2 . ? I1 Pb1 Pb2 57.03(3) . . ? I2 Pb1 Pb2 131.04(4) . 2 ? I2 Pb1 Pb2 51.69(3) 2 2 ? I3 Pb1 Pb2 127.17(4) . 2 ? I3 Pb1 Pb2 49.88(3) 2 2 ? I1 Pb1 Pb2 57.03(3) 2 2 ? I1 Pb1 Pb2 123.17(3) . 2 ? Pb2 Pb1 Pb2 176.86(4) . 2 ? I6 Pb2 I3 93.24(5) . . ? I6 Pb2 I4 96.76(5) . . ? I3 Pb2 I4 91.72(5) . . ? I6 Pb2 I2 98.01(5) . . ? I3 Pb2 I2 88.91(4) . . ? I4 Pb2 I2 165.16(4) . . ? I6 Pb2 I5 103.57(5) . . ? I3 Pb2 I5 163.16(5) . . ? I4 Pb2 I5 85.26(4) . . ? I2 Pb2 I5 89.85(4) . . ? I6 Pb2 I1 175.49(5) . . ? I3 Pb2 I1 82.35(4) . . ? I4 Pb2 I1 84.39(4) . . ? I2 Pb2 I1 80.99(4) . . ? I5 Pb2 I1 80.86(4) . . ? I6 Pb2 Pb1 125.05(4) . . ? I3 Pb2 Pb1 51.20(3) . . ? I4 Pb2 Pb1 120.81(4) . . ? I2 Pb2 Pb1 49.95(3) . . ? I5 Pb2 Pb1 117.03(4) . . ? I1 Pb2 Pb1 51.12(3) . . ? I6 Pb2 Pb3 133.12(4) . . ? I3 Pb2 Pb3 116.28(4) . . ? I4 Pb2 Pb3 50.06(3) . . ? I2 Pb2 Pb3 116.92(4) . . ? I5 Pb2 Pb3 50.24(3) . . ? I1 Pb2 Pb3 50.57(3) . . ? Pb1 Pb2 Pb3 101.68(2) . . ? I4 Pb3 I4 88.87(6) 2_655 . ? I4 Pb3 I5 175.69(5) 2_655 . ? I4 Pb3 I5 87.05(4) . . ? I4 Pb3 I5 87.05(4) 2_655 2_655 ? I4 Pb3 I5 175.69(5) . 2_655 ? I5 Pb3 I5 97.05(6) . 2_655 ? I4 Pb3 I1 89.48(4) 2_655 2_655 ? I4 Pb3 I1 91.82(4) . 2_655 ? I5 Pb3 I1 92.06(4) . 2_655 ? I5 Pb3 I1 86.73(4) 2_655 2_655 ? I4 Pb3 I1 91.82(4) 2_655 . ? I4 Pb3 I1 89.48(4) . . ? I5 Pb3 I1 86.73(4) . . ? I5 Pb3 I1 92.06(4) 2_655 . ? I1 Pb3 I1 178.17(7) 2_655 . ? I4 Pb3 Pb2 123.69(4) 2_655 . ? I4 Pb3 Pb2 50.38(3) . . ? I5 Pb3 Pb2 52.26(3) . . ? I5 Pb3 Pb2 133.55(4) 2_655 . ? I1 Pb3 Pb2 123.12(3) 2_655 . ? I1 Pb3 Pb2 57.01(3) . . ? I4 Pb3 Pb2 50.38(3) 2_655 2_655 ? I4 Pb3 Pb2 123.69(4) . 2_655 ? I5 Pb3 Pb2 133.55(4) . 2_655 ? I5 Pb3 Pb2 52.26(3) 2_655 2_655 ? I1 Pb3 Pb2 57.01(3) 2_655 2_655 ? I1 Pb3 Pb2 123.12(3) . 2_655 ? Pb2 Pb3 Pb2 173.34(4) . 2_655 ? Pb3 I1 Pb1 144.26(5) . . ? Pb3 I1 Pb2 72.43(3) . . ? Pb1 I1 Pb2 71.86(3) . . ? Pb1 I2 Pb2 78.36(4) . . ? Pb2 I3 Pb1 78.91(4) . . ? Pb3 I4 Pb2 79.56(4) . . ? Pb3 I5 Pb2 77.50(4) . . ? C7 N1 C1 117.2(18) . . ? C7 N1 C8 113.9(18) . . ? C1 N1 C8 107.3(18) . . ? C7 N1 C9 106.1(19) . . ? C1 N1 C9 104.3(16) . . ? C8 N1 C9 107.2(16) . . ? C10 N2 C12 111(3) . . ? C10 N2 C6 111(2) . . ? C12 N2 C6 110(2) . . ? C10 N2 C11 106(2) . . ? C12 N2 C11 108(3) . . ? C6 N2 C11 109.8(19) . . ? N1 C1 C2 117(2) . . ? C1 C2 C3 111(2) . . ? C4 C3 C2 113.8(19) . . ? C3 C4 C5 116(2) . . ? C4 C5 C6 110.7(17) . . ? N2 C6 C5 115.9(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.587 _refine_diff_density_min -1.255 _refine_diff_density_rms 0.283 #===END data_nk80n _database_code_CSD 153705 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 I16 N12 Na4 O12 Pb6' _chemical_formula_weight 4242.66 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.495(2) _cell_length_b 13.623(2) _cell_length_c 14.231(2) _cell_angle_alpha 80.470(10) _cell_angle_beta 84.660(10) _cell_angle_gamma 89.150(10) _cell_volume 2378.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 26.0 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 15.834 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4501 _exptl_absorpt_correction_T_max 0.5700 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15922 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7886 _reflns_number_gt 5624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _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^)+(0.0313P)^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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7886 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _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 Pb1 Pb 0.19671(3) 0.62157(3) 0.66004(2) 0.02829(9) Uani 1 1 d . . . Pb2 Pb 0.52433(3) 0.60326(3) 0.60737(3) 0.02779(8) Uani 1 1 d . . . Pb3 Pb 0.85310(3) 0.59445(3) 0.55804(2) 0.02828(9) Uani 1 1 d . . . I1 I 0.33739(5) 0.58705(4) 0.44845(4) 0.02907(13) Uani 1 1 d . . . I2 I 0.04487(5) 0.43455(5) 0.64555(4) 0.03214(14) Uani 1 1 d . . . I3 I 0.01512(6) 0.76308(5) 0.55345(6) 0.0521(2) Uani 1 1 d . . . I4 I 0.36716(5) 0.46392(5) 0.74667(4) 0.03511(15) Uani 1 1 d . . . I5 I 0.38373(5) 0.78571(5) 0.66398(5) 0.04319(17) Uani 1 1 d . . . I6 I 0.69028(5) 0.60537(5) 0.75622(4) 0.04016(16) Uani 1 1 d . . . I7 I 0.69755(5) 0.73802(5) 0.45776(5) 0.04004(16) Uani 1 1 d . . . I8 I 0.08859(6) 0.65353(6) 0.84463(5) 0.0518(2) Uani 1 1 d . . . Na1 Na 0.5000 0.0000 0.0000 0.0326(11) Uani 1 2 d S . . Na2 Na 0.7499(2) 0.0070(3) 0.0095(2) 0.0282(7) Uani 1 1 d . . . Na3 Na 1.0000 0.0000 0.0000 0.0281(11) Uani 1 2 d S . . O1 O 0.6176(5) 0.1321(5) 0.0187(5) 0.0394(16) Uani 1 1 d . . . N1 N 0.5691(6) 0.2922(6) 0.0298(5) 0.0321(18) Uani 1 1 d . . . C1 C 0.6332(7) 0.2144(7) 0.0405(7) 0.032(2) Uani 1 1 d . . . H1 H 0.6984 0.2224 0.0678 0.039 Uiso 1 1 calc R . . C2 C 0.5974(10) 0.3846(8) 0.0557(9) 0.055(3) Uani 1 1 d . . . H2A H 0.5391 0.4327 0.0436 0.082 Uiso 1 1 calc R . . H2B H 0.6635 0.4102 0.0175 0.082 Uiso 1 1 calc R . . H2C H 0.6090 0.3744 0.1238 0.082 Uiso 1 1 calc R . . C3 C 0.4642(10) 0.2857(9) -0.0111(9) 0.055(3) Uani 1 1 d . . . H3A H 0.4264 0.3494 -0.0131 0.083 Uiso 1 1 calc R . . H3B H 0.4202 0.2330 0.0290 0.083 Uiso 1 1 calc R . . H3C H 0.4770 0.2703 -0.0761 0.083 Uiso 1 1 calc R . . O2 O 0.6436(5) -0.0334(5) -0.1115(5) 0.0378(16) Uani 1 1 d . . . N2 N 0.7216(6) -0.0629(6) -0.2546(6) 0.0355(18) Uani 1 1 d . . . C4 C 0.6447(7) -0.0735(8) -0.1824(7) 0.035(2) Uani 1 1 d . . . H4 H 0.5859 -0.1156 -0.1862 0.043 Uiso 1 1 calc R . . C5 C 0.7132(9) -0.1134(9) -0.3387(8) 0.052(3) Uani 1 1 d . . . H5A H 0.7760 -0.0965 -0.3849 0.078 Uiso 1 1 calc R . . H5B H 0.6477 -0.0913 -0.3689 0.078 Uiso 1 1 calc R . . H5C H 0.7103 -0.1856 -0.3176 0.078 Uiso 1 1 calc R . . C6 C 0.8158(9) -0.0003(9) -0.2576(8) 0.052(3) Uani 1 1 d . . . H6A H 0.8614 -0.0024 -0.3171 0.078 Uiso 1 1 calc R . . H6B H 0.8564 -0.0248 -0.2028 0.078 Uiso 1 1 calc R . . H6C H 0.7929 0.0684 -0.2550 0.078 Uiso 1 1 calc R . . O3 O 0.6124(5) -0.0768(5) 0.1228(5) 0.0404(16) Uani 1 1 d . . . N3 N 0.5248(6) -0.1043(6) 0.2709(6) 0.039(2) Uani 1 1 d . . . C7 C 0.5911(7) -0.0559(7) 0.2046(8) 0.039(2) Uani 1 1 d . . . H7 H 0.6264 0.0001 0.2195 0.046 Uiso 1 1 calc R . . C8 C 0.5034(10) -0.0734(11) 0.3639(8) 0.062(4) Uani 1 1 d . . . H8A H 0.4512 -0.1188 0.4039 0.093 Uiso 1 1 calc R . . H8B H 0.4744 -0.0056 0.3555 0.093 Uiso 1 1 calc R . . H8C H 0.5704 -0.0749 0.3949 0.093 Uiso 1 1 calc R . . C9 C 0.4700(12) -0.1907(11) 0.2561(12) 0.081(5) Uani 1 1 d . . . H9A H 0.4239 -0.2169 0.3141 0.122 Uiso 1 1 calc R . . H9B H 0.5226 -0.2414 0.2417 0.122 Uiso 1 1 calc R . . H9C H 0.4257 -0.1732 0.2024 0.122 Uiso 1 1 calc R . . O4 O 0.8736(5) -0.1119(4) -0.0395(5) 0.0344(15) Uani 1 1 d . . . N4 N 0.8347(6) -0.2744(5) 0.0201(6) 0.0315(17) Uani 1 1 d . . . C10 C 0.8575(7) -0.1992(7) -0.0504(7) 0.032(2) Uani 1 1 d . . . H10 H 0.8618 -0.2128 -0.1140 0.039 Uiso 1 1 calc R . . C11 C 0.8210(8) -0.3747(6) 0.0022(7) 0.036(2) Uani 1 1 d . . . H11A H 0.8044 -0.4193 0.0631 0.053 Uiso 1 1 calc R . . H11B H 0.8874 -0.3965 -0.0305 0.053 Uiso 1 1 calc R . . H11C H 0.7618 -0.3760 -0.0382 0.053 Uiso 1 1 calc R . . C12 C 0.8236(10) -0.2581(8) 0.1177(7) 0.046(3) Uani 1 1 d . . . H12A H 0.8064 -0.3212 0.1602 0.069 Uiso 1 1 calc R . . H12B H 0.7656 -0.2102 0.1261 0.069 Uiso 1 1 calc R . . H12C H 0.8911 -0.2317 0.1333 0.069 Uiso 1 1 calc R . . O5 O 0.8805(5) 0.1251(4) -0.0758(4) 0.0302(14) Uani 1 1 d . . . N5 N 0.8512(6) 0.2900(6) -0.1230(5) 0.0336(18) Uani 1 1 d . . . C13 C 0.8913(7) 0.2149(7) -0.0714(6) 0.029(2) Uani 1 1 d . . . H13 H 0.9347 0.2295 -0.0240 0.034 Uiso 1 1 calc R . . C14 C 0.8689(10) 0.3907(7) -0.1093(8) 0.047(3) Uani 1 1 d . . . H14A H 0.8322 0.4369 -0.1562 0.071 Uiso 1 1 calc R . . H14B H 0.9462 0.4050 -0.1180 0.071 Uiso 1 1 calc R . . H14C H 0.8405 0.3988 -0.0446 0.071 Uiso 1 1 calc R . . C15 C 0.7826(12) 0.2770(9) -0.1973(10) 0.068(4) Uani 1 1 d . . . H15A H 0.7606 0.3423 -0.2296 0.102 Uiso 1 1 calc R . . H15B H 0.7188 0.2385 -0.1683 0.102 Uiso 1 1 calc R . . H15C H 0.8223 0.2414 -0.2439 0.102 Uiso 1 1 calc R . . O6 O 0.8701(5) 0.0120(6) 0.1304(5) 0.0413(17) Uani 1 1 d . . . N6 N 0.8869(6) -0.0259(6) 0.2884(5) 0.0337(18) Uani 1 1 d . . . C16 C 0.8615(7) 0.0310(8) 0.2122(7) 0.039(2) Uani 1 1 d . . . H16 H 0.8329 0.0945 0.2201 0.047 Uiso 1 1 calc R . . C17 C 0.9351(8) -0.1223(8) 0.2834(7) 0.040(2) Uani 1 1 d . . . H17A H 0.9479 -0.1554 0.3480 0.061 Uiso 1 1 calc R . . H17B H 1.0035 -0.1138 0.2433 0.061 Uiso 1 1 calc R . . H17C H 0.8865 -0.1631 0.2557 0.061 Uiso 1 1 calc R . . C18 C 0.8672(10) 0.0024(9) 0.3841(7) 0.050(3) Uani 1 1 d . . . H18A H 0.8913 -0.0513 0.4322 0.076 Uiso 1 1 calc R . . H18B H 0.7902 0.0139 0.3980 0.076 Uiso 1 1 calc R . . H18C H 0.9071 0.0634 0.3858 0.076 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 Pb1 0.02313(16) 0.03342(19) 0.02914(18) -0.00785(15) -0.00184(13) 0.00038(14) Pb2 0.02228(15) 0.03181(17) 0.02969(16) -0.00609(14) -0.00275(12) 0.00050(13) Pb3 0.02286(16) 0.03141(18) 0.03137(18) -0.00636(15) -0.00479(13) 0.00118(14) I1 0.0311(3) 0.0307(3) 0.0253(3) -0.0049(2) -0.0015(2) 0.0011(2) I2 0.0292(3) 0.0350(3) 0.0319(3) -0.0043(3) -0.0034(2) 0.0022(2) I3 0.0505(4) 0.0322(3) 0.0776(5) -0.0018(4) -0.0384(4) -0.0038(3) I4 0.0329(3) 0.0359(3) 0.0345(3) 0.0002(3) -0.0027(3) -0.0021(3) I5 0.0333(3) 0.0325(3) 0.0662(4) -0.0184(3) 0.0015(3) -0.0017(3) I6 0.0373(3) 0.0560(4) 0.0300(3) -0.0117(3) -0.0104(3) 0.0052(3) I7 0.0307(3) 0.0389(3) 0.0477(4) 0.0006(3) -0.0027(3) 0.0006(3) I8 0.0535(4) 0.0649(5) 0.0375(4) -0.0173(4) 0.0088(3) 0.0068(4) Na1 0.016(2) 0.042(3) 0.042(3) -0.013(2) -0.003(2) 0.004(2) Na2 0.0195(15) 0.0306(18) 0.0340(18) -0.0049(15) -0.0009(14) -0.0011(14) Na3 0.020(2) 0.026(2) 0.037(3) -0.002(2) -0.008(2) 0.0021(19) O1 0.030(3) 0.030(4) 0.061(4) -0.015(3) -0.007(3) 0.006(3) N1 0.031(4) 0.028(4) 0.038(4) -0.006(4) -0.006(3) 0.009(3) C1 0.024(4) 0.037(5) 0.036(5) -0.007(4) -0.001(4) 0.001(4) C2 0.053(7) 0.043(6) 0.072(8) -0.025(6) 0.002(6) 0.004(5) C3 0.061(7) 0.048(7) 0.066(7) -0.022(6) -0.035(6) 0.021(6) O2 0.026(3) 0.054(4) 0.036(4) -0.013(3) -0.008(3) 0.000(3) N2 0.033(4) 0.041(5) 0.036(4) -0.013(4) -0.006(3) 0.005(4) C4 0.017(4) 0.044(6) 0.048(6) -0.015(5) -0.010(4) 0.007(4) C5 0.051(6) 0.064(8) 0.045(6) -0.024(6) -0.003(5) 0.011(6) C6 0.052(7) 0.055(7) 0.050(6) -0.013(6) 0.005(5) -0.015(6) O3 0.035(4) 0.040(4) 0.045(4) -0.008(3) 0.002(3) -0.005(3) N3 0.037(4) 0.041(5) 0.034(4) 0.004(4) 0.007(4) -0.001(4) C7 0.024(5) 0.030(5) 0.059(7) -0.002(5) -0.005(5) 0.011(4) C8 0.057(7) 0.079(9) 0.044(6) 0.004(6) -0.002(5) 0.021(7) C9 0.082(10) 0.065(9) 0.093(11) -0.010(8) 0.014(9) -0.032(8) O4 0.027(3) 0.022(3) 0.055(4) -0.008(3) -0.003(3) 0.001(3) N4 0.032(4) 0.024(4) 0.041(4) -0.010(4) -0.009(3) -0.007(3) C10 0.023(4) 0.034(5) 0.041(5) -0.005(5) -0.008(4) -0.003(4) C11 0.046(5) 0.020(4) 0.040(5) 0.005(4) -0.013(4) 0.000(4) C12 0.066(7) 0.033(5) 0.038(6) -0.002(5) 0.003(5) -0.009(5) O5 0.034(3) 0.021(3) 0.034(3) -0.001(3) -0.003(3) 0.000(3) N5 0.042(4) 0.031(4) 0.028(4) -0.001(3) -0.009(3) 0.003(4) C13 0.025(4) 0.033(5) 0.028(4) -0.001(4) -0.006(4) 0.005(4) C14 0.071(7) 0.024(5) 0.042(6) -0.002(5) 0.008(5) 0.008(5) C15 0.094(10) 0.040(6) 0.076(9) 0.002(7) -0.064(8) -0.006(6) O6 0.031(3) 0.057(5) 0.036(4) -0.011(3) -0.003(3) 0.002(3) N6 0.037(4) 0.035(4) 0.030(4) -0.007(4) -0.005(3) -0.001(4) C16 0.031(5) 0.040(6) 0.047(6) -0.008(5) -0.009(4) -0.004(4) C17 0.046(6) 0.038(5) 0.038(5) -0.009(5) -0.005(5) 0.001(5) C18 0.066(7) 0.052(7) 0.040(6) -0.029(5) -0.008(5) 0.003(6) _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 Pb1 I8 2.9353(8) . ? Pb1 I4 3.1850(8) . ? Pb1 I2 3.2440(9) . ? Pb1 I5 3.2688(9) . ? Pb1 I3 3.2724(9) . ? Pb1 I1 3.4405(8) . ? Pb1 Pb2 4.1039(8) . ? Pb1 Pb3 4.6970(8) 1_455 ? Pb1 Pb3 4.7030(8) 2_666 ? Pb2 I4 3.0871(8) . ? Pb2 I6 3.1028(9) . ? Pb2 I5 3.1911(8) . ? Pb2 I7 3.2486(9) . ? Pb2 I1 3.2606(8) 2_666 ? Pb2 I1 3.4327(8) . ? Pb2 Pb3 4.1060(8) . ? Pb2 Pb2 4.5680(10) 2_666 ? Pb3 I7 3.0197(8) . ? Pb3 I3 3.0730(9) 1_655 ? Pb3 I2 3.1389(8) 2_666 ? Pb3 I6 3.3433(8) . ? Pb3 I2 3.3971(8) 1_655 ? Pb3 I1 3.4754(9) 2_666 ? Pb3 Pb1 4.6970(8) 1_655 ? Pb3 Pb1 4.7030(8) 2_666 ? Pb3 Pb3 4.7777(9) 2_766 ? I1 Pb2 3.2606(8) 2_666 ? I1 Pb3 3.4754(9) 2_666 ? I2 Pb3 3.1389(8) 2_666 ? I2 Pb3 3.3971(8) 1_455 ? I3 Pb3 3.0730(9) 1_455 ? Na1 O2 2.372(6) 2_655 ? Na1 O2 2.372(6) . ? Na1 O1 2.404(7) 2_655 ? Na1 O1 2.404(7) . ? Na1 O3 2.435(7) . ? Na1 O3 2.435(7) 2_655 ? Na1 Na2 3.142(3) 2_655 ? Na1 Na2 3.142(3) . ? Na2 O4 2.366(7) . ? Na2 O1 2.368(7) . ? Na2 O6 2.397(8) . ? Na2 O5 2.406(7) . ? Na2 O3 2.406(7) . ? Na2 O2 2.407(8) . ? Na2 Na3 3.116(3) . ? Na3 O6 2.374(6) 2_755 ? Na3 O6 2.374(6) . ? Na3 O4 2.378(7) 2_755 ? Na3 O4 2.378(7) . ? Na3 O5 2.432(6) . ? Na3 O5 2.432(6) 2_755 ? Na3 Na2 3.116(3) 2_755 ? O1 C1 1.234(11) . ? N1 C1 1.317(11) . ? N1 C2 1.427(14) . ? N1 C3 1.492(13) . ? O2 C4 1.222(12) . ? N2 C4 1.331(12) . ? N2 C6 1.456(14) . ? N2 C5 1.488(14) . ? O3 C7 1.248(13) . ? N3 C7 1.294(12) . ? N3 C9 1.425(17) . ? N3 C8 1.455(15) . ? O4 C10 1.246(11) . ? N4 C10 1.324(11) . ? N4 C12 1.436(13) . ? N4 C11 1.446(12) . ? O5 C13 1.245(11) . ? N5 C13 1.281(11) . ? N5 C14 1.440(13) . ? N5 C15 1.456(14) . ? O6 C16 1.229(12) . ? N6 C16 1.287(12) . ? N6 C17 1.446(13) . ? N6 C18 1.474(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 I8 Pb1 I4 96.12(2) . . ? I8 Pb1 I2 93.67(2) . . ? I4 Pb1 I2 87.50(2) . . ? I8 Pb1 I5 93.14(3) . . ? I4 Pb1 I5 84.74(2) . . ? I2 Pb1 I5 170.170(18) . . ? I8 Pb1 I3 88.62(3) . . ? I4 Pb1 I3 172.68(2) . . ? I2 Pb1 I3 86.64(2) . . ? I5 Pb1 I3 100.61(2) . . ? I8 Pb1 I1 176.67(2) . . ? I4 Pb1 I1 81.87(2) . . ? I2 Pb1 I1 88.90(2) . . ? I5 Pb1 I1 84.06(2) . . ? I3 Pb1 I1 93.65(2) . . ? I8 Pb1 Pb2 123.47(2) . . ? I4 Pb1 Pb2 48.106(15) . . ? I2 Pb1 Pb2 120.445(17) . . ? I5 Pb1 Pb2 49.726(16) . . ? I3 Pb1 Pb2 132.67(2) . . ? I1 Pb1 Pb2 53.251(14) . . ? I8 Pb1 Pb3 87.20(2) . 1_455 ? I4 Pb1 Pb3 133.801(18) . 1_455 ? I2 Pb1 Pb3 46.323(14) . 1_455 ? I5 Pb1 Pb3 141.252(17) . 1_455 ? I3 Pb1 Pb3 40.640(16) . 1_455 ? I1 Pb1 Pb3 96.105(17) . 1_455 ? Pb2 Pb1 Pb3 149.154(12) . 1_455 ? I8 Pb1 Pb3 135.25(2) . 2_666 ? I4 Pb1 Pb3 86.510(18) . 2_666 ? I2 Pb1 Pb3 41.681(14) . 2_666 ? I5 Pb1 Pb3 131.497(18) . 2_666 ? I3 Pb1 Pb3 86.20(2) . 2_666 ? I1 Pb1 Pb3 47.467(14) . 2_666 ? Pb2 Pb1 Pb3 90.918(13) . 2_666 ? Pb3 Pb1 Pb3 61.097(11) 1_455 2_666 ? I4 Pb2 I6 93.87(2) . . ? I4 Pb2 I5 87.69(2) . . ? I6 Pb2 I5 96.40(2) . . ? I4 Pb2 I7 176.53(2) . . ? I6 Pb2 I7 85.80(2) . . ? I5 Pb2 I7 95.78(2) . . ? I4 Pb2 I1 90.89(2) . 2_666 ? I6 Pb2 I1 84.21(2) . 2_666 ? I5 Pb2 I1 178.49(2) . 2_666 ? I7 Pb2 I1 85.64(2) . 2_666 ? I4 Pb2 I1 83.41(2) . . ? I6 Pb2 I1 176.72(2) . . ? I5 Pb2 I1 85.36(2) . . ? I7 Pb2 I1 96.79(2) . . ? I1 Pb2 I1 93.966(19) 2_666 . ? I4 Pb2 Pb1 50.175(16) . . ? I6 Pb2 Pb1 125.854(19) . . ? I5 Pb2 Pb1 51.401(16) . . ? I7 Pb2 Pb1 132.458(18) . . ? I1 Pb2 Pb1 127.160(18) 2_666 . ? I1 Pb2 Pb1 53.426(15) . . ? I4 Pb2 Pb3 130.761(19) . . ? I6 Pb2 Pb3 53.071(16) . . ? I5 Pb2 Pb3 126.58(2) . . ? I7 Pb2 Pb3 46.705(15) . . ? I1 Pb2 Pb3 54.859(15) 2_666 . ? I1 Pb2 Pb3 127.767(17) . . ? Pb1 Pb2 Pb3 177.955(14) . . ? I4 Pb2 Pb2 85.69(2) . 2_666 ? I6 Pb2 Pb2 132.70(2) . 2_666 ? I5 Pb2 Pb2 130.75(2) . 2_666 ? I7 Pb2 Pb2 91.98(2) . 2_666 ? I1 Pb2 Pb2 48.561(15) 2_666 2_666 ? I1 Pb2 Pb2 45.404(14) . 2_666 ? Pb1 Pb2 Pb2 89.048(15) . 2_666 ? Pb3 Pb2 Pb2 92.830(15) . 2_666 ? I7 Pb3 I3 91.09(2) . 1_655 ? I7 Pb3 I2 87.32(2) . 2_666 ? I3 Pb3 I2 88.56(2) 1_655 2_666 ? I7 Pb3 I6 85.48(2) . . ? I3 Pb3 I6 103.58(3) 1_655 . ? I2 Pb3 I6 165.99(2) 2_666 . ? I7 Pb3 I2 173.30(2) . 1_655 ? I3 Pb3 I2 87.26(2) 1_655 1_655 ? I2 Pb3 I2 86.14(2) 2_666 1_655 ? I6 Pb3 I2 101.21(2) . 1_655 ? I7 Pb3 I1 85.57(2) . 2_666 ? I3 Pb3 I1 176.42(2) 1_655 2_666 ? I2 Pb3 I1 90.00(2) 2_666 2_666 ? I6 Pb3 I1 77.48(2) . 2_666 ? I2 Pb3 I1 95.91(2) 1_655 2_666 ? I7 Pb3 Pb2 51.538(17) . . ? I3 Pb3 Pb2 128.18(2) 1_655 . ? I2 Pb3 Pb2 118.778(18) 2_666 . ? I6 Pb3 Pb2 47.892(15) . . ? I2 Pb3 Pb2 133.727(18) 1_655 . ? I1 Pb3 Pb2 50.102(14) 2_666 . ? I7 Pb3 Pb1 135.004(19) . 1_655 ? I3 Pb3 Pb1 43.911(16) 1_655 1_655 ? I2 Pb3 Pb1 90.598(18) 2_666 1_655 ? I6 Pb3 Pb1 102.980(18) . 1_655 ? I2 Pb3 Pb1 43.682(15) 1_655 1_655 ? I1 Pb3 Pb1 139.404(15) 2_666 1_655 ? Pb2 Pb3 Pb1 150.537(12) . 1_655 ? I7 Pb3 Pb1 88.85(2) . 2_666 ? I3 Pb3 Pb1 131.93(2) 1_655 2_666 ? I2 Pb3 Pb1 43.413(15) 2_666 2_666 ? I6 Pb3 Pb1 124.313(19) . 2_666 ? I2 Pb3 Pb1 87.424(17) 1_655 2_666 ? I1 Pb3 Pb1 46.844(13) 2_666 2_666 ? Pb2 Pb3 Pb1 87.193(14) . 2_666 ? Pb1 Pb3 Pb1 118.902(12) 1_655 2_666 ? I7 Pb3 Pb3 132.49(2) . 2_766 ? I3 Pb3 Pb3 87.10(2) 1_655 2_766 ? I2 Pb3 Pb3 45.187(14) 2_666 2_766 ? I6 Pb3 Pb3 140.869(18) . 2_766 ? I2 Pb3 Pb3 40.957(13) 1_655 2_766 ? I1 Pb3 Pb3 94.198(19) 2_666 2_766 ? Pb2 Pb3 Pb3 143.877(16) . 2_766 ? Pb1 Pb3 Pb3 59.513(13) 1_655 2_766 ? Pb1 Pb3 Pb3 59.389(12) 2_666 2_766 ? Pb2 I1 Pb2 86.034(19) 2_666 . ? Pb2 I1 Pb1 130.65(2) 2_666 . ? Pb2 I1 Pb1 73.323(18) . . ? Pb2 I1 Pb3 75.039(19) 2_666 2_666 ? Pb2 I1 Pb3 131.20(2) . 2_666 ? Pb1 I1 Pb3 85.689(18) . 2_666 ? Pb3 I2 Pb1 94.91(2) 2_666 . ? Pb3 I2 Pb3 93.86(2) 2_666 1_455 ? Pb1 I2 Pb3 90.00(2) . 1_455 ? Pb3 I3 Pb1 95.45(2) 1_455 . ? Pb2 I4 Pb1 81.72(2) . . ? Pb2 I5 Pb1 78.87(2) . . ? Pb2 I6 Pb3 79.04(2) . . ? Pb3 I7 Pb2 81.76(2) . . ? O2 Na1 O2 180.0(4) 2_655 . ? O2 Na1 O1 82.3(2) 2_655 2_655 ? O2 Na1 O1 97.7(2) . 2_655 ? O2 Na1 O1 97.7(2) 2_655 . ? O2 Na1 O1 82.3(2) . . ? O1 Na1 O1 180.0(3) 2_655 . ? O2 Na1 O3 94.1(2) 2_655 . ? O2 Na1 O3 85.9(2) . . ? O1 Na1 O3 103.9(2) 2_655 . ? O1 Na1 O3 76.1(2) . . ? O2 Na1 O3 85.9(2) 2_655 2_655 ? O2 Na1 O3 94.1(2) . 2_655 ? O1 Na1 O3 76.1(2) 2_655 2_655 ? O1 Na1 O3 103.9(2) . 2_655 ? O3 Na1 O3 180.0(4) . 2_655 ? O2 Na1 Na2 49.39(17) 2_655 2_655 ? O2 Na1 Na2 130.61(17) . 2_655 ? O1 Na1 Na2 48.33(15) 2_655 2_655 ? O1 Na1 Na2 131.67(15) . 2_655 ? O3 Na1 Na2 130.87(16) . 2_655 ? O3 Na1 Na2 49.13(16) 2_655 2_655 ? O2 Na1 Na2 130.61(17) 2_655 . ? O2 Na1 Na2 49.39(17) . . ? O1 Na1 Na2 131.67(15) 2_655 . ? O1 Na1 Na2 48.33(15) . . ? O3 Na1 Na2 49.13(16) . . ? O3 Na1 Na2 130.87(16) 2_655 . ? Na2 Na1 Na2 180.00(12) 2_655 . ? O4 Na2 O1 166.0(3) . . ? O4 Na2 O6 83.3(3) . . ? O1 Na2 O6 109.2(3) . . ? O4 Na2 O5 83.8(2) . . ? O1 Na2 O5 92.2(2) . . ? O6 Na2 O5 79.5(2) . . ? O4 Na2 O3 109.2(3) . . ? O1 Na2 O3 77.3(3) . . ? O6 Na2 O3 92.7(3) . . ? O5 Na2 O3 164.2(3) . . ? O4 Na2 O2 85.7(3) . . ? O1 Na2 O2 82.3(3) . . ? O6 Na2 O2 167.8(3) . . ? O5 Na2 O2 104.7(3) . . ? O3 Na2 O2 85.8(3) . . ? O4 Na2 Na3 49.11(17) . . ? O1 Na2 Na3 135.3(2) . . ? O6 Na2 Na3 48.90(16) . . ? O5 Na2 Na3 50.27(15) . . ? O3 Na2 Na3 132.2(2) . . ? O2 Na2 Na3 125.31(19) . . ? O4 Na2 Na1 125.1(2) . . ? O1 Na2 Na1 49.31(18) . . ? O6 Na2 Na1 136.7(2) . . ? O5 Na2 Na1 129.89(19) . . ? O3 Na2 Na1 49.95(18) . . ? O2 Na2 Na1 48.43(16) . . ? Na3 Na2 Na1 173.50(13) . . ? O6 Na3 O6 180.0(3) 2_755 . ? O6 Na3 O4 83.6(2) 2_755 2_755 ? O6 Na3 O4 96.4(2) . 2_755 ? O6 Na3 O4 96.4(2) 2_755 . ? O6 Na3 O4 83.6(2) . . ? O4 Na3 O4 180.0(4) 2_755 . ? O6 Na3 O5 100.5(2) 2_755 . ? O6 Na3 O5 79.5(2) . . ? O4 Na3 O5 97.0(2) 2_755 . ? O4 Na3 O5 83.0(2) . . ? O6 Na3 O5 79.5(2) 2_755 2_755 ? O6 Na3 O5 100.5(2) . 2_755 ? O4 Na3 O5 83.0(2) 2_755 2_755 ? O4 Na3 O5 97.0(2) . 2_755 ? O5 Na3 O5 180.0(4) . 2_755 ? O6 Na3 Na2 130.46(18) 2_755 . ? O6 Na3 Na2 49.54(18) . . ? O4 Na3 Na2 131.22(15) 2_755 . ? O4 Na3 Na2 48.78(15) . . ? O5 Na3 Na2 49.54(15) . . ? O5 Na3 Na2 130.46(15) 2_755 . ? O6 Na3 Na2 49.54(18) 2_755 2_755 ? O6 Na3 Na2 130.46(18) . 2_755 ? O4 Na3 Na2 48.78(15) 2_755 2_755 ? O4 Na3 Na2 131.22(15) . 2_755 ? O5 Na3 Na2 130.46(15) . 2_755 ? O5 Na3 Na2 49.54(15) 2_755 2_755 ? Na2 Na3 Na2 180.00(13) . 2_755 ? C1 O1 Na2 124.9(6) . . ? C1 O1 Na1 151.4(6) . . ? Na2 O1 Na1 82.4(2) . . ? C1 N1 C2 121.6(9) . . ? C1 N1 C3 120.2(9) . . ? C2 N1 C3 118.2(8) . . ? O1 C1 N1 126.8(9) . . ? C4 O2 Na1 131.2(6) . . ? C4 O2 Na2 144.6(6) . . ? Na1 O2 Na2 82.2(2) . . ? C4 N2 C6 122.8(9) . . ? C4 N2 C5 120.7(9) . . ? C6 N2 C5 116.5(8) . . ? O2 C4 N2 125.4(9) . . ? C7 O3 Na2 123.1(7) . . ? C7 O3 Na1 116.6(6) . . ? Na2 O3 Na1 80.9(2) . . ? C7 N3 C9 121.4(10) . . ? C7 N3 C8 121.5(10) . . ? C9 N3 C8 117.1(10) . . ? O3 C7 N3 125.3(11) . . ? C10 O4 Na2 129.4(5) . . ? C10 O4 Na3 145.2(6) . . ? Na2 O4 Na3 82.1(2) . . ? C10 N4 C12 120.3(8) . . ? C10 N4 C11 121.8(8) . . ? C12 N4 C11 118.0(8) . . ? O4 C10 N4 124.9(9) . . ? C13 O5 Na2 129.7(5) . . ? C13 O5 Na3 121.2(6) . . ? Na2 O5 Na3 80.20(19) . . ? C13 N5 C14 122.3(9) . . ? C13 N5 C15 121.0(9) . . ? C14 N5 C15 116.6(8) . . ? O5 C13 N5 128.0(9) . . ? C16 O6 Na3 141.7(6) . . ? C16 O6 Na2 135.4(6) . . ? Na3 O6 Na2 81.6(2) . . ? C16 N6 C17 120.8(9) . . ? C16 N6 C18 122.3(9) . . ? C17 N6 C18 116.9(8) . . ? O6 C16 N6 126.9(10) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.212 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.176 #===END data_pb2x _database_code_CSD 153706 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H98 I12 N14 Na4 O14 Pb4' _chemical_formula_weight 3466.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.8919 1.1868 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -1.1676 6.9287 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0218 0.0150 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.9400(12) _cell_length_b 16.5477(15) _cell_length_c 19.0790(17) _cell_angle_alpha 95.357(11) _cell_angle_beta 104.678(9) _cell_angle_gamma 93.966(10) _cell_volume 4824.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 22.5 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 5.875 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4178 _exptl_absorpt_correction_T_max 0.6508 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35815 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 19.00 _reflns_number_total 15252 _reflns_number_gt 9267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0428P)^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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15252 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.03596(3) 0.27400(3) 0.23123(2) 0.04011(11) Uani 1 d . . . Pb2 Pb 0.28583(3) 0.26427(3) 0.23170(2) 0.04019(10) Uani 1 d . . . Pb3 Pb 0.53723(3) 0.25928(3) 0.23858(2) 0.04212(11) Uani 1 d . . . Pb4 Pb 0.78680(3) 0.26788(3) 0.23729(2) 0.03946(10) Uani 1 d . . . I1 I 0.15191(6) 0.38345(5) 0.15084(4) 0.0530(2) Uani 1 d . . . I2 I 0.20198(6) 0.29030(5) 0.36892(4) 0.0560(2) Uani 1 d . . . I3 I 0.12787(5) 0.12202(4) 0.16869(4) 0.04750(19) Uani 1 d . . . I4 I 0.44432(6) 0.40820(5) 0.29374(5) 0.0560(2) Uani 1 d . . . I5 I 0.42021(6) 0.14174(5) 0.31041(5) 0.0551(2) Uani 1 d . . . I6 I 0.37227(5) 0.23743(5) 0.09787(4) 0.0489(2) Uani 1 d . . . I7 I 0.64047(6) 0.37695(5) 0.15961(5) 0.0569(2) Uani 1 d . . . I8 I 0.70716(6) 0.28924(5) 0.37813(4) 0.0529(2) Uani 1 d . . . I9 I 0.64290(6) 0.11118(5) 0.18413(5) 0.0585(2) Uani 1 d . . . I10 I 0.93366(5) 0.15573(4) 0.31390(4) 0.04731(19) Uani 1 d . . . I11 I 0.85996(6) 0.25925(5) 0.09647(4) 0.0553(2) Uani 1 d . . . I12 I 0.94052(6) 0.41865(4) 0.29497(5) 0.0529(2) Uani 1 d . . . Na1 Na 0.9291(3) 0.7969(2) 0.2743(2) 0.0448(10) Uani 1 d . . . Na2 Na 0.7233(3) 0.7906(3) 0.2582(2) 0.0506(11) Uani 1 d . . . Na3 Na 0.5294(3) 0.7679(3) 0.2660(3) 0.0534(12) Uani 1 d . . . Na4 Na 0.3373(3) 0.7378(3) 0.2691(3) 0.0612(13) Uani 1 d . . . O1 O 0.9679(7) 0.7860(6) 0.1671(5) 0.077(3) Uani 1 d . . . C1 C 1.0005(9) 0.8373(8) 0.1386(7) 0.058(3) Uiso 1 d . . . H1 H 1.0330 0.8830 0.1687 0.069 Uiso 1 calc R . . N1 N 0.9933(6) 0.8336(5) 0.0673(5) 0.046(2) Uiso 1 d . . . C2 C 1.0346(9) 0.8972(8) 0.0361(7) 0.062(3) Uiso 1 d . . . H2A H 1.0219 0.8835 -0.0163 0.093 Uiso 1 calc R . . H2B H 1.0971 0.9018 0.0571 0.093 Uiso 1 calc R . . H2C H 1.0123 0.9488 0.0467 0.093 Uiso 1 calc R . . C3 C 0.9491(10) 0.7664(8) 0.0190(7) 0.068(4) Uiso 1 d . . . H3A H 0.9510 0.7749 -0.0302 0.103 Uiso 1 calc R . . H3B H 0.8890 0.7601 0.0213 0.103 Uiso 1 calc R . . H3C H 0.9767 0.7177 0.0325 0.103 Uiso 1 calc R . . O2 O 1.0176(6) 0.9198(5) 0.3130(5) 0.061(2) Uani 1 d . . . C4 C 1.0834(8) 0.9657(7) 0.3190(6) 0.048(3) Uiso 1 d . . . H4 H 1.0753 1.0212 0.3162 0.057 Uiso 1 calc R . . N2 N 1.1626(7) 0.9469(6) 0.3288(5) 0.050(2) Uiso 1 d . . . C5 C 1.2350(10) 1.0065(8) 0.3345(7) 0.069(4) Uiso 1 d . . . H5A H 1.2883 0.9798 0.3418 0.103 Uiso 1 calc R . . H5B H 1.2395 1.0473 0.3755 0.103 Uiso 1 calc R . . H5C H 1.2259 1.0324 0.2900 0.103 Uiso 1 calc R . . C6 C 1.1817(12) 0.8629(9) 0.3337(9) 0.088(5) Uiso 1 d . . . H6A H 1.2438 0.8597 0.3411 0.132 Uiso 1 calc R . . H6B H 1.1504 0.8297 0.2888 0.132 Uiso 1 calc R . . H6C H 1.1636 0.8431 0.3743 0.132 Uiso 1 calc R . . O3 O 1.0138(6) 0.7032(5) 0.3326(5) 0.067(3) Uani 1 d . . . C7 C 1.0059(10) 0.6595(9) 0.3787(8) 0.073(4) Uiso 1 d . . . H7 H 0.9847 0.6047 0.3629 0.087 Uiso 1 calc R . . N3 N 1.0249(8) 0.6835(7) 0.4496(7) 0.075(3) Uiso 1 d . . . C8 C 1.0496(14) 0.7677(12) 0.4788(10) 0.115(6) Uiso 1 d . . . H8A H 1.0608 0.7727 0.5315 0.173 Uiso 1 calc R . . H8B H 1.0029 0.8002 0.4588 0.173 Uiso 1 calc R . . H8C H 1.1019 0.7868 0.4657 0.173 Uiso 1 calc R . . C9 C 1.0155(19) 0.6286(16) 0.4994(14) 0.172(11) Uiso 1 d . . . H9A H 1.0325 0.6569 0.5484 0.258 Uiso 1 calc R . . H9B H 1.0523 0.5849 0.4960 0.258 Uiso 1 calc R . . H9C H 0.9551 0.6061 0.4881 0.258 Uiso 1 calc R . . O4 O 0.7994(7) 0.8759(5) 0.2049(5) 0.075(3) Uani 1 d . . . C10 C 0.8277(9) 0.9402(8) 0.1863(7) 0.062(3) Uiso 1 d . . . H10 H 0.8557 0.9820 0.2233 0.074 Uiso 1 calc R . . N4 N 0.8210(6) 0.9534(5) 0.1190(5) 0.041(2) Uiso 1 d . . . C11 C 0.8562(13) 1.0293(11) 0.1024(10) 0.106(6) Uiso 1 d . . . H11A H 0.8455 1.0285 0.0500 0.160 Uiso 1 calc R . . H11B H 0.9185 1.0371 0.1248 0.160 Uiso 1 calc R . . H11C H 0.8285 1.0737 0.1213 0.160 Uiso 1 calc R . . C12 C 0.7748(13) 0.8969(11) 0.0602(10) 0.107(6) Uiso 1 d . . . H12A H 0.7773 0.9176 0.0148 0.161 Uiso 1 calc R . . H12B H 0.7145 0.8886 0.0619 0.161 Uiso 1 calc R . . H12C H 0.8006 0.8455 0.0633 0.161 Uiso 1 calc R . . O5 O 0.8119(6) 0.6903(5) 0.2326(4) 0.058(2) Uani 1 d . . . C13 C 0.8195(8) 0.6263(8) 0.2003(6) 0.054(3) Uiso 1 d . . . H13 H 0.8522 0.5900 0.2284 0.065 Uiso 1 calc R . . N5 N 0.7875(7) 0.6009(6) 0.1305(5) 0.052(2) Uiso 1 d . . . C14 C 0.7979(11) 0.5197(9) 0.0978(8) 0.079(4) Uiso 1 d . . . H14A H 0.7695 0.5137 0.0460 0.118 Uiso 1 calc R . . H14B H 0.7717 0.4785 0.1208 0.118 Uiso 1 calc R . . H14C H 0.8594 0.5132 0.1051 0.118 Uiso 1 calc R . . C15 C 0.7408(13) 0.6548(11) 0.0832(10) 0.107(6) Uiso 1 d . . . H15A H 0.7216 0.6276 0.0338 0.161 Uiso 1 calc R . . H15B H 0.7788 0.7036 0.0841 0.161 Uiso 1 calc R . . H15C H 0.6907 0.6698 0.0997 0.161 Uiso 1 calc R . . O6 O 0.8509(6) 0.8345(5) 0.3628(4) 0.059(2) Uani 1 d . . . C16 C 0.8659(8) 0.9056(7) 0.3906(6) 0.051(3) Uiso 1 d . . . H16 H 0.8818 0.9438 0.3617 0.061 Uiso 1 calc R . . N6 N 0.8624(6) 0.9342(5) 0.4556(5) 0.048(2) Uiso 1 d . . . C17 C 0.8823(10) 1.0172(8) 0.4844(7) 0.068(4) Uiso 1 d . . . H17A H 0.8751 1.0240 0.5336 0.102 Uiso 1 calc R . . H17B H 0.8435 1.0501 0.4540 0.102 Uiso 1 calc R . . H17C H 0.9421 1.0344 0.4856 0.102 Uiso 1 calc R . . C18 C 0.8355(11) 0.8779(10) 0.5040(9) 0.089(5) Uiso 1 d . . . H18A H 0.8361 0.9084 0.5501 0.133 Uiso 1 calc R . . H18B H 0.8756 0.8363 0.5126 0.133 Uiso 1 calc R . . H18C H 0.7771 0.8524 0.4809 0.133 Uiso 1 calc R . . O7 O 0.5869(6) 0.7843(5) 0.1645(5) 0.065(2) Uani 1 d . . . C19 C 0.5756(10) 0.8403(9) 0.1266(8) 0.069(4) Uiso 1 d . . . H19 H 0.6151 0.8873 0.1414 0.083 Uiso 1 calc R . . N7 N 0.5134(9) 0.8400(8) 0.0676(7) 0.078(3) Uiso 1 d . . . C20 C 0.4535(14) 0.7747(12) 0.0403(11) 0.120(7) Uiso 1 d . . . H20A H 0.4128 0.7870 -0.0037 0.179 Uiso 1 calc R . . H20B H 0.4222 0.7628 0.0761 0.179 Uiso 1 calc R . . H20C H 0.4828 0.7277 0.0289 0.179 Uiso 1 calc R . . C21 C 0.5074(13) 0.9099(11) 0.0257(10) 0.103(6) Uiso 1 d . . . H21A H 0.4573 0.8995 -0.0163 0.154 Uiso 1 calc R . . H21B H 0.5599 0.9185 0.0094 0.154 Uiso 1 calc R . . H21C H 0.5010 0.9582 0.0561 0.154 Uiso 1 calc R . . O8 O 0.6381(6) 0.8778(5) 0.3156(5) 0.075(3) Uani 1 d . . . C22 C 0.6579(11) 0.9487(9) 0.3391(8) 0.077(4) Uiso 1 d . . . H22 H 0.6983 0.9780 0.3204 0.092 Uiso 1 calc R . . N8 N 0.6279(9) 0.9876(7) 0.3881(7) 0.076(3) Uiso 1 d . . . C23 C 0.6547(14) 1.0762(12) 0.4110(11) 0.119(7) Uiso 1 d . . . H23A H 0.6268 1.0954 0.4482 0.178 Uiso 1 calc R . . H23B H 0.6374 1.1062 0.3691 0.178 Uiso 1 calc R . . H23C H 0.7175 1.0846 0.4304 0.178 Uiso 1 calc R . . C24 C 0.5639(16) 0.9523(14) 0.4175(12) 0.141(8) Uiso 1 d . . . H24A H 0.5512 0.9918 0.4534 0.212 Uiso 1 calc R . . H24B H 0.5849 0.9052 0.4408 0.212 Uiso 1 calc R . . H24C H 0.5113 0.9354 0.3789 0.212 Uiso 1 calc R . . O9 O 0.6417(7) 0.6873(5) 0.2959(7) 0.094(4) Uani 1 d . . . C25 C 0.6498(11) 0.6155(10) 0.3032(8) 0.078(4) Uiso 1 d . . . H25 H 0.6127 0.5760 0.2686 0.094 Uiso 1 calc R . . N9 N 0.7078(7) 0.5908(6) 0.3569(5) 0.057(3) Uiso 1 d . . . C26 C 0.7177(13) 0.5063(11) 0.3669(10) 0.106(6) Uiso 1 d . . . H26A H 0.7643 0.5029 0.4102 0.159 Uiso 1 calc R . . H26B H 0.7319 0.4790 0.3247 0.159 Uiso 1 calc R . . H26C H 0.6638 0.4802 0.3724 0.159 Uiso 1 calc R . . C27 C 0.7646(19) 0.6528(16) 0.4076(14) 0.172(11) Uiso 1 d . . . H27A H 0.8042 0.6276 0.4448 0.258 Uiso 1 calc R . . H27B H 0.7303 0.6879 0.4304 0.258 Uiso 1 calc R . . H27C H 0.7978 0.6850 0.3821 0.258 Uiso 1 calc R . . O10 O 0.4095(6) 0.8487(5) 0.2332(5) 0.063(2) Uani 1 d . . . C28 C 0.4133(8) 0.9108(7) 0.2041(6) 0.052(3) Uiso 1 d . . . H28 H 0.4655 0.9453 0.2201 0.062 Uiso 1 calc R . . N10 N 0.3523(7) 0.9336(6) 0.1533(5) 0.055(3) Uiso 1 d . . . C29 C 0.3573(10) 1.0106(9) 0.1219(8) 0.076(4) Uiso 1 d . . . H29A H 0.3039 1.0137 0.0845 0.113 Uiso 1 calc R . . H29B H 0.4064 1.0133 0.1004 0.113 Uiso 1 calc R . . H29C H 0.3650 1.0558 0.1598 0.113 Uiso 1 calc R . . C30 C 0.2695(14) 0.8856(13) 0.1241(11) 0.122(7) Uiso 1 d . . . H30A H 0.2331 0.9126 0.0863 0.182 Uiso 1 calc R . . H30B H 0.2409 0.8796 0.1628 0.182 Uiso 1 calc R . . H30C H 0.2789 0.8321 0.1035 0.182 Uiso 1 calc R . . O11 O 0.4222(6) 0.6566(5) 0.2104(5) 0.071(3) Uani 1 d . . . C31 C 0.3931(14) 0.5902(12) 0.1721(11) 0.110(6) Uiso 1 d . . . H31 H 0.3415 0.5656 0.1793 0.132 Uiso 1 calc R . . N11 N 0.4227(8) 0.5523(7) 0.1260(6) 0.064(3) Uiso 1 d . . . C32 C 0.5077(14) 0.5801(12) 0.1156(11) 0.115(6) Uiso 1 d . . . H32A H 0.5205 0.5439 0.0775 0.173 Uiso 1 calc R . . H32B H 0.5525 0.5799 0.1608 0.173 Uiso 1 calc R . . H32C H 0.5062 0.6350 0.1017 0.173 Uiso 1 calc R . . C33 C 0.3917(16) 0.4725(13) 0.0880(12) 0.133(8) Uiso 1 d . . . H33A H 0.4272 0.4582 0.0551 0.199 Uiso 1 calc R . . H33B H 0.3316 0.4724 0.0602 0.199 Uiso 1 calc R . . H33C H 0.3953 0.4330 0.1229 0.199 Uiso 1 calc R . . O12 O 0.4724(7) 0.7449(6) 0.3638(5) 0.076(3) Uani 1 d . . . C34 C 0.4820(15) 0.6773(14) 0.3866(13) 0.123(7) Uiso 1 d . . . H34 H 0.4750 0.6300 0.3534 0.147 Uiso 1 calc R . . N12 N 0.5016(10) 0.6718(10) 0.4563(9) 0.099(4) Uiso 1 d . . . C35 C 0.513(3) 0.737(2) 0.5084(19) 0.240(16) Uiso 1 d . . . H35A H 0.5276 0.7182 0.5564 0.360 Uiso 1 calc R . . H35B H 0.4605 0.7641 0.5016 0.360 Uiso 1 calc R . . H35C H 0.5609 0.7748 0.5044 0.360 Uiso 1 calc R . . C36 C 0.516(3) 0.598(3) 0.483(2) 0.30(2) Uiso 1 d . . . H36A H 0.5303 0.6057 0.5354 0.446 Uiso 1 calc R . . H36B H 0.5649 0.5767 0.4673 0.446 Uiso 1 calc R . . H36C H 0.4647 0.5602 0.4636 0.446 Uiso 1 calc R . . O13 O 0.2105(7) 0.7150(8) 0.1825(7) 0.104(4) Uani 1 d . . . C37 C 0.1434(15) 0.6771(12) 0.1841(12) 0.114(6) Uiso 1 d . . . H37 H 0.1242 0.6853 0.2266 0.137 Uiso 1 calc R . . N13 N 0.0957(9) 0.6251(7) 0.1299(7) 0.076(3) Uiso 1 d . . . C38 C 0.0198(17) 0.5889(14) 0.1466(13) 0.146(9) Uiso 1 d . . . H38A H 0.0171 0.6124 0.1944 0.218 Uiso 1 calc R . . H38B H 0.0227 0.5305 0.1464 0.218 Uiso 1 calc R . . H38C H -0.0319 0.5994 0.1103 0.218 Uiso 1 calc R . . C39 C 0.1136(18) 0.6042(15) 0.0690(13) 0.155(9) Uiso 1 d . . . H39A H 0.0676 0.5650 0.0388 0.232 Uiso 1 calc R . . H39B H 0.1684 0.5799 0.0784 0.232 Uiso 1 calc R . . H39C H 0.1182 0.6520 0.0440 0.232 Uiso 1 calc R . . O14 O 0.2739(8) 0.7014(6) 0.3551(6) 0.088(3) Uani 1 d . . . C40 C 0.2495(10) 0.6602(9) 0.3967(8) 0.068(4) Uiso 1 d . . . H40 H 0.2445 0.6869 0.4410 0.082 Uiso 1 calc R . . N14 N 0.2296(8) 0.5809(7) 0.3842(6) 0.067(3) Uiso 1 d . . . C41 C 0.1926(15) 0.5353(13) 0.4349(11) 0.125(7) Uiso 1 d . . . H41A H 0.1828 0.4778 0.4169 0.187 Uiso 1 calc R . . H41B H 0.1378 0.5556 0.4378 0.187 Uiso 1 calc R . . H41C H 0.2332 0.5430 0.4829 0.187 Uiso 1 calc R . . C42 C 0.2301(14) 0.5338(12) 0.3197(10) 0.113(6) Uiso 1 d . . . H42A H 0.2135 0.4771 0.3229 0.170 Uiso 1 calc R . . H42B H 0.2881 0.5392 0.3122 0.170 Uiso 1 calc R . . H42C H 0.1891 0.5525 0.2790 0.170 Uiso 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 Pb1 0.0343(3) 0.0409(2) 0.0468(2) 0.00643(18) 0.01280(18) 0.00479(18) Pb2 0.0310(2) 0.0430(2) 0.0453(2) 0.00271(17) 0.00899(16) 0.00225(16) Pb3 0.0307(3) 0.0447(2) 0.0490(2) 0.00013(18) 0.00990(18) -0.00054(18) Pb4 0.0321(2) 0.0408(2) 0.0456(2) 0.00187(17) 0.01160(16) 0.00317(16) I1 0.0574(6) 0.0432(4) 0.0594(5) 0.0145(4) 0.0136(4) 0.0063(4) I2 0.0581(6) 0.0661(5) 0.0425(4) 0.0038(4) 0.0129(4) 0.0017(4) I3 0.0480(5) 0.0401(4) 0.0496(4) 0.0015(3) 0.0058(3) 0.0015(3) I4 0.0523(6) 0.0485(5) 0.0624(5) -0.0125(4) 0.0146(4) -0.0006(4) I5 0.0432(5) 0.0556(5) 0.0666(5) 0.0197(4) 0.0109(4) 0.0017(4) I6 0.0517(5) 0.0498(4) 0.0405(4) -0.0028(3) 0.0081(3) -0.0013(4) I7 0.0439(5) 0.0576(5) 0.0747(6) 0.0233(4) 0.0183(4) 0.0099(4) I8 0.0517(5) 0.0618(5) 0.0417(4) -0.0039(4) 0.0106(4) -0.0003(4) I9 0.0521(6) 0.0450(4) 0.0704(6) -0.0115(4) 0.0092(4) -0.0005(4) I10 0.0515(5) 0.0422(4) 0.0506(4) 0.0107(3) 0.0143(4) 0.0097(4) I11 0.0588(6) 0.0683(5) 0.0419(4) 0.0058(4) 0.0178(4) 0.0118(4) I12 0.0545(6) 0.0357(4) 0.0632(5) -0.0026(4) 0.0098(4) 0.0013(3) Na1 0.056(3) 0.042(2) 0.036(2) 0.0048(18) 0.014(2) -0.002(2) Na2 0.049(3) 0.047(3) 0.055(3) 0.009(2) 0.015(2) -0.005(2) Na3 0.044(3) 0.045(3) 0.072(3) 0.020(2) 0.012(2) 0.004(2) Na4 0.050(3) 0.064(3) 0.072(3) 0.017(3) 0.018(3) 0.003(2) O1 0.116(9) 0.073(6) 0.055(5) 0.014(5) 0.042(6) 0.019(6) O2 0.045(5) 0.057(5) 0.077(6) 0.000(4) 0.016(4) -0.014(4) O3 0.080(7) 0.059(5) 0.062(5) 0.023(4) 0.009(5) 0.013(5) O4 0.086(8) 0.068(6) 0.072(6) 0.034(5) 0.016(5) -0.013(5) O5 0.061(6) 0.049(5) 0.064(5) -0.006(4) 0.022(4) 0.001(4) O6 0.061(6) 0.068(6) 0.044(5) -0.014(4) 0.015(4) -0.010(4) O7 0.079(7) 0.059(5) 0.062(5) 0.022(4) 0.021(5) 0.004(5) O8 0.072(7) 0.053(5) 0.090(7) -0.012(5) 0.015(5) -0.008(5) O9 0.074(7) 0.052(6) 0.182(11) 0.075(7) 0.051(7) 0.026(5) O10 0.062(6) 0.041(5) 0.087(6) 0.031(4) 0.012(5) 0.015(4) O11 0.071(7) 0.049(5) 0.087(7) -0.019(5) 0.023(5) -0.009(5) O12 0.080(7) 0.082(7) 0.068(6) 0.033(5) 0.016(5) -0.001(5) O13 0.056(7) 0.128(10) 0.128(10) 0.045(8) 0.023(6) -0.027(7) O14 0.106(9) 0.069(6) 0.108(8) 0.033(6) 0.054(7) 0.013(6) _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 Pb1 I2 3.1974(10) . ? Pb1 I10 3.2274(10) 1_455 ? Pb1 I12 3.2280(10) 1_455 ? Pb1 I1 3.2467(10) . ? Pb1 I11 3.2670(10) 1_455 ? Pb1 I3 3.2757(10) . ? Pb2 I6 3.2049(10) . ? Pb2 I1 3.2107(10) . ? Pb2 I3 3.2316(10) . ? Pb2 I2 3.2354(10) . ? Pb2 I5 3.2393(10) . ? Pb2 I4 3.2531(10) . ? Pb3 I7 3.1828(11) . ? Pb3 I4 3.1913(10) . ? Pb3 I6 3.2189(10) . ? Pb3 I5 3.2298(10) . ? Pb3 I8 3.2535(10) . ? Pb3 I9 3.3022(10) . ? Pb4 I11 3.1839(10) . ? Pb4 I7 3.1975(10) . ? Pb4 I10 3.2303(10) . ? Pb4 I9 3.2436(10) . ? Pb4 I8 3.2514(10) . ? Pb4 I12 3.2732(10) . ? I10 Pb1 3.2274(10) 1_655 ? I11 Pb1 3.2670(10) 1_655 ? I12 Pb1 3.2280(10) 1_655 ? Na1 O1 2.278(9) . ? Na1 O3 2.305(9) . ? Na1 O2 2.339(9) . ? Na1 O5 2.401(9) . ? Na1 O6 2.403(9) . ? Na1 O4 2.655(11) . ? Na1 Na2 3.210(7) . ? Na2 O4 2.270(9) . ? Na2 O5 2.348(10) . ? Na2 O9 2.351(10) . ? Na2 O8 2.419(11) . ? Na2 O7 2.427(10) . ? Na2 O6 2.474(9) . ? Na2 Na3 3.131(7) . ? Na3 O9 2.296(10) . ? Na3 O12 2.322(11) . ? Na3 O8 2.370(10) . ? Na3 O7 2.372(10) . ? Na3 O11 2.390(10) . ? Na3 O10 2.394(9) . ? Na3 C34 3.08(2) . ? Na3 Na4 3.084(7) . ? Na4 O14 2.239(11) . ? Na4 O13 2.245(12) . ? Na4 O10 2.346(9) . ? Na4 O11 2.373(11) . ? Na4 O12 2.423(11) . ? Na4 C34 3.08(2) . ? O1 C1 1.206(15) . ? C1 N1 1.331(14) . ? N1 C3 1.397(15) . ? N1 C2 1.454(15) . ? O2 C4 1.225(14) . ? C4 N2 1.292(14) . ? N2 C5 1.441(16) . ? N2 C6 1.450(17) . ? O3 C7 1.214(16) . ? C7 N3 1.325(17) . ? N3 C9 1.40(3) . ? N3 C8 1.44(2) . ? O4 C10 1.243(15) . ? C10 N4 1.301(14) . ? N4 C12 1.402(19) . ? N4 C11 1.435(19) . ? O5 C13 1.204(13) . ? C13 N5 1.316(14) . ? N5 C15 1.438(19) . ? N5 C14 1.465(16) . ? O6 C16 1.226(13) . ? C16 N6 1.301(14) . ? N6 C17 1.414(15) . ? N6 C18 1.487(17) . ? O7 C19 1.223(15) . ? C19 N7 1.296(18) . ? N7 C20 1.36(2) . ? N7 C21 1.462(19) . ? O8 C22 1.208(16) . ? C22 N8 1.294(18) . ? N8 C24 1.40(2) . ? N8 C23 1.49(2) . ? O9 C25 1.220(16) . ? C25 N9 1.312(17) . ? N9 C27 1.43(3) . ? N9 C26 1.442(19) . ? O10 C28 1.218(13) . ? C28 N10 1.293(15) . ? N10 C30 1.44(2) . ? N10 C29 1.463(16) . ? O11 C31 1.25(2) . ? C31 N11 1.24(2) . ? N11 C33 1.44(2) . ? N11 C32 1.47(2) . ? O12 C34 1.24(2) . ? C34 N12 1.30(2) . ? N12 C35 1.37(3) . ? N12 C36 1.37(4) . ? O13 C37 1.21(2) . ? C37 N13 1.32(2) . ? N13 C39 1.29(2) . ? N13 C38 1.43(2) . ? O14 C40 1.211(16) . ? C40 N14 1.315(16) . ? N14 C42 1.396(19) . ? N14 C41 1.49(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 I2 Pb1 I10 89.13(3) . 1_455 ? I2 Pb1 I12 95.65(3) . 1_455 ? I10 Pb1 I12 85.83(2) 1_455 1_455 ? I2 Pb1 I1 87.92(3) . . ? I10 Pb1 I1 175.28(2) 1_455 . ? I12 Pb1 I1 98.13(3) 1_455 . ? I2 Pb1 I11 176.98(3) . 1_455 ? I10 Pb1 I11 88.83(3) 1_455 1_455 ? I12 Pb1 I11 81.98(3) 1_455 1_455 ? I1 Pb1 I11 94.26(3) . 1_455 ? I2 Pb1 I3 84.69(3) . . ? I10 Pb1 I3 91.95(2) 1_455 . ? I12 Pb1 I3 177.74(3) 1_455 . ? I1 Pb1 I3 84.11(2) . . ? I11 Pb1 I3 97.60(3) 1_455 . ? I6 Pb2 I1 93.16(3) . . ? I6 Pb2 I3 95.70(2) . . ? I1 Pb2 I3 85.41(2) . . ? I6 Pb2 I2 178.87(3) . . ? I1 Pb2 I2 87.89(3) . . ? I3 Pb2 I2 84.80(3) . . ? I6 Pb2 I5 86.04(3) . . ? I1 Pb2 I5 178.91(3) . . ? I3 Pb2 I5 93.93(2) . . ? I2 Pb2 I5 92.92(3) . . ? I6 Pb2 I4 84.00(3) . . ? I1 Pb2 I4 94.18(3) . . ? I3 Pb2 I4 179.48(3) . . ? I2 Pb2 I4 95.52(3) . . ? I5 Pb2 I4 86.47(3) . . ? I7 Pb3 I4 90.87(3) . . ? I7 Pb3 I6 90.21(3) . . ? I4 Pb3 I6 84.77(3) . . ? I7 Pb3 I5 176.02(3) . . ? I4 Pb3 I5 87.68(3) . . ? I6 Pb3 I5 85.97(2) . . ? I7 Pb3 I8 87.23(3) . . ? I4 Pb3 I8 94.32(3) . . ? I6 Pb3 I8 177.28(3) . . ? I5 Pb3 I8 96.57(3) . . ? I7 Pb3 I9 87.07(3) . . ? I4 Pb3 I9 177.06(3) . . ? I6 Pb3 I9 97.32(3) . . ? I5 Pb3 I9 94.52(3) . . ? I8 Pb3 I9 83.50(3) . . ? I11 Pb4 I7 89.34(3) . . ? I11 Pb4 I10 90.24(3) . . ? I7 Pb4 I10 179.21(3) . . ? I11 Pb4 I9 97.34(3) . . ? I7 Pb4 I9 87.83(3) . . ? I10 Pb4 I9 91.56(3) . . ? I11 Pb4 I8 175.88(3) . . ? I7 Pb4 I8 87.02(3) . . ? I10 Pb4 I8 93.42(3) . . ? I9 Pb4 I8 84.46(3) . . ? I11 Pb4 I12 82.56(3) . . ? I7 Pb4 I12 95.58(3) . . ? I10 Pb4 I12 85.04(2) . . ? I9 Pb4 I12 176.59(3) . . ? I8 Pb4 I12 95.87(3) . . ? Pb2 I1 Pb1 76.44(2) . . ? Pb1 I2 Pb2 76.78(2) . . ? Pb2 I3 Pb1 75.75(2) . . ? Pb3 I4 Pb2 76.34(2) . . ? Pb3 I5 Pb2 76.00(2) . . ? Pb2 I6 Pb3 76.63(2) . . ? Pb3 I7 Pb4 77.13(2) . . ? Pb4 I8 Pb3 75.39(2) . . ? Pb4 I9 Pb3 74.83(2) . . ? Pb1 I10 Pb4 76.48(2) 1_655 . ? Pb4 I11 Pb1 76.56(2) . 1_655 ? Pb1 I12 Pb4 75.87(2) 1_655 . ? O1 Na1 O3 99.1(4) . . ? O1 Na1 O2 90.6(4) . . ? O3 Na1 O2 103.1(4) . . ? O1 Na1 O5 93.7(4) . . ? O3 Na1 O5 88.4(3) . . ? O2 Na1 O5 167.0(4) . . ? O1 Na1 O6 160.1(4) . . ? O3 Na1 O6 100.4(3) . . ? O2 Na1 O6 88.7(3) . . ? O5 Na1 O6 83.1(3) . . ? O1 Na1 O4 85.5(4) . . ? O3 Na1 O4 165.6(4) . . ? O2 Na1 O4 90.5(3) . . ? O5 Na1 O4 77.7(3) . . ? O6 Na1 O4 74.6(3) . . ? O1 Na1 Na2 115.0(3) . . ? O3 Na1 Na2 122.3(3) . . ? O2 Na1 Na2 120.5(3) . . ? O5 Na1 Na2 46.8(2) . . ? O6 Na1 Na2 49.8(2) . . ? O4 Na1 Na2 44.3(2) . . ? O4 Na2 O5 86.9(4) . . ? O4 Na2 O9 170.6(5) . . ? O5 Na2 O9 87.1(3) . . ? O4 Na2 O8 104.8(4) . . ? O5 Na2 O8 164.3(4) . . ? O9 Na2 O8 82.5(4) . . ? O4 Na2 O7 95.5(3) . . ? O5 Na2 O7 112.4(4) . . ? O9 Na2 O7 80.1(4) . . ? O8 Na2 O7 77.3(3) . . ? O4 Na2 O6 80.6(3) . . ? O5 Na2 O6 82.7(3) . . ? O9 Na2 O6 105.8(4) . . ? O8 Na2 O6 88.9(3) . . ? O7 Na2 O6 164.2(4) . . ? O4 Na2 Na3 134.7(3) . . ? O5 Na2 Na3 128.4(3) . . ? O9 Na2 Na3 46.9(3) . . ? O8 Na2 Na3 48.5(2) . . ? O7 Na2 Na3 48.5(2) . . ? O6 Na2 Na3 125.6(3) . . ? O4 Na2 Na1 54.7(3) . . ? O5 Na2 Na1 48.2(2) . . ? O9 Na2 Na1 124.5(3) . . ? O8 Na2 Na1 131.4(3) . . ? O7 Na2 Na1 140.1(3) . . ? O6 Na2 Na1 47.9(2) . . ? Na3 Na2 Na1 170.11(19) . . ? O9 Na3 O12 95.9(4) . . ? O9 Na3 O8 84.8(4) . . ? O12 Na3 O8 102.9(4) . . ? O9 Na3 O7 82.4(4) . . ? O12 Na3 O7 177.1(4) . . ? O8 Na3 O7 79.3(4) . . ? O9 Na3 O11 94.6(4) . . ? O12 Na3 O11 80.0(4) . . ? O8 Na3 O11 177.1(4) . . ? O7 Na3 O11 97.7(4) . . ? O9 Na3 O10 178.4(4) . . ? O12 Na3 O10 83.9(4) . . ? O8 Na3 O10 96.8(3) . . ? O7 Na3 O10 97.7(3) . . ? O11 Na3 O10 83.8(3) . . ? O9 Na3 C34 77.7(5) . . ? O12 Na3 C34 21.2(5) . . ? O8 Na3 C34 111.5(5) . . ? O7 Na3 C34 156.1(5) . . ? O11 Na3 C34 71.2(5) . . ? O10 Na3 C34 101.8(5) . . ? O9 Na3 Na4 130.1(3) . . ? O12 Na3 Na4 50.9(3) . . ? O8 Na3 Na4 132.8(3) . . ? O7 Na3 Na4 128.7(3) . . ? O11 Na3 Na4 49.4(3) . . ? O10 Na3 Na4 48.7(2) . . ? C34 Na3 Na4 59.9(4) . . ? O9 Na3 Na2 48.4(3) . . ? O12 Na3 Na2 130.2(3) . . ? O8 Na3 Na2 49.9(3) . . ? O7 Na3 Na2 50.0(3) . . ? O11 Na3 Na2 127.9(3) . . ? O10 Na3 Na2 132.7(3) . . ? C34 Na3 Na2 120.1(5) . . ? Na4 Na3 Na2 177.3(2) . . ? O14 Na4 O13 91.9(5) . . ? O14 Na4 O10 142.9(4) . . ? O13 Na4 O10 103.3(4) . . ? O14 Na4 O11 126.2(4) . . ? O13 Na4 O11 98.5(5) . . ? O10 Na4 O11 85.2(3) . . ? O14 Na4 O12 85.0(4) . . ? O13 Na4 O12 173.0(4) . . ? O10 Na4 O12 82.7(3) . . ? O11 Na4 O12 78.4(4) . . ? O14 Na4 C34 74.2(5) . . ? O13 Na4 C34 150.7(6) . . ? O10 Na4 C34 103.1(5) . . ? O11 Na4 C34 71.4(5) . . ? O12 Na4 C34 22.3(4) . . ? O14 Na4 Na3 132.8(4) . . ? O13 Na4 Na3 133.9(4) . . ? O10 Na4 Na3 50.1(2) . . ? O11 Na4 Na3 49.9(2) . . ? O12 Na4 Na3 48.1(3) . . ? C34 Na4 Na3 60.0(4) . . ? C1 O1 Na1 129.7(9) . . ? O1 C1 N1 124.3(12) . . ? C1 N1 C3 121.6(11) . . ? C1 N1 C2 121.8(10) . . ? C3 N1 C2 116.5(10) . . ? C4 O2 Na1 154.1(9) . . ? O2 C4 N2 127.6(12) . . ? C4 N2 C5 122.6(10) . . ? C4 N2 C6 120.3(11) . . ? C5 N2 C6 117.0(12) . . ? C7 O3 Na1 133.4(10) . . ? O3 C7 N3 124.7(14) . . ? C7 N3 C9 121.1(16) . . ? C7 N3 C8 122.0(14) . . ? C9 N3 C8 116.7(16) . . ? C10 O4 Na2 159.8(10) . . ? C10 O4 Na1 110.9(9) . . ? Na2 O4 Na1 81.0(3) . . ? O4 C10 N4 124.4(13) . . ? C10 N4 C12 121.7(12) . . ? C10 N4 C11 120.7(12) . . ? C12 N4 C11 117.4(13) . . ? C13 O5 Na2 149.6(9) . . ? C13 O5 Na1 122.7(8) . . ? Na2 O5 Na1 85.1(3) . . ? O5 C13 N5 128.0(12) . . ? C13 N5 C15 119.2(12) . . ? C13 N5 C14 123.0(11) . . ? C15 N5 C14 117.8(11) . . ? C16 O6 Na1 115.5(8) . . ? C16 O6 Na2 121.2(8) . . ? Na1 O6 Na2 82.3(3) . . ? O6 C16 N6 127.4(12) . . ? C16 N6 C17 124.2(10) . . ? C16 N6 C18 119.5(11) . . ? C17 N6 C18 116.2(10) . . ? C19 O7 Na3 125.7(9) . . ? C19 O7 Na2 118.0(9) . . ? Na3 O7 Na2 81.4(3) . . ? O7 C19 N7 125.3(15) . . ? C19 N7 C20 122.5(15) . . ? C19 N7 C21 120.5(14) . . ? C20 N7 C21 117.0(14) . . ? C22 O8 Na3 149.8(10) . . ? C22 O8 Na2 126.1(10) . . ? Na3 O8 Na2 81.6(3) . . ? O8 C22 N8 125.1(16) . . ? C22 N8 C24 123.1(16) . . ? C22 N8 C23 120.3(15) . . ? C24 N8 C23 116.4(16) . . ? C25 O9 Na3 137.1(11) . . ? C25 O9 Na2 134.1(10) . . ? Na3 O9 Na2 84.7(3) . . ? O9 C25 N9 123.4(15) . . ? C25 N9 C27 116.7(15) . . ? C25 N9 C26 124.2(13) . . ? C27 N9 C26 119.1(16) . . ? C28 O10 Na4 154.5(9) . . ? C28 O10 Na3 123.4(8) . . ? Na4 O10 Na3 81.2(3) . . ? O10 C28 N10 126.0(12) . . ? C28 N10 C30 122.1(13) . . ? C28 N10 C29 124.6(12) . . ? C30 N10 C29 113.2(13) . . ? C31 O11 Na4 123.5(12) . . ? C31 O11 Na3 155.8(12) . . ? Na4 O11 Na3 80.7(3) . . ? N11 C31 O11 129(2) . . ? C31 N11 C33 127.4(17) . . ? C31 N11 C32 120.3(16) . . ? C33 N11 C32 111.2(15) . . ? C34 O12 Na3 116.2(13) . . ? C34 O12 Na4 109.9(12) . . ? Na3 O12 Na4 81.0(3) . . ? O12 C34 N12 120(2) . . ? O12 C34 Na4 47.8(10) . . ? N12 C34 Na4 139.0(15) . . ? O12 C34 Na3 42.6(10) . . ? N12 C34 Na3 144.6(16) . . ? Na4 C34 Na3 60.1(4) . . ? C34 N12 C35 124(2) . . ? C34 N12 C36 121(3) . . ? C35 N12 C36 115(3) . . ? C37 O13 Na4 128.9(13) . . ? O13 C37 N13 124(2) . . ? C39 N13 C37 126(2) . . ? C39 N13 C38 121.4(19) . . ? C37 N13 C38 112.3(17) . . ? C40 O14 Na4 160.5(10) . . ? O14 C40 N14 124.4(14) . . ? C40 N14 C42 124.1(14) . . ? C40 N14 C41 121.4(13) . . ? C42 N14 C41 113.9(14) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.100 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.156 #===END data_263 _database_code_CSD 153707 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 I6 N2 Pb2' _chemical_formula_weight 1374.13 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' 'I' 'I' -0.4742 1.8119 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhomic _symmetry_space_group_name_H-M 'P2(1)2(1)2' #No. 18) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 29.662(4) _cell_length_b 20.711(3) _cell_length_c 9.0290(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5546.8(13) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4752 _exptl_absorpt_coefficient_mu 18.803 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50976 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9773 _reflns_number_gt 8129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _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^)+(0.0548P)^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 'idealized positions' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(5) _refine_ls_number_reflns 9773 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _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 Pb1 Pb 0.170293(19) 0.33825(3) 0.31721(6) 0.04830(14) Uani 1 1 d . . . Pb2 Pb 0.192278(18) 0.25131(3) 0.74169(6) 0.04739(14) Uani 1 1 d . . . Pb3 Pb 0.03995(2) 0.28467(3) 0.80100(6) 0.05437(16) Uani 1 1 d . . . Pb4 Pb 0.06431(2) 0.18547(3) 1.22390(6) 0.05162(15) Uani 1 1 d . . . I1 I 0.11788(4) 0.37578(6) 0.63591(12) 0.0659(3) Uani 1 1 d . . . I2 I 0.15116(4) 0.18147(6) 0.44149(12) 0.0630(3) Uani 1 1 d . . . I3 I 0.08074(4) 0.34304(6) 1.10672(12) 0.0616(3) Uani 1 1 d . . . I4 I 0.12111(4) 0.16325(6) 0.92069(13) 0.0666(3) Uani 1 1 d . . . I5 I 0.25806(3) 0.32441(7) 0.51252(12) 0.0651(3) Uani 1 1 d . . . I6 I 0.23265(4) 0.31105(6) 1.03815(11) 0.0635(3) Uani 1 1 d . . . I7 I 0.17890(4) 0.48063(5) 0.27209(14) 0.0661(3) Uani 1 1 d . . . I8 I 0.25863(5) 0.14419(7) 0.75395(15) 0.0805(4) Uani 1 1 d . . . I9 I -0.02044(4) 0.19158(7) 1.00115(12) 0.0646(3) Uani 1 1 d . . . I10 I 0.00188(4) 0.22194(6) 0.50401(11) 0.0630(3) Uani 1 1 d . . . I11 I -0.03103(4) 0.39032(7) 0.79777(12) 0.0720(3) Uani 1 1 d . . . I12 I 0.06363(7) 0.04143(7) 1.25657(14) 0.0985(5) Uani 1 1 d . . . N1 N 0.2432(5) 0.0143(8) 0.2174(18) 0.069(4) Uiso 1 1 d . . . N2 N 0.2997(6) 0.1079(9) 0.240(2) 0.083(4) Uiso 1 1 d . . . C1 C 0.2842(11) -0.0004(19) 0.143(4) 0.150(12) Uiso 1 1 d . . . H1A H 0.2774 -0.0166 0.0449 0.180 Uiso 1 1 calc R . . H1B H 0.2999 -0.0341 0.1970 0.180 Uiso 1 1 calc R . . C2 C 0.3156(8) 0.0603(13) 0.130(3) 0.099(7) Uiso 1 1 d . . . H2A H 0.3466 0.0484 0.1502 0.119 Uiso 1 1 calc R . . H2B H 0.3139 0.0783 0.0311 0.119 Uiso 1 1 calc R . . C3 C 0.2242(9) 0.0769(13) 0.155(3) 0.108(8) Uiso 1 1 d . . . H3A H 0.1944 0.0848 0.1952 0.130 Uiso 1 1 calc R . . H3B H 0.2216 0.0736 0.0477 0.130 Uiso 1 1 calc R . . C4 C 0.2558(9) 0.1323(14) 0.195(3) 0.113(8) Uiso 1 1 d . . . H4A H 0.2594 0.1607 0.1104 0.136 Uiso 1 1 calc R . . H4B H 0.2428 0.1572 0.2753 0.136 Uiso 1 1 calc R . . C5 C 0.2552(8) 0.0301(13) 0.372(3) 0.100(7) Uiso 1 1 d . . . H5A H 0.2297 0.0512 0.4191 0.120 Uiso 1 1 calc R . . H5B H 0.2610 -0.0097 0.4255 0.120 Uiso 1 1 calc R . . C6 C 0.2937(9) 0.0709(15) 0.383(3) 0.113(8) Uiso 1 1 d . . . H6A H 0.3203 0.0450 0.4019 0.136 Uiso 1 1 calc R . . H6B H 0.2899 0.1009 0.4643 0.136 Uiso 1 1 calc R . . C7 C 0.1984(14) -0.038(2) 0.254(5) 0.185(16) Uiso 1 1 d . . . H7A H 0.2085 -0.0761 0.3073 0.222 Uiso 1 1 calc R . . H7B H 0.1749 -0.0169 0.3105 0.222 Uiso 1 1 calc R . . C8 C 0.185(3) -0.053(4) 0.126(10) 0.34(4) Uiso 1 1 d . . . H8A H 0.2088 -0.0703 0.0655 0.406 Uiso 1 1 calc R . . H8B H 0.1713 -0.0160 0.0763 0.406 Uiso 1 1 calc R . . C9 C 0.1467(15) -0.108(2) 0.170(5) 0.204(19) Uiso 1 1 d . . . H9A H 0.1310 -0.1218 0.0821 0.306 Uiso 1 1 calc R . . H9B H 0.1255 -0.0906 0.2392 0.306 Uiso 1 1 calc R . . H9C H 0.1615 -0.1449 0.2138 0.306 Uiso 1 1 calc R . . C10 C 0.3312(13) 0.169(2) 0.278(4) 0.166(14) Uiso 1 1 d . . . H10A H 0.3137 0.1976 0.3424 0.199 Uiso 1 1 calc R . . H10B H 0.3563 0.1536 0.3370 0.199 Uiso 1 1 calc R . . C11 C 0.3519(18) 0.214(3) 0.151(7) 0.25(2) Uiso 1 1 d . . . H11A H 0.3752 0.1921 0.0940 0.295 Uiso 1 1 calc R . . H11B H 0.3292 0.2317 0.0856 0.295 Uiso 1 1 calc R . . C12 C 0.3704(12) 0.262(2) 0.261(5) 0.165(14) Uiso 1 1 d . . . H12A H 0.3844 0.2972 0.2091 0.247 Uiso 1 1 calc R . . H12B H 0.3922 0.2414 0.3238 0.247 Uiso 1 1 calc R . . H12C H 0.3462 0.2785 0.3212 0.247 Uiso 1 1 calc R . . N3 N 0.4557(6) 0.4952(10) 0.261(2) 0.093(5) Uiso 1 1 d . . . C13 C 0.4741(6) 0.5602(10) 0.328(2) 0.077(5) Uiso 1 1 d . . . H13A H 0.4669 0.5956 0.2613 0.093 Uiso 1 1 calc R . . H13B H 0.4594 0.5685 0.4218 0.093 Uiso 1 1 calc R . . C14 C 0.4764(6) 0.4424(9) 0.350(2) 0.066(4) Uiso 1 1 d . . . H14A H 0.4700 0.4496 0.4543 0.079 Uiso 1 1 calc R . . H14B H 0.4632 0.4014 0.3219 0.079 Uiso 1 1 calc R . . C15 C 0.4784(9) 0.4960(19) 0.116(4) 0.139(11) Uiso 1 1 d . . . H15A H 0.4719 0.4555 0.0662 0.167 Uiso 1 1 calc R . . H15B H 0.4651 0.5302 0.0568 0.167 Uiso 1 1 calc R . . C16 C 0.3997(8) 0.5022(15) 0.323(3) 0.105(8) Uiso 1 1 d . . . H16A H 0.3988 0.5034 0.4306 0.126 Uiso 1 1 calc R . . H16B H 0.3863 0.5417 0.2857 0.126 Uiso 1 1 calc R . . C17 C 0.3786(19) 0.455(3) 0.277(8) 0.27(3) Uiso 1 1 d . . . H17A H 0.3842 0.4179 0.3408 0.328 Uiso 1 1 calc R . . H17B H 0.3890 0.4437 0.1780 0.328 Uiso 1 1 calc R . . C18 C 0.3295(10) 0.4683(15) 0.272(4) 0.132(10) Uiso 1 1 d . . . H18A H 0.3132 0.4313 0.3073 0.197 Uiso 1 1 calc R . . H18B H 0.3206 0.4776 0.1723 0.197 Uiso 1 1 calc R . . H18C H 0.3229 0.5047 0.3343 0.197 Uiso 1 1 calc R . . N4 N 0.0328(6) 0.5459(9) 0.334(2) 0.084(5) Uiso 1 1 d . . . C19 C 0.0469(7) 0.4902(12) 0.421(3) 0.090(6) Uiso 1 1 d . . . H19A H 0.0475 0.5017 0.5254 0.108 Uiso 1 1 calc R . . H19B H 0.0771 0.4773 0.3925 0.108 Uiso 1 1 calc R . . C20 C -0.0108(7) 0.5724(12) 0.395(3) 0.092(6) Uiso 1 1 d . . . H20A H -0.0237 0.6031 0.3256 0.110 Uiso 1 1 calc R . . H20B H -0.0052 0.5944 0.4877 0.110 Uiso 1 1 calc R . . C21 C 0.0166(9) 0.5193(15) 0.185(3) 0.128(10) Uiso 1 1 d . . . H21A H 0.0089 0.5558 0.1222 0.154 Uiso 1 1 calc R . . H21B H 0.0419 0.4975 0.1382 0.154 Uiso 1 1 calc R . . C22 C 0.0705(11) 0.5958(17) 0.344(4) 0.136(11) Uiso 1 1 d . . . H22A H 0.0716 0.6118 0.4453 0.164 Uiso 1 1 calc R . . H22B H 0.0990 0.5745 0.3244 0.164 Uiso 1 1 calc R . . C23 C 0.0661(10) 0.6506(16) 0.245(4) 0.130(10) Uiso 1 1 d . . . H23A H 0.0680 0.6366 0.1423 0.156 Uiso 1 1 calc R . . H23B H 0.0375 0.6723 0.2597 0.156 Uiso 1 1 calc R . . C24 C 0.1023(12) 0.692(2) 0.280(5) 0.168(14) Uiso 1 1 d . . . H24A H 0.1011 0.7296 0.2182 0.252 Uiso 1 1 calc R . . H24B H 0.1303 0.6697 0.2642 0.252 Uiso 1 1 calc R . . H24C H 0.1001 0.7046 0.3821 0.252 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 Pb1 0.0523(3) 0.0479(3) 0.0447(3) 0.0030(2) -0.0035(2) -0.0047(2) Pb2 0.0493(3) 0.0491(3) 0.0438(3) 0.0032(3) -0.0009(2) 0.0055(2) Pb3 0.0586(3) 0.0612(4) 0.0433(3) 0.0022(3) -0.0033(3) -0.0020(3) Pb4 0.0580(3) 0.0575(3) 0.0394(3) 0.0012(2) -0.0030(2) -0.0046(3) I1 0.0661(6) 0.0730(8) 0.0586(6) 0.0147(5) 0.0140(5) 0.0172(6) I2 0.0678(6) 0.0632(7) 0.0581(6) -0.0073(5) -0.0165(5) -0.0050(5) I3 0.0618(6) 0.0649(7) 0.0583(6) -0.0150(5) -0.0143(5) 0.0046(5) I4 0.0726(7) 0.0624(7) 0.0649(6) -0.0078(6) 0.0252(6) -0.0103(6) I5 0.0504(5) 0.0892(9) 0.0557(6) 0.0101(6) -0.0032(5) -0.0125(5) I6 0.0735(6) 0.0722(7) 0.0449(5) -0.0112(5) 0.0023(5) 0.0000(6) I7 0.0814(7) 0.0484(6) 0.0684(7) -0.0023(5) 0.0053(6) -0.0123(5) I8 0.0921(8) 0.0809(8) 0.0684(7) -0.0020(7) 0.0012(7) 0.0437(7) I9 0.0566(5) 0.0826(8) 0.0548(5) 0.0002(6) -0.0045(5) -0.0111(6) I10 0.0748(6) 0.0724(7) 0.0418(5) -0.0068(5) 0.0024(5) 0.0040(6) I11 0.0828(7) 0.0836(8) 0.0497(6) -0.0001(6) -0.0004(6) 0.0145(6) I12 0.1802(16) 0.0646(8) 0.0508(6) 0.0020(6) -0.0234(9) -0.0294(9) _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 Pb1 I7 2.9878(13) . ? Pb1 I5 3.1575(12) . ? Pb1 I6 3.1759(12) 1_554 ? Pb1 I3 3.2677(12) 1_554 ? Pb1 I1 3.3618(13) . ? Pb1 I2 3.4820(14) . ? Pb1 Pb2 4.2845(9) . ? Pb1 Pb4 4.5392(9) 1_554 ? Pb2 I8 2.9679(13) . ? Pb2 I6 3.1827(12) . ? Pb2 I5 3.2220(12) . ? Pb2 I4 3.2241(13) . ? Pb2 I2 3.3056(12) . ? Pb2 I1 3.5253(13) . ? Pb2 Pb3 4.6021(10) . ? Pb3 I11 3.0367(15) . ? Pb3 I10 3.1865(13) . ? Pb3 I9 3.1926(13) . ? Pb3 I3 3.2473(12) . ? Pb3 I1 3.3354(14) . ? Pb3 I4 3.6452(16) . ? Pb3 Pb4 4.3959(9) . ? Pb4 I12 2.9978(16) . ? Pb4 I9 3.2220(12) . ? Pb4 I10 3.2244(12) 1_556 ? Pb4 I2 3.2407(12) 1_556 ? Pb4 I4 3.2473(12) . ? Pb4 I3 3.4652(15) . ? Pb4 Pb1 4.5392(9) 1_556 ? I2 Pb4 3.2407(12) 1_554 ? I3 Pb1 3.2677(12) 1_556 ? I6 Pb1 3.1759(12) 1_556 ? I10 Pb4 3.2244(12) 1_554 ? N1 C1 1.42(4) . ? N1 C5 1.48(3) . ? N1 C3 1.52(3) . ? N1 C7 1.75(4) . ? N2 C4 1.45(3) . ? N2 C2 1.48(3) . ? N2 C6 1.51(3) . ? N2 C10 1.62(4) . ? C1 C2 1.57(4) . ? C3 C4 1.53(3) . ? C5 C6 1.43(3) . ? C7 C8 1.26(8) . ? C8 C9 1.66(8) . ? C10 C11 1.59(6) . ? C11 C12 1.52(6) . ? N3 C15 1.47(4) . ? N3 C14 1.49(3) . ? N3 C13 1.57(3) . ? N3 C16 1.76(3) . ? C13 C14 1.48(2) 2_665 ? C14 C13 1.48(2) 2_665 ? C15 C15 1.29(5) 2_665 ? C16 C17 1.24(6) . ? C17 C18 1.48(5) . ? N4 C19 1.46(3) . ? N4 C20 1.51(3) . ? N4 C22 1.52(4) . ? N4 C21 1.53(3) . ? C19 C20 1.70(3) 2_565 ? C20 C19 1.70(3) 2_565 ? C21 C21 1.27(5) 2_565 ? C22 C23 1.45(4) . ? C23 C24 1.41(4) . ? 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 I7 Pb1 I5 95.47(4) . . ? I7 Pb1 I6 90.98(4) . 1_554 ? I5 Pb1 I6 86.95(3) . 1_554 ? I7 Pb1 I3 87.72(4) . 1_554 ? I5 Pb1 I3 176.23(4) . 1_554 ? I6 Pb1 I3 91.00(3) 1_554 1_554 ? I7 Pb1 I1 85.87(4) . . ? I5 Pb1 I1 85.66(3) . . ? I6 Pb1 I1 171.65(4) 1_554 . ? I3 Pb1 I1 96.60(3) 1_554 . ? I7 Pb1 I2 168.02(4) . . ? I5 Pb1 I2 82.52(3) . . ? I6 Pb1 I2 100.67(4) 1_554 . ? I3 Pb1 I2 94.77(3) 1_554 . ? I1 Pb1 I2 82.20(3) . . ? I7 Pb1 Pb2 121.58(3) . . ? I5 Pb1 Pb2 48.45(2) . . ? I6 Pb1 Pb2 123.13(3) 1_554 . ? I3 Pb1 Pb2 131.05(3) 1_554 . ? I1 Pb1 Pb2 53.26(2) . . ? I2 Pb1 Pb2 49.05(2) . . ? I7 Pb1 Pb4 136.21(3) . 1_554 ? I5 Pb1 Pb4 127.69(3) . 1_554 ? I6 Pb1 Pb4 97.61(3) 1_554 1_554 ? I3 Pb1 Pb4 49.48(3) 1_554 1_554 ? I1 Pb1 Pb4 89.98(3) . 1_554 ? I2 Pb1 Pb4 45.32(2) . 1_554 ? Pb2 Pb1 Pb4 88.766(16) . 1_554 ? I8 Pb2 I6 90.56(4) . . ? I8 Pb2 I5 88.49(4) . . ? I6 Pb2 I5 97.45(3) . . ? I8 Pb2 I4 89.58(4) . . ? I6 Pb2 I4 92.56(3) . . ? I5 Pb2 I4 169.82(4) . . ? I8 Pb2 I2 87.03(4) . . ? I6 Pb2 I2 176.93(4) . . ? I5 Pb2 I2 84.40(3) . . ? I4 Pb2 I2 85.52(3) . . ? I8 Pb2 I1 166.38(4) . . ? I6 Pb2 I1 100.32(4) . . ? I5 Pb2 I1 82.04(3) . . ? I4 Pb2 I1 98.02(4) . . ? I2 Pb2 I1 82.35(3) . . ? I8 Pb2 Pb1 116.64(3) . . ? I6 Pb2 Pb1 130.26(3) . . ? I5 Pb2 Pb1 47.17(2) . . ? I4 Pb2 Pb1 125.91(3) . . ? I2 Pb2 Pb1 52.71(3) . . ? I1 Pb2 Pb1 49.84(2) . . ? I8 Pb2 Pb3 139.37(4) . . ? I6 Pb2 Pb3 102.31(3) . . ? I5 Pb2 Pb3 126.78(3) . . ? I4 Pb2 Pb3 51.96(3) . . ? I2 Pb2 Pb3 78.39(2) . . ? I1 Pb2 Pb3 46.14(2) . . ? Pb1 Pb2 Pb3 83.774(14) . . ? I11 Pb3 I10 92.29(4) . . ? I11 Pb3 I9 92.95(4) . . ? I10 Pb3 I9 91.79(4) . . ? I11 Pb3 I3 89.90(4) . . ? I10 Pb3 I3 177.67(4) . . ? I9 Pb3 I3 87.29(3) . . ? I11 Pb3 I1 93.93(4) . . ? I10 Pb3 I1 95.75(4) . . ? I9 Pb3 I1 169.57(3) . . ? I3 Pb3 I1 84.90(4) . . ? I11 Pb3 I4 163.30(3) . . ? I10 Pb3 I4 101.67(4) . . ? I9 Pb3 I4 77.65(3) . . ? I3 Pb3 I4 76.04(3) . . ? I1 Pb3 I4 93.73(3) . . ? I11 Pb3 Pb4 117.33(3) . . ? I10 Pb3 Pb4 126.78(3) . . ? I9 Pb3 Pb4 47.02(2) . . ? I3 Pb3 Pb4 51.27(3) . . ? I1 Pb3 Pb4 122.59(3) . . ? I4 Pb3 Pb4 46.49(2) . . ? I11 Pb3 Pb2 141.98(3) . . ? I10 Pb3 Pb2 100.89(3) . . ? I9 Pb3 Pb2 121.74(3) . . ? I3 Pb3 Pb2 77.82(2) . . ? I1 Pb3 Pb2 49.65(2) . . ? I4 Pb3 Pb2 44.15(2) . . ? Pb4 Pb3 Pb2 82.502(14) . . ? I12 Pb4 I9 95.46(4) . . ? I12 Pb4 I10 98.75(4) . 1_556 ? I9 Pb4 I10 91.85(3) . 1_556 ? I12 Pb4 I2 85.43(4) . 1_556 ? I9 Pb4 I2 178.46(4) . 1_556 ? I10 Pb4 I2 89.26(3) 1_556 1_556 ? I12 Pb4 I4 86.87(4) . . ? I9 Pb4 I4 83.34(3) . . ? I10 Pb4 I4 172.96(4) 1_556 . ? I2 Pb4 I4 95.46(4) 1_556 . ? I12 Pb4 I3 165.51(4) . . ? I9 Pb4 I3 83.23(3) . . ? I10 Pb4 I3 95.72(3) 1_556 . ? I2 Pb4 I3 95.59(3) 1_556 . ? I4 Pb4 I3 78.64(3) . . ? I12 Pb4 Pb3 123.33(3) . . ? I9 Pb4 Pb3 46.46(2) . . ? I10 Pb4 Pb3 118.52(3) 1_556 . ? I2 Pb4 Pb3 132.00(3) 1_556 . ? I4 Pb4 Pb3 54.49(3) . . ? I3 Pb4 Pb3 46.98(2) . . ? I12 Pb4 Pb1 132.85(4) . 1_556 ? I9 Pb4 Pb1 128.96(3) . 1_556 ? I10 Pb4 Pb1 95.10(3) 1_556 1_556 ? I2 Pb4 Pb1 49.82(2) 1_556 1_556 ? I4 Pb4 Pb1 84.03(3) . 1_556 ? I3 Pb4 Pb1 45.79(2) . 1_556 ? Pb3 Pb4 Pb1 87.091(16) . 1_556 ? Pb3 I1 Pb1 124.90(5) . . ? Pb3 I1 Pb2 84.21(3) . . ? Pb1 I1 Pb2 76.90(3) . . ? Pb4 I2 Pb2 141.19(4) 1_554 . ? Pb4 I2 Pb1 84.86(3) 1_554 . ? Pb2 I2 Pb1 78.23(3) . . ? Pb3 I3 Pb1 141.81(4) . 1_556 ? Pb3 I3 Pb4 81.75(3) . . ? Pb1 I3 Pb4 84.73(3) 1_556 . ? Pb2 I4 Pb4 133.01(4) . . ? Pb2 I4 Pb3 83.89(3) . . ? Pb4 I4 Pb3 79.02(3) . . ? Pb1 I5 Pb2 84.38(3) . . ? Pb1 I6 Pb2 121.14(4) 1_556 . ? Pb3 I9 Pb4 86.52(3) . . ? Pb3 I10 Pb4 123.50(4) . 1_554 ? C1 N1 C5 107(2) . . ? C1 N1 C3 109(2) . . ? C5 N1 C3 104.7(19) . . ? C1 N1 C7 127(2) . . ? C5 N1 C7 98(2) . . ? C3 N1 C7 109(2) . . ? C4 N2 C2 109(2) . . ? C4 N2 C6 108(2) . . ? C2 N2 C6 105.8(19) . . ? C4 N2 C10 108(2) . . ? C2 N2 C10 119(2) . . ? C6 N2 C10 107(2) . . ? N1 C1 C2 112(3) . . ? N2 C2 C1 107(2) . . ? N1 C3 C4 109(2) . . ? N2 C4 C3 111(2) . . ? C6 C5 N1 113(2) . . ? C5 C6 N2 110(2) . . ? C8 C7 N1 103(5) . . ? C7 C8 C9 100(6) . . ? C11 C10 N2 121(3) . . ? C12 C11 C10 93(4) . . ? C15 N3 C14 108(2) . . ? C15 N3 C13 100(2) . . ? C14 N3 C13 106.1(16) . . ? C15 N3 C16 136(2) . . ? C14 N3 C16 106.1(17) . . ? C13 N3 C16 97.7(16) . . ? C14 C13 N3 111.3(17) 2_665 . ? C13 C14 N3 111.2(16) 2_665 . ? C15 C15 N3 117.0(14) 2_665 . ? C17 C16 N3 108(4) . . ? C16 C17 C18 111(5) . . ? C19 N4 C20 109.5(18) . . ? C19 N4 C22 107.0(19) . . ? C20 N4 C22 111(2) . . ? C19 N4 C21 106(2) . . ? C20 N4 C21 100.5(18) . . ? C22 N4 C21 122(2) . . ? N4 C19 C20 110.3(17) . 2_565 ? N4 C20 C19 108.4(17) . 2_565 ? C21 C21 N4 118.1(12) 2_565 . ? C23 C22 N4 115(3) . . ? C24 C23 C22 105(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.510 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.206 #===END data_4815n _database_code_CSD 153708 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H116 I24 N4 Pb10' _chemical_formula_weight 5914.99 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' #(No. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2503(9) _cell_length_b 16.4790(13) _cell_length_c 18.6012(16) _cell_angle_alpha 102.047(10) _cell_angle_beta 96.651(10) _cell_angle_gamma 98.144(9) _cell_volume 3300.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 26.0 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 _exptl_absorpt_coefficient_mu 18.337 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1072 _exptl_absorpt_correction_T_max 0.4058 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33736 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10919 _reflns_number_gt 8203 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2 (Berndt, Brandenburg, 1998)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0714P)^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 'idelized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10919 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.52152(3) 0.64241(2) 0.47007(2) 0.04195(11) Uani 1 d . . . Pb2 Pb 0.56521(4) 0.62432(3) 0.73481(2) 0.05319(12) Uani 1 d . . . Pb3 Pb 0.90931(4) 0.72074(2) 0.63511(2) 0.05035(12) Uani 1 d . . . Pb4 Pb 0.81451(4) 0.46236(2) 0.41816(2) 0.04545(11) Uani 1 d . . . Pb5 Pb 0.84867(4) 0.42803(2) 0.68311(2) 0.04552(11) Uani 1 d . . . I1 I 0.68890(6) 0.53456(3) 0.56964(3) 0.03873(15) Uani 1 d . . . I2 I 0.64711(7) 0.55788(4) 0.33195(4) 0.05024(17) Uani 1 d . . . I3 I 0.38981(7) 0.69909(4) 0.61597(4) 0.05049(17) Uani 1 d . . . I4 I 0.77682(9) 0.77716(6) 0.76502(5) 0.0786(3) Uani 1 d . . . I5 I 0.72323(7) 0.79522(4) 0.53074(4) 0.0573(2) Uani 1 d . . . I6 I 0.37331(7) 0.72543(4) 0.36680(5) 0.0588(2) Uani 1 d . . . I7 I 0.72515(7) 0.51153(5) 0.81185(4) 0.0573(2) Uani 1 d . . . I8 I 0.47537(14) 0.69437(8) 0.86860(8) 0.1289(5) Uani 1 d . . . I9 I 0.97618(6) 0.36493(4) 0.52573(4) 0.04881(17) Uani 1 d . . . I10 I 0.93640(7) 0.39967(4) 0.27876(4) 0.05194(18) Uani 1 d . . . I11 I 1.09974(8) 0.87011(5) 0.67837(5) 0.0702(2) Uani 1 d . . . I12 I 0.99065(7) 0.33654(4) 0.77233(4) 0.05478(19) Uani 1 d . . . N1 N 0.0760(7) 0.9348(4) 0.4239(4) 0.0374(18) Uani 1 d . . . C1 C 0.0308(9) 1.0097(5) 0.4682(5) 0.0348(19) Uani 1 d . . . H1A H 0.0991 1.0551 0.4877 0.042 Uiso 1 calc R . . H1B H -0.0259 1.0293 0.4351 0.042 Uiso 1 calc R . . C2 C -0.0277(10) 0.8620(5) 0.3898(6) 0.048(2) Uani 1 d . . . H2A H 0.0069 0.8138 0.3674 0.058 Uiso 1 calc R . . H2B H -0.0681 0.8469 0.4296 0.058 Uiso 1 calc R . . C3 C -0.1215(11) 0.8767(6) 0.3325(6) 0.058(3) Uani 1 d . . . H3A H -0.0860 0.8803 0.2879 0.069 Uiso 1 calc R . . H3B H -0.1468 0.9301 0.3509 0.069 Uiso 1 calc R . . C4 C -0.2315(12) 0.8075(8) 0.3130(8) 0.075(4) Uani 1 d . . . H4A H -0.2047 0.7538 0.2989 0.090 Uiso 1 calc R . . H4B H -0.2701 0.8071 0.3569 0.090 Uiso 1 calc R . . C5 C -0.3223(18) 0.8156(14) 0.2523(10) 0.134(7) Uani 1 d . . . H5A H -0.3888 0.7695 0.2429 0.202 Uiso 1 calc R . . H5B H -0.2856 0.8149 0.2081 0.202 Uiso 1 calc R . . H5C H -0.3516 0.8677 0.2663 0.202 Uiso 1 calc R . . C6 C 0.1671(10) 0.8997(6) 0.4721(6) 0.048(2) Uani 1 d . . . H6A H 0.1240 0.8733 0.5059 0.057 Uiso 1 calc R . . H6B H 0.1988 0.8562 0.4400 0.057 Uiso 1 calc R . . C7 C 0.2718(10) 0.9637(7) 0.5169(7) 0.060(3) Uani 1 d . . . H7A H 0.2424 1.0023 0.5549 0.073 Uiso 1 calc R . . H7B H 0.3088 0.9959 0.4847 0.073 Uiso 1 calc R . . C8 C 0.3662(12) 0.9217(8) 0.5533(8) 0.072(4) Uani 1 d . . . H8A H 0.3253 0.8814 0.5774 0.086 Uiso 1 calc R . . H8B H 0.4043 0.8906 0.5147 0.086 Uiso 1 calc R . . C9 C 0.4619(16) 0.9798(12) 0.6085(10) 0.112(6) Uani 1 d . . . H9A H 0.5176 0.9482 0.6286 0.168 Uiso 1 calc R . . H9B H 0.4257 1.0098 0.6479 0.168 Uiso 1 calc R . . H9C H 0.5048 1.0191 0.5850 0.168 Uiso 1 calc R . . C10 C 0.1346(9) 0.9679(5) 0.3637(5) 0.042(2) Uani 1 d . . . H10A H 0.0724 0.9858 0.3329 0.050 Uiso 1 calc R . . H10B H 0.1943 1.0175 0.3876 0.050 Uiso 1 calc R . . C11 C 0.1958(12) 0.9086(6) 0.3136(7) 0.064(3) Uani 1 d . . . H11A H 0.1400 0.8563 0.2922 0.077 Uiso 1 calc R . . H11B H 0.2657 0.8958 0.3422 0.077 Uiso 1 calc R . . C12 C 0.2360(16) 0.9483(9) 0.2525(8) 0.089(5) Uani 1 d . . . H12A H 0.2699 1.0073 0.2730 0.106 Uiso 1 calc R . . H12B H 0.2991 0.9208 0.2317 0.106 Uiso 1 calc R . . C13 C 0.133(2) 0.9413(15) 0.1930(11) 0.151(8) Uani 1 d . . . H13A H 0.1615 0.9670 0.1549 0.227 Uiso 1 calc R . . H13B H 0.0716 0.9694 0.2134 0.227 Uiso 1 calc R . . H13C H 0.1007 0.8830 0.1722 0.227 Uiso 1 calc R . . N2 N 0.1184(8) 0.5955(5) 0.9929(4) 0.0437(19) Uani 1 d . . . C14 C 0.0492(9) 0.5298(6) 1.0275(5) 0.045(2) Uani 1 d . . . H14A H 0.1060 0.4980 1.0474 0.055 Uiso 1 calc R . . H14B H 0.0135 0.5586 1.0685 0.055 Uiso 1 calc R . . C15 C 0.2107(10) 0.6523(7) 1.0562(6) 0.053(3) Uani 1 d . . . H15A H 0.1668 0.6755 1.0953 0.064 Uiso 1 calc R . . H15B H 0.2623 0.6173 1.0762 0.064 Uiso 1 calc R . . C16 C 0.2899(12) 0.7227(8) 1.0390(6) 0.070(3) Uani 1 d . . . H16A H 0.2402 0.7602 1.0215 0.085 Uiso 1 calc R . . H16B H 0.3338 0.7008 0.9994 0.085 Uiso 1 calc R . . C17 C 0.3795(14) 0.7717(9) 1.1059(8) 0.086(4) Uani 1 d . . . H17A H 0.3350 0.7907 1.1461 0.103 Uiso 1 calc R . . H17B H 0.4308 0.7342 1.1219 0.103 Uiso 1 calc R . . C18 C 0.4585(18) 0.8463(10) 1.0927(11) 0.124(7) Uani 1 d . . . H18A H 0.5128 0.8740 1.1376 0.186 Uiso 1 calc R . . H18B H 0.4089 0.8846 1.0782 0.186 Uiso 1 calc R . . H18C H 0.5048 0.8281 1.0540 0.186 Uiso 1 calc R . . C19 C 0.1788(10) 0.5542(7) 0.9302(5) 0.051(3) Uani 1 d . . . H19A H 0.2199 0.5978 0.9096 0.061 Uiso 1 calc R . . H19B H 0.1162 0.5193 0.8914 0.061 Uiso 1 calc R . . C20 C 0.2698(12) 0.5001(9) 0.9509(7) 0.072(4) Uani 1 d . . . H20A H 0.3337 0.5346 0.9891 0.086 Uiso 1 calc R . . H20B H 0.2295 0.4560 0.9714 0.086 Uiso 1 calc R . . C21 C 0.3246(14) 0.4611(9) 0.8859(8) 0.084(4) Uani 1 d . . . H21A H 0.2594 0.4267 0.8486 0.101 Uiso 1 calc R . . H21B H 0.3611 0.5060 0.8648 0.101 Uiso 1 calc R . . C22 C 0.4172(18) 0.4085(13) 0.8992(12) 0.141(8) Uani 1 d . . . H22A H 0.4451 0.3869 0.8533 0.212 Uiso 1 calc R . . H22B H 0.3822 0.3624 0.9185 0.212 Uiso 1 calc R . . H22C H 0.4843 0.4419 0.9345 0.212 Uiso 1 calc R . . C23 C 0.0341(11) 0.6468(7) 0.9600(6) 0.059(3) Uani 1 d . . . H23A H -0.0265 0.6086 0.9221 0.071 Uiso 1 calc R . . H23B H 0.0810 0.6839 0.9355 0.071 Uiso 1 calc R . . C24 C -0.0314(13) 0.7000(9) 1.0149(8) 0.078(4) Uani 1 d . . . H24A H -0.0725 0.6644 1.0431 0.093 Uiso 1 calc R . . H24B H 0.0280 0.7431 1.0496 0.093 Uiso 1 calc R . . C25 C -0.1215(18) 0.7409(11) 0.9770(10) 0.116(6) Uani 1 d . . . H25A H -0.1765 0.6975 0.9399 0.140 Uiso 1 calc R . . H25B H -0.0785 0.7782 0.9509 0.140 Uiso 1 calc R . . C26 C -0.196(2) 0.7909(13) 1.0260(15) 0.177(11) Uani 1 d . . . H26A H -0.2509 0.8146 0.9960 0.265 Uiso 1 calc R . . H26B H -0.1433 0.8354 1.0621 0.265 Uiso 1 calc R . . H26C H -0.2418 0.7545 1.0509 0.265 Uiso 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 Pb1 0.0371(2) 0.03658(19) 0.0503(2) 0.01121(15) 0.00173(17) 0.00206(15) Pb2 0.0509(3) 0.0621(2) 0.0480(2) 0.01260(18) 0.01125(19) 0.0114(2) Pb3 0.0529(3) 0.0450(2) 0.0530(2) 0.01240(17) 0.0103(2) 0.00397(18) Pb4 0.0383(2) 0.0544(2) 0.0450(2) 0.01246(17) 0.00809(17) 0.00949(18) Pb5 0.0486(3) 0.0510(2) 0.0383(2) 0.01317(16) 0.00439(17) 0.01020(18) I1 0.0399(4) 0.0369(3) 0.0384(3) 0.0094(2) 0.0046(3) 0.0032(3) I2 0.0527(5) 0.0548(4) 0.0471(4) 0.0164(3) 0.0089(3) 0.0141(3) I3 0.0501(5) 0.0463(3) 0.0568(4) 0.0142(3) 0.0094(3) 0.0094(3) I4 0.0854(7) 0.0760(5) 0.0659(5) 0.0011(4) 0.0319(5) -0.0092(4) I5 0.0538(5) 0.0420(3) 0.0691(5) 0.0179(3) -0.0046(4) -0.0113(3) I6 0.0555(5) 0.0483(4) 0.0718(5) 0.0185(3) -0.0061(4) 0.0114(3) I7 0.0628(5) 0.0745(5) 0.0403(4) 0.0159(3) 0.0062(3) 0.0278(4) I8 0.1422(12) 0.1242(9) 0.1145(10) -0.0080(7) 0.0923(9) -0.0031(8) I9 0.0481(5) 0.0530(4) 0.0462(4) 0.0113(3) 0.0093(3) 0.0096(3) I10 0.0545(5) 0.0578(4) 0.0441(4) 0.0114(3) 0.0107(3) 0.0090(3) I11 0.0627(6) 0.0617(4) 0.0837(6) 0.0288(4) -0.0004(4) -0.0059(4) I12 0.0666(5) 0.0561(4) 0.0404(4) 0.0040(3) -0.0002(3) 0.0239(4) N1 0.044(5) 0.026(3) 0.042(4) 0.009(3) 0.010(4) 0.006(3) C1 0.045(6) 0.023(4) 0.038(5) 0.009(3) 0.008(4) 0.008(4) C2 0.054(7) 0.032(4) 0.051(6) -0.003(4) 0.016(5) -0.004(4) C3 0.064(8) 0.048(6) 0.056(7) 0.003(5) 0.003(6) 0.006(5) C4 0.063(10) 0.070(8) 0.082(9) 0.007(7) 0.001(7) 0.001(6) C5 0.104(17) 0.20(2) 0.078(12) 0.023(13) -0.015(11) -0.013(14) C6 0.053(7) 0.040(5) 0.056(6) 0.018(5) 0.008(5) 0.019(5) C7 0.048(8) 0.055(6) 0.076(8) 0.013(6) 0.001(6) 0.014(5) C8 0.063(9) 0.061(7) 0.090(10) 0.019(6) -0.008(7) 0.019(6) C9 0.076(13) 0.144(15) 0.100(13) 0.018(11) -0.021(10) 0.014(11) C10 0.042(6) 0.032(4) 0.050(6) 0.007(4) 0.010(5) 0.003(4) C11 0.081(9) 0.040(5) 0.074(8) 0.004(5) 0.036(7) 0.014(5) C12 0.110(14) 0.086(9) 0.074(10) 0.009(7) 0.042(9) 0.021(9) C13 0.17(2) 0.19(2) 0.088(14) 0.024(14) 0.023(15) 0.021(18) N2 0.045(5) 0.056(5) 0.027(4) 0.012(3) 0.000(3) -0.001(4) C14 0.053(7) 0.059(6) 0.021(4) 0.006(4) 0.004(4) 0.007(5) C15 0.046(7) 0.068(7) 0.038(6) 0.003(5) 0.004(5) -0.002(5) C16 0.068(9) 0.087(8) 0.046(7) 0.016(6) -0.002(6) -0.013(7) C17 0.077(11) 0.079(9) 0.083(10) 0.011(7) -0.018(8) -0.012(7) C18 0.126(18) 0.098(12) 0.126(16) 0.026(11) -0.004(13) -0.036(11) C19 0.055(7) 0.065(6) 0.032(5) 0.011(4) 0.012(5) 0.002(5) C20 0.068(9) 0.095(9) 0.054(7) 0.004(6) 0.024(6) 0.026(7) C21 0.101(12) 0.086(9) 0.065(9) -0.005(7) 0.043(8) 0.020(8) C22 0.113(16) 0.158(18) 0.155(19) -0.008(14) 0.065(14) 0.064(14) C23 0.065(8) 0.066(7) 0.050(6) 0.029(5) 0.003(6) 0.010(6) C24 0.081(10) 0.083(9) 0.079(9) 0.027(7) 0.014(8) 0.031(8) C25 0.118(16) 0.109(13) 0.119(15) 0.023(11) -0.018(12) 0.044(12) C26 0.15(2) 0.111(15) 0.26(3) 0.001(17) 0.02(2) 0.080(15) _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 Pb1 I6 3.0568(8) . ? Pb1 I5 3.0604(9) . ? Pb1 I2 3.2314(9) . ? Pb1 I3 3.2708(9) . ? Pb1 I1 3.3754(8) 2_666 ? Pb1 I1 3.4130(7) . ? Pb1 Pb5 4.6165(8) 2_666 ? Pb1 Pb4 4.7867(7) . ? Pb1 Pb4 4.8024(7) 2_666 ? Pb1 Pb3 4.8756(8) . ? Pb1 Pb2 4.9673(7) . ? Pb1 Pb1 5.0164(8) 2_666 ? Pb2 I8 2.8742(11) . ? Pb2 I4 3.1189(11) . ? Pb2 I7 3.1950(8) . ? Pb2 I3 3.3338(8) . ? Pb2 I2 3.4624(10) 2_666 ? Pb2 I1 3.6388(8) . ? Pb2 Pb3 4.7011(7) . ? Pb2 Pb4 4.7060(8) 2_666 ? Pb2 Pb5 4.8880(7) . ? Pb2 Pb1 5.0723(9) 2_666 ? Pb3 I11 2.9286(10) . ? Pb3 I4 3.0356(10) . ? Pb3 I5 3.2309(9) . ? Pb3 I10 3.3430(8) 2_766 ? Pb3 I9 3.4997(9) 2_766 ? Pb3 I1 3.5539(8) . ? Pb3 Pb4 4.6757(7) 2_766 ? Pb3 Pb5 5.0533(7) . ? Pb3 Pb4 5.1083(9) . ? Pb4 I10 3.1271(8) . ? Pb4 I2 3.1290(8) . ? Pb4 I3 3.1606(9) 2_666 ? Pb4 I9 3.3205(9) 2_766 ? Pb4 I9 3.3488(8) . ? Pb4 I1 3.3690(8) . ? Pb4 Pb3 4.6757(7) 2_766 ? Pb4 Pb2 4.7060(9) 2_666 ? Pb4 Pb4 4.7160(10) 2_766 ? Pb4 Pb5 4.7228(7) 2_766 ? Pb4 Pb1 4.8024(7) 2_666 ? Pb5 I12 2.9482(8) . ? Pb5 I7 3.0817(9) . ? Pb5 I6 3.1918(10) 2_666 ? Pb5 I10 3.3509(9) 2_766 ? Pb5 I9 3.4401(8) . ? Pb5 I1 3.5113(7) . ? Pb5 Pb1 4.6165(8) 2_666 ? Pb5 Pb4 4.7228(7) 2_766 ? I1 Pb1 3.3754(8) 2_666 ? I2 Pb2 3.4624(10) 2_666 ? I3 Pb4 3.1606(9) 2_666 ? I6 Pb5 3.1918(10) 2_666 ? I9 Pb4 3.3205(9) 2_766 ? I9 Pb3 3.4997(9) 2_766 ? I10 Pb3 3.3430(8) 2_766 ? I10 Pb5 3.3509(9) 2_766 ? N1 C10 1.519(11) . ? N1 C1 1.521(10) . ? N1 C2 1.523(12) . ? N1 C6 1.537(11) . ? C1 C1 1.505(16) 2_576 ? C2 C3 1.493(15) . ? C3 C4 1.513(16) . ? C4 C5 1.47(2) . ? C6 C7 1.499(15) . ? C7 C8 1.518(14) . ? C8 C9 1.47(2) . ? C10 C11 1.503(13) . ? C11 C12 1.508(17) . ? C12 C13 1.48(2) . ? N2 C19 1.506(12) . ? N2 C23 1.515(12) . ? N2 C15 1.524(13) . ? N2 C14 1.536(12) . ? C14 C14 1.500(19) 2_567 ? C15 C16 1.473(15) . ? C16 C17 1.509(17) . ? C17 C18 1.492(19) . ? C19 C20 1.517(15) . ? C20 C21 1.489(16) . ? C21 C22 1.48(2) . ? C23 C24 1.530(17) . ? C24 C25 1.485(18) . ? C25 C26 1.51(3) . ? 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 I6 Pb1 I5 95.77(2) . . ? I6 Pb1 I2 89.63(2) . . ? I5 Pb1 I2 96.31(3) . . ? I6 Pb1 I3 96.68(2) . . ? I5 Pb1 I3 89.35(2) . . ? I2 Pb1 I3 171.08(2) . . ? I6 Pb1 I1 92.68(2) . 2_666 ? I5 Pb1 I1 170.50(2) . 2_666 ? I2 Pb1 I1 88.06(2) . 2_666 ? I3 Pb1 I1 85.36(2) . 2_666 ? I6 Pb1 I1 174.16(2) . . ? I5 Pb1 I1 87.26(2) . . ? I2 Pb1 I1 85.069(19) . . ? I3 Pb1 I1 88.333(19) . . ? I1 Pb1 I1 84.716(19) 2_666 . ? Pb5 Pb1 Pb4 117.249(13) 2_666 . ? Pb5 Pb1 Pb4 64.866(11) 2_666 2_666 ? Pb4 Pb1 Pb4 116.915(10) . 2_666 ? Pb5 Pb1 Pb3 178.905(11) 2_666 . ? Pb4 Pb1 Pb3 63.825(12) . . ? Pb4 Pb1 Pb3 114.585(12) 2_666 . ? Pb5 Pb1 Pb2 122.363(13) 2_666 . ? Pb4 Pb1 Pb2 91.784(13) . . ? Pb4 Pb1 Pb2 57.562(12) 2_666 . ? Pb3 Pb1 Pb2 57.050(11) . . ? Pb5 Pb1 Pb1 91.735(15) 2_666 2_666 ? Pb4 Pb1 Pb1 58.610(11) . 2_666 ? Pb4 Pb1 Pb1 58.305(11) 2_666 2_666 ? Pb3 Pb1 Pb1 88.704(14) . 2_666 ? Pb2 Pb1 Pb1 61.066(13) . 2_666 ? I8 Pb2 I4 91.24(4) . . ? I8 Pb2 I7 94.30(4) . . ? I4 Pb2 I7 93.77(3) . . ? I8 Pb2 I3 98.30(4) . . ? I4 Pb2 I3 94.37(3) . . ? I7 Pb2 I3 164.82(2) . . ? I8 Pb2 I2 100.30(3) . 2_666 ? I4 Pb2 I2 168.43(2) . 2_666 ? I7 Pb2 I2 86.31(2) . 2_666 ? I3 Pb2 I2 83.15(2) . 2_666 ? I8 Pb2 I1 177.88(4) . . ? I4 Pb2 I1 87.94(2) . . ? I7 Pb2 I1 83.81(2) . . ? I3 Pb2 I1 83.710(19) . . ? I2 Pb2 I1 80.56(2) 2_666 . ? Pb3 Pb2 Pb4 119.922(13) . 2_666 ? Pb3 Pb2 Pb5 63.568(10) . . ? Pb4 Pb2 Pb5 113.604(14) 2_666 . ? Pb3 Pb2 Pb1 60.493(12) . . ? Pb4 Pb2 Pb1 59.459(12) 2_666 . ? Pb5 Pb2 Pb1 89.188(13) . . ? Pb3 Pb2 Pb1 90.001(14) . 2_666 ? Pb4 Pb2 Pb1 58.476(12) 2_666 2_666 ? Pb5 Pb2 Pb1 55.187(11) . 2_666 ? Pb1 Pb2 Pb1 59.945(11) . 2_666 ? I11 Pb3 I4 93.75(3) . . ? I11 Pb3 I5 97.29(2) . . ? I4 Pb3 I5 89.34(3) . . ? I11 Pb3 I10 95.44(3) . 2_766 ? I4 Pb3 I10 94.11(3) . 2_766 ? I5 Pb3 I10 166.56(2) . 2_766 ? I11 Pb3 I9 94.18(3) . 2_766 ? I4 Pb3 I9 171.78(3) . 2_766 ? I5 Pb3 I9 87.50(2) . 2_766 ? I10 Pb3 I9 87.31(2) 2_766 2_766 ? I11 Pb3 I1 175.42(3) . . ? I4 Pb3 I1 90.82(2) . . ? I5 Pb3 I1 82.36(2) . . ? I10 Pb3 I1 84.61(2) 2_766 . ? I9 Pb3 I1 81.25(2) 2_766 . ? Pb4 Pb3 Pb2 117.943(12) 2_766 . ? Pb4 Pb3 Pb1 114.661(13) 2_766 . ? Pb2 Pb3 Pb1 62.457(11) . . ? Pb4 Pb3 Pb5 57.926(10) 2_766 . ? Pb2 Pb3 Pb5 60.017(11) . . ? Pb1 Pb3 Pb5 88.338(13) . . ? Pb4 Pb3 Pb4 57.429(12) 2_766 . ? Pb2 Pb3 Pb4 91.041(14) . . ? Pb1 Pb3 Pb4 57.241(12) . . ? Pb5 Pb3 Pb4 59.647(10) . . ? I10 Pb4 I2 92.56(2) . . ? I10 Pb4 I3 94.31(2) . 2_666 ? I2 Pb4 I3 91.65(2) . 2_666 ? I10 Pb4 I9 91.76(2) . 2_766 ? I2 Pb4 I9 90.66(2) . 2_766 ? I3 Pb4 I9 173.40(2) 2_666 2_766 ? I10 Pb4 I9 93.65(2) . . ? I2 Pb4 I9 173.74(2) . . ? I3 Pb4 I9 87.03(2) 2_666 . ? I9 Pb4 I9 90.00(2) 2_766 . ? I10 Pb4 I1 178.47(2) . . ? I2 Pb4 I1 87.43(2) . . ? I3 Pb4 I1 87.22(2) 2_666 . ? I9 Pb4 I1 86.71(2) 2_766 . ? I9 Pb4 I1 86.392(19) . . ? Pb3 Pb4 Pb2 113.844(13) 2_766 2_666 ? Pb3 Pb4 Pb4 65.900(13) 2_766 2_766 ? Pb2 Pb4 Pb4 176.165(14) 2_666 2_766 ? Pb3 Pb4 Pb5 65.048(10) 2_766 2_766 ? Pb2 Pb4 Pb5 118.838(12) 2_666 2_766 ? Pb4 Pb4 Pb5 64.748(12) 2_766 2_766 ? Pb3 Pb4 Pb1 178.193(11) 2_766 . ? Pb2 Pb4 Pb1 64.591(12) 2_666 . ? Pb4 Pb4 Pb1 115.595(15) 2_766 . ? Pb5 Pb4 Pb1 116.367(11) 2_766 . ? Pb3 Pb4 Pb1 115.545(11) 2_766 2_666 ? Pb2 Pb4 Pb1 62.979(11) 2_666 2_666 ? Pb4 Pb4 Pb1 113.466(14) 2_766 2_666 ? Pb5 Pb4 Pb1 177.879(11) 2_766 2_666 ? Pb1 Pb4 Pb1 63.085(10) . 2_666 ? I12 Pb5 I7 95.22(2) . . ? I12 Pb5 I6 92.69(2) . 2_666 ? I7 Pb5 I6 90.99(3) . 2_666 ? I12 Pb5 I10 94.20(2) . 2_766 ? I7 Pb5 I10 89.15(2) . 2_766 ? I6 Pb5 I10 173.06(2) 2_666 2_766 ? I12 Pb5 I9 94.26(2) . . ? I7 Pb5 I9 169.63(2) . . ? I6 Pb5 I9 92.76(2) 2_666 . ? I10 Pb5 I9 85.97(2) 2_766 . ? I12 Pb5 I1 177.04(2) . . ? I7 Pb5 I1 87.659(19) . . ? I6 Pb5 I1 87.91(2) 2_666 . ? I10 Pb5 I1 85.162(19) 2_766 . ? I9 Pb5 I1 82.821(18) . . ? Pb1 Pb5 Pb4 116.893(12) 2_666 2_766 ? Pb1 Pb5 Pb2 64.433(12) 2_666 . ? Pb4 Pb5 Pb2 113.438(12) 2_766 . ? Pb1 Pb5 Pb3 91.206(13) 2_666 . ? Pb4 Pb5 Pb3 57.025(11) 2_766 . ? Pb2 Pb5 Pb3 56.414(10) . . ? Pb1 Pb5 Pb4 59.347(11) 2_666 . ? Pb4 Pb5 Pb4 57.561(13) 2_766 . ? Pb2 Pb5 Pb4 89.574(13) . . ? Pb3 Pb5 Pb4 60.717(12) . . ? Pb4 I1 Pb1 90.80(2) . 2_666 ? Pb4 I1 Pb1 89.785(18) . . ? Pb1 I1 Pb1 95.284(19) 2_666 . ? Pb4 I1 Pb5 94.514(18) . . ? Pb1 I1 Pb5 84.161(17) 2_666 . ? Pb1 I1 Pb5 175.67(2) . . ? Pb4 I1 Pb3 95.07(2) . . ? Pb1 I1 Pb3 172.86(2) 2_666 . ? Pb1 I1 Pb3 88.802(17) . . ? Pb5 I1 Pb3 91.323(19) . . ? Pb4 I1 Pb2 176.62(2) . . ? Pb1 I1 Pb2 92.55(2) 2_666 . ? Pb1 I1 Pb2 89.503(18) . . ? Pb5 I1 Pb2 86.235(17) . . ? Pb3 I1 Pb2 81.617(19) . . ? Pb4 I2 Pb1 97.62(2) . . ? Pb4 I2 Pb2 90.97(2) . 2_666 ? Pb1 I2 Pb2 98.47(2) . 2_666 ? Pb4 I3 Pb1 96.60(2) 2_666 . ? Pb4 I3 Pb2 92.84(2) 2_666 . ? Pb1 I3 Pb2 97.54(2) . . ? Pb3 I4 Pb2 99.60(3) . . ? Pb1 I5 Pb3 101.57(2) . . ? Pb1 I6 Pb5 95.23(2) . 2_666 ? Pb5 I7 Pb2 102.28(2) . . ? Pb4 I9 Pb4 90.00(2) 2_766 . ? Pb4 I9 Pb5 88.61(2) 2_766 . ? Pb4 I9 Pb5 96.21(2) . . ? Pb4 I9 Pb3 96.97(2) 2_766 2_766 ? Pb4 I9 Pb3 86.085(19) . 2_766 ? Pb5 I9 Pb3 173.98(2) . 2_766 ? Pb4 I10 Pb3 92.49(2) . 2_766 ? Pb4 I10 Pb5 93.55(2) . 2_766 ? Pb3 I10 Pb5 98.03(2) 2_766 2_766 ? C10 N1 C1 104.9(6) . . ? C10 N1 C2 110.8(7) . . ? C1 N1 C2 111.5(7) . . ? C10 N1 C6 111.2(7) . . ? C1 N1 C6 112.5(7) . . ? C2 N1 C6 106.0(7) . . ? C1 C1 N1 113.6(7) 2_576 . ? C3 C2 N1 116.6(8) . . ? C2 C3 C4 112.2(9) . . ? C5 C4 C3 114.3(13) . . ? C7 C6 N1 114.8(7) . . ? C6 C7 C8 111.1(9) . . ? C9 C8 C7 114.9(11) . . ? C11 C10 N1 117.1(7) . . ? C10 C11 C12 109.7(9) . . ? C13 C12 C11 111.2(15) . . ? C19 N2 C23 106.2(7) . . ? C19 N2 C15 111.8(8) . . ? C23 N2 C15 110.2(8) . . ? C19 N2 C14 111.3(7) . . ? C23 N2 C14 111.7(8) . . ? C15 N2 C14 105.7(7) . . ? C14 C14 N2 112.4(9) 2_567 . ? C16 C15 N2 117.6(9) . . ? C15 C16 C17 112.0(10) . . ? C18 C17 C16 114.4(13) . . ? N2 C19 C20 115.5(8) . . ? C21 C20 C19 112.1(11) . . ? C22 C21 C20 117.4(14) . . ? N2 C23 C24 115.9(9) . . ? C25 C24 C23 112.2(12) . . ? C24 C25 C26 116.4(17) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 2.700 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.212 #=END