# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yu Hui' _publ_contact_author_email jiehuiyu@yahoo.com.cn _publ_author_name 'Yu Hui' # Attachment '3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 745949' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H14 I8 N2 Pb3' _chemical_formula_weight 1750.96 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0277(5) _cell_length_b 12.4356(6) _cell_length_c 13.0643(9) _cell_angle_alpha 76.319(4) _cell_angle_beta 80.802(4) _cell_angle_gamma 68.890(3) _cell_volume 1324.90(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 28.328 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.042 _exptl_absorpt_correction_T_max 0.059 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type siements _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9757 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6547 _reflns_number_gt 4097 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker _computing_cell_refinement Bruker _computing_data_reduction Bruker _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1284P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6547 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2149 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _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 0.43766(8) 0.32895(6) 0.09390(6) 0.0340(2) Uani 1 1 d . . . Pb2 Pb 0.09878(8) 0.34471(6) 0.41255(6) 0.0354(2) Uani 1 1 d . . . Pb3 Pb -0.06693(8) 0.32803(6) 0.09078(6) 0.0333(2) Uani 1 1 d . . . I1 I 0.78158(16) 0.15641(12) 0.04067(13) 0.0456(4) Uani 1 1 d . . . I2 I 0.58386(14) 0.50632(10) 0.15562(11) 0.0359(3) Uani 1 1 d . . . I3 I 0.44722(14) 0.19250(10) 0.32479(10) 0.0354(3) Uani 1 1 d . . . I4 I 0.07852(15) 0.51518(11) 0.15616(10) 0.0383(3) Uani 1 1 d . . . I5 I 0.28228(14) 0.16435(10) 0.02742(10) 0.0342(3) Uani 1 1 d . . . I6 I 0.14929(17) 0.15268(13) 0.60395(12) 0.0500(4) Uani 1 1 d . . . I7 I 0.25789(13) 0.50002(9) 0.50127(11) 0.0379(3) Uani 1 1 d . . . N1 N 0.4242(17) 0.7274(12) 0.3343(13) 0.033(3) Uani 1 1 d . . . N2 N 0.3255(17) 0.9476(12) 0.2848(11) 0.028(3) Uani 1 1 d . . . C1 C 0.371(3) 0.782(2) 0.4311(18) 0.058(6) Uani 1 1 d . . . H1A H 0.2849 0.7575 0.4712 0.069 Uiso 1 1 calc R . . H1B H 0.4592 0.7546 0.4756 0.069 Uiso 1 1 calc R . . C2 C 0.319(3) 0.908(2) 0.4013(16) 0.052(6) Uani 1 1 d . . . H2A H 0.3869 0.9374 0.4300 0.062 Uiso 1 1 calc R . . H2B H 0.2112 0.9408 0.4313 0.062 Uiso 1 1 calc R . . C3 C 0.553(2) 0.7690(16) 0.2740(15) 0.038(4) Uani 1 1 d . . . H3A H 0.5902 0.7342 0.2115 0.046 Uiso 1 1 calc R . . H3B H 0.6417 0.7442 0.3172 0.046 Uiso 1 1 calc R . . C4 C 0.494(2) 0.9014(17) 0.2414(18) 0.043(5) Uani 1 1 d . . . H4A H 0.5594 0.9339 0.2685 0.052 Uiso 1 1 calc R . . H4B H 0.5013 0.9240 0.1649 0.052 Uiso 1 1 calc R . . C5 C 0.282(2) 0.7683(16) 0.2710(17) 0.040(5) Uani 1 1 d . . . H5A H 0.1983 0.7413 0.3119 0.048 Uiso 1 1 calc R . . H5B H 0.3116 0.7361 0.2070 0.048 Uiso 1 1 calc R . . C6 C 0.223(2) 0.9024(16) 0.2429(17) 0.039(4) Uani 1 1 d . . . H6A H 0.2253 0.9279 0.1667 0.046 Uiso 1 1 calc R . . H6B H 0.1145 0.9332 0.2725 0.046 Uiso 1 1 calc R . . I8 I -0.05414(14) 0.19190(10) 0.32268(10) 0.0340(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0407(4) 0.0309(4) 0.0304(4) -0.0024(3) -0.0046(3) -0.0135(3) Pb2 0.0448(4) 0.0310(4) 0.0279(4) -0.0034(3) -0.0059(3) -0.0099(3) Pb3 0.0367(4) 0.0314(4) 0.0270(4) 0.0003(3) -0.0078(3) -0.0073(3) I1 0.0468(7) 0.0465(8) 0.0475(9) -0.0240(7) -0.0070(6) -0.0096(6) I2 0.0431(7) 0.0259(6) 0.0371(8) -0.0106(5) -0.0041(5) -0.0067(5) I3 0.0450(6) 0.0308(6) 0.0258(7) -0.0039(5) -0.0035(5) -0.0083(5) I4 0.0484(7) 0.0328(7) 0.0282(7) 0.0025(5) -0.0090(5) -0.0101(5) I5 0.0408(6) 0.0302(6) 0.0295(7) -0.0050(5) -0.0015(5) -0.0103(5) I6 0.0528(8) 0.0533(9) 0.0387(9) 0.0093(7) -0.0120(6) -0.0197(7) I7 0.0392(6) 0.0224(6) 0.0500(9) -0.0040(6) -0.0087(6) -0.0078(5) N1 0.047(8) 0.021(7) 0.028(9) -0.011(6) -0.006(7) -0.004(6) N2 0.050(8) 0.020(7) 0.008(7) -0.001(5) 0.003(6) -0.007(6) C1 0.078(15) 0.071(16) 0.022(12) -0.031(12) 0.006(10) -0.013(13) C2 0.071(14) 0.072(16) 0.007(10) -0.016(10) 0.005(9) -0.015(12) C3 0.059(11) 0.038(11) 0.018(10) -0.008(8) -0.002(8) -0.015(9) C4 0.048(11) 0.036(11) 0.034(12) -0.002(9) 0.004(9) -0.008(9) C5 0.040(10) 0.036(10) 0.042(13) -0.009(9) -0.019(9) -0.003(8) C6 0.049(10) 0.033(10) 0.032(12) 0.000(8) -0.014(8) -0.012(8) I8 0.0471(7) 0.0301(6) 0.0233(7) -0.0032(5) -0.0060(5) -0.0111(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I3 3.0890(15) . ? Pb1 I1 3.1534(14) . ? Pb1 I5 3.1954(13) . ? Pb1 I2 3.2459(13) . ? Pb1 I4 3.3431(14) . ? Pb1 I2 3.4085(16) 2_665 ? Pb2 I6 2.9864(16) . ? Pb2 I8 3.2185(13) . ? Pb2 I3 3.2213(13) . ? Pb2 I7 3.2751(13) . ? Pb2 I7 3.2795(13) 2_566 ? Pb3 I8 3.0988(14) . ? Pb3 I1 3.1469(14) 1_455 ? Pb3 I5 3.1792(13) . ? Pb3 I2 3.2514(13) 1_455 ? Pb3 I4 3.3476(15) 2_565 ? Pb3 I4 3.3721(14) . ? I1 Pb3 3.1469(14) 1_655 ? I2 Pb3 3.2514(13) 1_655 ? I2 Pb1 3.4085(16) 2_665 ? I4 Pb3 3.3476(15) 2_565 ? I7 Pb2 3.2795(13) 2_566 ? N1 C3 1.48(2) . ? N1 C5 1.50(2) . ? N1 C1 1.50(2) . ? N2 C6 1.46(2) . ? N2 C2 1.48(2) . ? N2 C4 1.49(2) . ? C1 C2 1.44(3) . ? C3 C4 1.51(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 I3 Pb1 I1 89.52(4) . . ? I3 Pb1 I5 91.59(4) . . ? I1 Pb1 I5 90.35(3) . . ? I3 Pb1 I2 90.21(4) . . ? I1 Pb1 I2 91.50(3) . . ? I5 Pb1 I2 177.43(4) . . ? I3 Pb1 I4 89.60(4) . . ? I1 Pb1 I4 177.97(4) . . ? I5 Pb1 I4 91.50(3) . . ? I2 Pb1 I4 86.67(3) . . ? I3 Pb1 I2 176.79(4) . 2_665 ? I1 Pb1 I2 93.04(4) . 2_665 ? I5 Pb1 I2 90.34(4) . 2_665 ? I2 Pb1 I2 87.77(4) . 2_665 ? I4 Pb1 I2 87.78(3) . 2_665 ? I6 Pb2 I8 85.53(4) . . ? I6 Pb2 I3 85.39(4) . . ? I8 Pb2 I3 89.49(3) . . ? I6 Pb2 I7 94.87(4) . . ? I8 Pb2 I7 179.24(4) . . ? I3 Pb2 I7 89.89(3) . . ? I6 Pb2 I7 95.13(4) . 2_566 ? I8 Pb2 I7 89.94(3) . 2_566 ? I3 Pb2 I7 179.19(4) . 2_566 ? I7 Pb2 I7 90.67(3) . 2_566 ? I8 Pb3 I1 88.38(4) . 1_455 ? I8 Pb3 I5 91.86(4) . . ? I1 Pb3 I5 91.50(4) 1_455 . ? I8 Pb3 I2 88.85(4) . 1_455 ? I1 Pb3 I2 91.51(3) 1_455 1_455 ? I5 Pb3 I2 176.92(4) . 1_455 ? I8 Pb3 I4 177.46(4) . 2_565 ? I1 Pb3 I4 94.04(4) 1_455 2_565 ? I5 Pb3 I4 88.80(4) . 2_565 ? I2 Pb3 I4 90.35(4) 1_455 2_565 ? I8 Pb3 I4 89.60(4) . . ? I1 Pb3 I4 176.64(4) 1_455 . ? I5 Pb3 I4 91.25(3) . . ? I2 Pb3 I4 85.75(3) 1_455 . ? I4 Pb3 I4 87.94(4) 2_565 . ? Pb3 I1 Pb1 90.18(4) 1_655 . ? Pb1 I2 Pb3 86.74(3) . 1_655 ? Pb1 I2 Pb1 92.23(4) . 2_665 ? Pb3 I2 Pb1 91.19(4) 1_655 2_665 ? Pb1 I3 Pb2 97.77(4) . . ? Pb1 I4 Pb3 90.68(4) . 2_565 ? Pb1 I4 Pb3 85.68(3) . . ? Pb3 I4 Pb3 92.06(4) 2_565 . ? Pb3 I5 Pb1 91.50(3) . . ? Pb2 I7 Pb2 89.33(3) . 2_566 ? C3 N1 C5 110.8(16) . . ? C3 N1 C1 107.9(15) . . ? C5 N1 C1 107.2(15) . . ? C6 N2 C2 108.5(15) . . ? C6 N2 C4 111.1(14) . . ? C2 N2 C4 108.2(16) . . ? C2 C1 N1 110.3(19) . . ? C1 C2 N2 111.6(16) . . ? N1 C3 C4 110.7(15) . . ? N2 C4 C3 108.6(15) . . ? N1 C5 C6 108.9(14) . . ? N2 C6 C5 109.8(15) . . ? Pb3 I8 Pb2 97.60(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 5.327 _refine_diff_density_min -4.298 _refine_diff_density_rms 0.613 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 745951' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H22 I6 N2 O Pb2' _chemical_formula_weight 1338.06 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' O O 0.0106 0.0060 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9629(3) _cell_length_b 14.8833(6) _cell_length_c 21.0907(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.165(3) _cell_angle_gamma 90.00 _cell_volume 2485.09(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 20.982 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.107 _exptl_absorpt_correction_T_max 0.123 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type siements _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17700 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6130 _reflns_number_gt 3829 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker _computing_cell_refinement Bruker _computing_data_reduction Bruker _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0534P)^2^+20.4927P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6130 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.25297(6) 0.92686(4) 0.03558(3) 0.03897(15) Uani 1 1 d . . . Pb2 Pb 0.24367(7) 1.21168(4) -0.08533(3) 0.04066(15) Uani 1 1 d . . . I1 I 0.07994(14) 0.73410(7) 0.02046(6) 0.0625(3) Uani 1 1 d . . . I2 I 0.44264(13) 0.85808(8) 0.16392(5) 0.0546(3) Uani 1 1 d . . . I3 I -0.04785(11) 1.00782(7) 0.10409(4) 0.0446(2) Uani 1 1 d . . . I4 I 0.43108(11) 1.12193(6) 0.04790(4) 0.0411(2) Uani 1 1 d . . . I5 I 0.08251(18) 1.29859(10) -0.21189(6) 0.0807(4) Uani 1 1 d . . . I6 I 0.40084(12) 1.38195(6) -0.03098(5) 0.0474(3) Uani 1 1 d . . . N1 N -0.2239(15) 1.4601(9) -0.1816(5) 0.049(3) Uani 1 1 d . . . N2 N 0.0441(15) 1.5884(8) -0.1377(5) 0.045(3) Uani 1 1 d . . . C1 C -0.018(2) 1.5215(11) -0.0963(7) 0.055(4) Uani 1 1 d . . . H1A H -0.0059 1.5441 -0.0529 0.066 Uiso 1 1 calc R . . H1B H 0.0509 1.4679 -0.0972 0.066 Uiso 1 1 calc R . . C2 C -0.2061(19) 1.4958(11) -0.1153(6) 0.049(4) Uani 1 1 d . . . H2A H -0.2411 1.4507 -0.0863 0.059 Uiso 1 1 calc R . . H2B H -0.2774 1.5483 -0.1129 0.059 Uiso 1 1 calc R . . C3 C -0.1658(19) 1.5307(11) -0.2242(7) 0.050(4) Uani 1 1 d . . . H3A H -0.1804 1.5092 -0.2678 0.061 Uiso 1 1 calc R . . H3B H -0.2354 1.5838 -0.2218 0.061 Uiso 1 1 calc R . . C4 C 0.0104(18) 1.5548(11) -0.2073(7) 0.053(4) Uani 1 1 d . . . H4A H 0.0415 1.6015 -0.2359 0.063 Uiso 1 1 calc R . . H4B H 0.0809 1.5029 -0.2128 0.063 Uiso 1 1 calc R . . C5 C -0.4024(19) 1.4292(12) -0.1996(8) 0.062(5) Uani 1 1 d . . . H5A H -0.4338 1.3885 -0.1670 0.074 Uiso 1 1 calc R . . H5B H -0.4768 1.4809 -0.2002 0.074 Uiso 1 1 calc R . . C6 C -0.429(2) 1.3847(14) -0.2606(9) 0.079(6) Uani 1 1 d . . . H6A H -0.5458 1.3672 -0.2688 0.119 Uiso 1 1 calc R . . H6B H -0.3590 1.3323 -0.2602 0.119 Uiso 1 1 calc R . . H6C H -0.4014 1.4249 -0.2935 0.119 Uiso 1 1 calc R . . C7 C 0.2283(19) 1.6075(12) -0.1187(9) 0.062(5) Uani 1 1 d . . . H7A H 0.2458 1.6164 -0.0729 0.074 Uiso 1 1 calc R . . H7B H 0.2937 1.5554 -0.1288 0.074 Uiso 1 1 calc R . . C8 C 0.292(2) 1.6864(14) -0.1502(9) 0.078(6) Uani 1 1 d . . . H8A H 0.4111 1.6928 -0.1375 0.118 Uiso 1 1 calc R . . H8D H 0.2343 1.7392 -0.1379 0.118 Uiso 1 1 calc R . . H8B H 0.2732 1.6790 -0.1956 0.118 Uiso 1 1 calc R . . OW1 O 0.1878(18) 0.2706(10) 0.1405(7) 0.094(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0350(3) 0.0400(3) 0.0425(3) 0.0036(2) 0.0068(2) 0.0012(2) Pb2 0.0426(3) 0.0341(3) 0.0454(3) -0.0021(2) 0.0049(2) -0.0011(2) I1 0.0575(6) 0.0476(6) 0.0857(9) -0.0116(6) 0.0226(6) -0.0071(5) I2 0.0536(6) 0.0684(7) 0.0412(6) 0.0054(5) 0.0032(4) 0.0099(5) I3 0.0447(5) 0.0539(6) 0.0367(5) 0.0004(4) 0.0109(4) 0.0044(4) I4 0.0455(5) 0.0355(5) 0.0431(5) -0.0015(4) 0.0089(4) 0.0024(4) I5 0.0972(10) 0.0760(9) 0.0663(8) 0.0000(7) -0.0036(7) 0.0242(7) I6 0.0475(5) 0.0358(5) 0.0576(6) -0.0009(4) 0.0009(4) -0.0065(4) N1 0.063(8) 0.053(8) 0.033(7) -0.001(6) 0.008(6) -0.004(6) N2 0.058(7) 0.050(7) 0.027(6) -0.002(5) 0.008(5) 0.005(6) C1 0.074(11) 0.046(9) 0.046(9) 0.005(7) 0.007(8) 0.007(8) C2 0.070(10) 0.049(9) 0.028(8) 0.000(6) 0.011(7) -0.002(8) C3 0.065(10) 0.060(10) 0.028(7) -0.006(7) 0.013(7) -0.017(8) C4 0.054(9) 0.058(10) 0.047(9) -0.011(8) 0.014(7) -0.003(8) C5 0.051(9) 0.071(12) 0.065(12) -0.001(9) 0.015(8) -0.009(8) C6 0.090(14) 0.087(15) 0.060(12) -0.010(11) 0.004(10) -0.029(11) C7 0.055(10) 0.058(11) 0.068(12) -0.013(9) -0.011(8) 0.006(8) C8 0.073(12) 0.089(15) 0.072(14) -0.002(11) 0.003(10) -0.026(11) _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 3.1268(11) . ? Pb1 I3 3.1656(10) . ? Pb1 I1 3.1836(12) . ? Pb1 I4 3.2294(10) . ? Pb1 I4 3.3028(10) 3_675 ? Pb1 I3 3.3551(11) 3_575 ? Pb2 I6 2.9991(11) . ? Pb2 I5 3.1159(14) . ? Pb2 I1 3.1497(12) 3_575 ? Pb2 I2 3.3096(12) 3_675 ? Pb2 I4 3.3177(11) . ? I1 Pb2 3.1497(12) 3_575 ? I2 Pb2 3.3096(12) 3_675 ? I3 Pb1 3.3551(11) 3_575 ? I4 Pb1 3.3028(10) 3_675 ? N1 C3 1.487(18) . ? N1 C2 1.489(17) . ? N1 C5 1.503(19) . ? N2 C1 1.446(18) . ? N2 C7 1.505(19) . ? N2 C4 1.547(18) . ? C1 C2 1.56(2) . ? C3 C4 1.455(19) . ? C5 C6 1.44(2) . ? C7 C8 1.47(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 I3 92.77(3) . . ? I2 Pb1 I1 87.44(4) . . ? I3 Pb1 I1 92.76(3) . . ? I2 Pb1 I4 93.30(3) . . ? I3 Pb1 I4 88.19(3) . . ? I1 Pb1 I4 178.77(3) . . ? I2 Pb1 I4 93.71(3) . 3_675 ? I3 Pb1 I4 169.76(3) . 3_675 ? I1 Pb1 I4 95.44(3) . 3_675 ? I4 Pb1 I4 83.54(3) . 3_675 ? I2 Pb1 I3 177.73(3) . 3_575 ? I3 Pb1 I3 88.26(3) . 3_575 ? I1 Pb1 I3 90.49(3) . 3_575 ? I4 Pb1 I3 88.76(3) . 3_575 ? I4 Pb1 I3 85.56(3) 3_675 3_575 ? I6 Pb2 I5 95.35(4) . . ? I6 Pb2 I1 86.83(3) . 3_575 ? I5 Pb2 I1 89.13(4) . 3_575 ? I6 Pb2 I2 98.63(3) . 3_675 ? I5 Pb2 I2 87.98(3) . 3_675 ? I1 Pb2 I2 174.03(3) 3_575 3_675 ? I6 Pb2 I4 83.41(3) . . ? I5 Pb2 I4 177.59(4) . . ? I1 Pb2 I4 92.85(3) 3_575 . ? I2 Pb2 I4 90.16(3) 3_675 . ? Pb2 I1 Pb1 95.23(3) 3_575 . ? Pb1 I2 Pb2 89.40(3) . 3_675 ? Pb1 I3 Pb1 91.74(3) . 3_575 ? Pb1 I4 Pb1 96.46(3) . 3_675 ? Pb1 I4 Pb2 98.05(3) . . ? Pb1 I4 Pb2 86.34(3) 3_675 . ? C3 N1 C2 108.0(12) . . ? C3 N1 C5 114.2(12) . . ? C2 N1 C5 109.8(12) . . ? C1 N2 C7 110.9(12) . . ? C1 N2 C4 108.3(12) . . ? C7 N2 C4 112.2(11) . . ? N2 C1 C2 113.4(12) . . ? N1 C2 C1 108.7(12) . . ? C4 C3 N1 112.4(13) . . ? C3 C4 N2 112.1(12) . . ? C6 C5 N1 114.3(14) . . ? C8 C7 N2 114.0(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.886 _refine_diff_density_min -3.065 _refine_diff_density_rms 0.299 data_1 _database_code_depnum_ccdc_archive 'CCDC 745952' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H26 I6 N2 O Pb2' _chemical_formula_weight 1366.11 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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8807(5) _cell_length_b 11.6550(7) _cell_length_c 14.2611(10) _cell_angle_alpha 108.705(4) _cell_angle_beta 95.269(4) _cell_angle_gamma 92.523(4) _cell_volume 1387.99(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 18.787 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.133 _exptl_absorpt_correction_T_max 0.153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type siements _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10170 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.24 _reflns_number_total 6823 _reflns_number_gt 3734 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker _computing_cell_refinement Bruker _computing_data_reduction Bruker _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0150P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6823 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.47098(5) 0.53293(5) 0.17563(4) 0.04283(14) Uani 1 1 d . . . Pb2 Pb 0.05530(5) 0.69009(5) 0.12376(4) 0.04581(15) Uani 1 1 d . . . I1 I 0.52021(11) 0.39520(10) 0.32364(8) 0.0674(3) Uani 1 1 d . . . I2 I 0.78192(9) 0.70327(10) 0.25254(8) 0.0670(3) Uani 1 1 d . . . I3 I 0.36089(9) 0.67084(8) 0.00132(7) 0.0509(2) Uani 1 1 d . . . I4 I 0.14556(10) 0.37642(9) 0.09391(8) 0.0636(3) Uani 1 1 d . . . I5 I 0.29792(9) 0.73084(8) 0.31848(7) 0.0479(2) Uani 1 1 d . . . I6 I 0.06224(10) 0.95233(9) 0.14103(8) 0.0649(3) Uani 1 1 d . . . OW1 O -0.1088(14) 0.3102(12) 0.2622(11) 0.119(4) Uiso 1 1 d . . . N1 N 0.0379(13) 0.3765(10) 0.4489(9) 0.064(4) Uani 1 1 d . . . N2 N 0.4711(10) 0.0210(9) -0.0944(7) 0.042(3) Uani 1 1 d . . . C1 C -0.046(2) 0.4093(18) 0.5352(15) 0.112(7) Uani 1 1 d . . . H1A H -0.1123 0.3393 0.5322 0.134 Uiso 1 1 calc R . . H1B H 0.0251 0.4280 0.5948 0.134 Uiso 1 1 calc R . . C2 C 0.1362(17) 0.4897(16) 0.4559(15) 0.096(6) Uani 1 1 d . . . H2A H 0.2119 0.5090 0.5133 0.115 Uiso 1 1 calc R . . H2B H 0.1886 0.4744 0.3968 0.115 Uiso 1 1 calc R . . C3 C 0.148(2) 0.280(2) 0.4481(15) 0.110(7) Uani 1 1 d . . . H3A H 0.2083 0.2686 0.3928 0.132 Uiso 1 1 calc R . . H3B H 0.2159 0.3055 0.5095 0.132 Uiso 1 1 calc R . . C4 C 0.060(2) 0.1664(17) 0.4378(16) 0.114(7) Uani 1 1 d . . . H4A H -0.0072 0.1415 0.3761 0.136 Uiso 1 1 calc R . . H4B H -0.0016 0.1792 0.4925 0.136 Uiso 1 1 calc R . . C5 C 0.167(2) 0.0649(19) 0.4380(16) 0.149(10) Uani 1 1 d . . . H5A H 0.1080 -0.0084 0.4323 0.224 Uiso 1 1 calc R . . H5B H 0.2339 0.0897 0.4991 0.224 Uiso 1 1 calc R . . H5C H 0.2260 0.0507 0.3827 0.224 Uiso 1 1 calc R . . C6 C 0.5606(13) -0.0842(13) -0.0864(10) 0.054(4) Uani 1 1 d . . . H6A H 0.6351 -0.1009 -0.1338 0.065 Uiso 1 1 calc R . . H6B H 0.4934 -0.1568 -0.1000 0.065 Uiso 1 1 calc R . . C7 C 0.3613(14) 0.0456(14) -0.0197(10) 0.058(4) Uani 1 1 d . . . H7A H 0.2945 -0.0269 -0.0318 0.070 Uiso 1 1 calc R . . H7B H 0.2996 0.1094 -0.0274 0.070 Uiso 1 1 calc R . . C8 C 0.3855(16) -0.0129(14) -0.1987(10) 0.065(4) Uani 1 1 d . . . H8A H 0.3239 -0.0885 -0.2124 0.078 Uiso 1 1 calc R . . H8B H 0.3179 0.0496 -0.2005 0.078 Uiso 1 1 calc R . . C9 C 0.4884(17) -0.0272(16) -0.2779(11) 0.079(5) Uani 1 1 d . . . H9A H 0.5558 -0.0900 -0.2764 0.095 Uiso 1 1 calc R . . H9B H 0.5502 0.0483 -0.2643 0.095 Uiso 1 1 calc R . . C10 C 0.397(2) -0.0618(18) -0.3851(12) 0.108(7) Uani 1 1 d . . . H10A H 0.4674 -0.0701 -0.4339 0.162 Uiso 1 1 calc R . . H10B H 0.3319 0.0009 -0.3872 0.162 Uiso 1 1 calc R . . H10C H 0.3377 -0.1374 -0.3994 0.162 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 0.0396(3) 0.0482(3) 0.0411(3) 0.0146(3) 0.0049(2) 0.0056(2) Pb2 0.0406(3) 0.0526(3) 0.0456(3) 0.0179(3) 0.0050(2) 0.0037(2) I1 0.0714(6) 0.0787(8) 0.0623(7) 0.0376(7) 0.0041(5) 0.0090(5) I2 0.0425(5) 0.0939(8) 0.0588(7) 0.0185(6) 0.0091(5) -0.0127(5) I3 0.0563(5) 0.0518(6) 0.0500(6) 0.0196(5) 0.0205(5) 0.0082(4) I4 0.0538(5) 0.0656(7) 0.0634(7) 0.0178(6) -0.0128(5) -0.0145(5) I5 0.0517(5) 0.0493(6) 0.0408(5) 0.0107(5) 0.0092(4) 0.0060(4) I6 0.0596(6) 0.0584(6) 0.0777(8) 0.0278(6) -0.0048(5) -0.0013(5) N1 0.086(8) 0.051(8) 0.067(9) 0.025(7) 0.039(8) 0.027(7) N2 0.050(6) 0.050(7) 0.031(6) 0.022(6) -0.002(5) 0.005(5) C1 0.146(17) 0.098(15) 0.121(19) 0.059(15) 0.083(15) 0.014(14) C2 0.063(10) 0.095(15) 0.110(17) 0.001(13) 0.040(11) -0.010(10) C3 0.118(15) 0.14(2) 0.098(17) 0.067(16) 0.017(13) 0.019(15) C4 0.149(18) 0.070(13) 0.13(2) 0.040(15) 0.033(16) 0.015(14) C5 0.24(3) 0.119(19) 0.10(2) 0.044(17) 0.054(19) 0.08(2) C6 0.042(7) 0.067(10) 0.049(9) 0.017(8) -0.011(7) 0.008(7) C7 0.056(8) 0.072(11) 0.042(9) 0.011(8) 0.010(7) 0.006(8) C8 0.077(10) 0.072(11) 0.047(10) 0.025(9) -0.007(8) -0.004(8) C9 0.091(11) 0.096(14) 0.049(11) 0.031(11) -0.018(9) -0.012(10) C10 0.140(16) 0.140(19) 0.033(10) 0.022(12) -0.010(11) -0.002(14) _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 3.0479(10) . ? Pb1 I5 3.1154(10) . ? Pb1 I2 3.2146(11) . ? Pb1 I4 3.2545(10) . ? Pb1 I3 3.3761(10) 2_665 ? Pb2 I6 2.9839(11) . ? Pb2 I2 3.1562(10) 1_455 ? Pb2 I5 3.2472(11) . ? Pb2 I4 3.2767(11) 2_565 ? Pb2 I3 3.3372(9) . ? I2 Pb2 3.1562(10) 1_655 ? I3 Pb1 3.3761(10) 2_665 ? I4 Pb2 3.2767(11) 2_565 ? N1 C1 1.453(18) . ? N1 C3 1.52(2) . ? N1 C2 1.520(17) . ? N2 C7 1.479(14) . ? N2 C6 1.519(15) . ? N2 C8 1.527(16) . ? C1 C2 1.43(2) 2_566 ? C2 C1 1.43(2) 2_566 ? C3 C4 1.47(2) . ? C4 C5 1.55(2) . ? C6 C7 1.523(17) 2_655 ? C7 C6 1.523(17) 2_655 ? C8 C9 1.490(18) . ? C9 C10 1.583(19) . ? 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 I5 93.16(3) . . ? I1 Pb1 I2 95.07(3) . . ? I5 Pb1 I2 90.27(3) . . ? I1 Pb1 I4 88.40(3) . . ? I5 Pb1 I4 87.40(3) . . ? I2 Pb1 I4 175.92(3) . . ? I1 Pb1 I3 93.29(3) . 2_665 ? I5 Pb1 I3 173.16(3) . 2_665 ? I2 Pb1 I3 91.43(3) . 2_665 ? I4 Pb1 I3 90.51(3) . 2_665 ? I6 Pb2 I2 94.08(3) . 1_455 ? I6 Pb2 I5 95.01(3) . . ? I2 Pb2 I5 91.02(3) 1_455 . ? I6 Pb2 I4 89.06(3) . 2_565 ? I2 Pb2 I4 97.45(3) 1_455 2_565 ? I5 Pb2 I4 170.32(3) . 2_565 ? I6 Pb2 I3 87.90(3) . . ? I2 Pb2 I3 175.56(3) 1_455 . ? I5 Pb2 I3 84.83(2) . . ? I4 Pb2 I3 86.55(3) 2_565 . ? Pb2 I2 Pb1 123.74(4) 1_655 . ? Pb2 I3 Pb1 140.13(3) . 2_665 ? Pb1 I4 Pb2 129.79(3) . 2_565 ? Pb1 I5 Pb2 85.02(3) . . ? C1 N1 C3 113.9(13) . . ? C1 N1 C2 106.3(13) . . ? C3 N1 C2 105.3(12) . . ? C7 N2 C6 108.9(9) . . ? C7 N2 C8 109.4(9) . . ? C6 N2 C8 109.4(10) . . ? C2 C1 N1 114.9(14) 2_566 . ? C1 C2 N1 110.9(12) 2_566 . ? C4 C3 N1 108.4(15) . . ? C3 C4 C5 110.6(18) . . ? N2 C6 C7 106.5(11) . 2_655 ? N2 C7 C6 112.2(10) . 2_655 ? C9 C8 N2 112.9(11) . . ? C8 C9 C10 112.0(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.611 _refine_diff_density_min -1.735 _refine_diff_density_rms 0.277