# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chen, Zhi Rong' _publ_contact_author_email zrchen@fzu.edu.cn _publ_section_title ; Hybrid Polymeric Iodoplumbates Constructed from Morpholine and Its Derivatives: Structures and Properties ; loop_ _publ_author_name 'Hao-Hong Li' 'Zhi Rong Chen' 'Li-Chuan Cheng' 'Yun-Jie Wang' ; Miao Feng ; 'Min Wang' # Attachment '- new cif file of 2.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 733611' #TrackingRef '- new cif file of 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 I8 N2 O2 Pb3, 2(C3 H7 N O)' _chemical_formula_sum 'C16 H36 I8 N4 O4 Pb3' _chemical_formula_weight 1985.29 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 P1 _symmetry_space_group_name_Hall P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.4126(19) _cell_length_b 9.941(2) _cell_length_c 12.019(2) _cell_angle_alpha 66.53(3) _cell_angle_beta 76.86(3) _cell_angle_gamma 86.97(3) _cell_volume 1003.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 18.726 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 9822 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7459 _reflns_number_gt 5924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.0794P)^2^+1.6809P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(12) _refine_ls_number_reflns 7459 _refine_ls_number_parameters 231 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.004 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 0.88518(9) 0.46259(8) 0.35128(8) 0.0347(3) Uani 1 1 d . . . Pb3 Pb 0.8651(2) 1.1181(2) -0.3325(2) 0.03836(14) Uani 1 1 d . . . Pb2 Pb 0.84503(9) 0.77422(8) -0.01554(8) 0.0340(3) Uani 1 1 d . . . I7 I 0.5939(3) 0.9900(3) -0.1017(3) 0.0583(8) Uani 1 1 d . . . I4 I 0.6570(4) 0.7047(4) 0.2637(3) 0.0719(10) Uani 1 1 d . . . I8 I 0.9189(3) 0.7890(3) -0.2856(3) 0.0508(7) Uani 1 1 d . . . I6 I 1.0331(3) 1.0673(3) -0.1053(3) 0.0550(7) Uani 1 1 d . . . I3 I 0.8106(3) 0.4495(3) 0.6209(3) 0.0574(8) Uani 1 1 d . . . I1 I 0.6977(3) 0.1746(3) 0.4402(3) 0.0556(8) Uani 1 1 d . . . I2 I 1.1369(3) 0.2464(3) 0.4393(3) 0.0575(7) Uani 1 1 d . . . I5 I 1.0756(3) 0.5354(4) 0.0723(3) 0.0711(10) Uani 1 1 d . . . N1 N 1.2120(19) 0.9769(17) 0.2502(19) 0.032(5) Uiso 1 1 d D . . H1N H 1.2332 0.9569 0.3253 0.038 Uiso 1 1 calc R . . N2 N 1.5021(16) 1.2814(15) 0.0810(16) 0.019(3) Uiso 1 1 d D . . H2N H 1.4617 1.3154 0.0134 0.023 Uiso 1 1 calc R . . O1 O 1.042(2) 0.718(2) 0.301(2) 0.040(5) Uani 1 1 d D . . O2 O 1.687(3) 1.536(3) 0.008(3) 0.077(9) Uani 1 1 d D . . O3 O 1.350(3) -0.136(3) 0.437(3) 0.060(6) Uiso 1 1 d . . . N3 N 1.409(4) -0.171(3) 0.621(3) 0.051(8) Uiso 1 1 d D . . C1 C 1.262(2) 0.843(3) 0.207(3) 0.029(5) Uiso 1 1 d D . . H1A H 1.2424 0.8666 0.1255 0.035 Uiso 1 1 calc R . . H1B H 1.3660 0.8320 0.2000 0.035 Uiso 1 1 calc R . . C2 C 1.190(2) 0.713(3) 0.289(3) 0.042(5) Uiso 1 1 d D . . H2A H 1.2255 0.6362 0.2604 0.051 Uiso 1 1 calc R . . H2B H 1.2121 0.6880 0.3696 0.051 Uiso 1 1 calc R . . C3 C 0.983(2) 0.831(2) 0.356(2) 0.046(6) Uani 1 1 d D . . H3A H 0.8774 0.8348 0.3676 0.055 Uiso 1 1 calc R . . H3B H 1.0068 0.8063 0.4365 0.055 Uiso 1 1 calc R . . C4 C 1.0549(18) 0.978(2) 0.263(2) 0.032(4) Uiso 1 1 d D . . H4A H 1.0326 0.9997 0.1833 0.039 Uiso 1 1 calc R . . H4B H 1.0161 1.0547 0.2910 0.039 Uiso 1 1 calc R . . C5 C 1.284(3) 1.118(3) 0.159(3) 0.047(8) Uani 1 1 d D . . H5A H 1.2327 1.1967 0.1764 0.056 Uiso 1 1 calc R . . H5B H 1.2766 1.1290 0.0764 0.056 Uiso 1 1 calc R . . C6 C 1.446(3) 1.131(2) 0.160(3) 0.032(6) Uiso 1 1 d D . . H6A H 1.4566 1.1055 0.2441 0.038 Uiso 1 1 calc R . . H6B H 1.5021 1.0630 0.1285 0.038 Uiso 1 1 calc R . . C7 C 1.461(3) 1.372(3) 0.149(3) 0.048(8) Uani 1 1 d D . . H7A H 1.5048 1.3394 0.2203 0.058 Uiso 1 1 calc R . . H7B H 1.3553 1.3664 0.1785 0.058 Uiso 1 1 calc R . . C8 C 1.519(3) 1.545(3) 0.052(3) 0.056(7) Uiso 1 1 d D . . H8A H 1.4728 1.5792 -0.0186 0.068 Uiso 1 1 calc R . . H8B H 1.4971 1.6106 0.0947 0.068 Uiso 1 1 calc R . . C9 C 1.720(2) 1.443(2) -0.045(2) 0.034(5) Uiso 1 1 d D . . H9A H 1.8247 1.4463 -0.0738 0.041 Uiso 1 1 calc R . . H9B H 1.6772 1.4744 -0.1171 0.041 Uiso 1 1 calc R . . C10 C 1.6695(18) 1.288(2) 0.036(2) 0.031(4) Uiso 1 1 d D . . H10A H 1.7146 1.2521 0.1070 0.037 Uiso 1 1 calc R . . H10B H 1.6974 1.2265 -0.0103 0.037 Uiso 1 1 calc R . . C11 C 1.322(2) -0.111(2) 0.5384(19) 0.025(4) Uiso 1 1 d D . . H11 H 1.2451 -0.0538 0.5539 0.030 Uiso 1 1 calc R . . C12 C 1.331(5) -0.094(5) 0.709(5) 0.129(16) Uiso 1 1 d . . . H12A H 1.3766 -0.1207 0.7785 0.194 Uiso 1 1 calc R . . H12B H 1.2298 -0.1251 0.7389 0.194 Uiso 1 1 calc R . . H12C H 1.3399 0.0104 0.6637 0.194 Uiso 1 1 calc R . . C13 C 1.530(3) -0.256(3) 0.595(3) 0.055(6) Uiso 1 1 d . . . H13A H 1.5787 -0.2897 0.6630 0.083 Uiso 1 1 calc R . . H13B H 1.5970 -0.1969 0.5199 0.083 Uiso 1 1 calc R . . H13C H 1.4953 -0.3396 0.5859 0.083 Uiso 1 1 calc R . . O4 O 1.399(3) 0.357(3) -0.114(2) 0.063(7) Uani 1 1 d . . . N4 N 1.331(4) 0.403(3) -0.288(3) 0.049(8) Uani 1 1 d . . . C14 C 1.402(6) 0.367(5) -0.203(6) 0.107(17) Uiso 1 1 d . . . H14A H 1.4928 0.3390 -0.2338 0.128 Uiso 1 1 calc R . . C15 C 1.201(4) 0.475(5) -0.295(4) 0.104(13) Uiso 1 1 d . . . H15A H 1.1678 0.4969 -0.2231 0.156 Uiso 1 1 calc R . . H15B H 1.1289 0.4127 -0.2989 0.156 Uiso 1 1 calc R . . H15C H 1.2163 0.5641 -0.3688 0.156 Uiso 1 1 calc R . . C16 C 1.350(3) 0.391(3) -0.402(3) 0.070(7) Uiso 1 1 d . . . H16A H 1.4417 0.3490 -0.4196 0.104 Uiso 1 1 calc R . . H16B H 1.3477 0.4867 -0.4661 0.104 Uiso 1 1 calc R . . H16C H 1.2722 0.3293 -0.3982 0.104 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 0.0414(7) 0.0340(6) 0.0232(7) -0.0058(5) -0.0063(6) -0.0020(5) Pb3 0.0487(3) 0.0333(2) 0.0261(3) -0.0052(2) -0.0068(2) -0.0014(2) Pb2 0.0386(6) 0.0334(6) 0.0254(8) -0.0078(6) -0.0048(6) -0.0020(5) I7 0.0453(13) 0.0585(14) 0.073(2) -0.0270(14) -0.0185(13) 0.0164(11) I4 0.073(2) 0.108(2) 0.0353(19) -0.0292(18) -0.0224(17) 0.048(2) I8 0.0709(17) 0.0507(13) 0.0292(15) -0.0150(12) -0.0091(13) -0.0001(12) I6 0.0584(15) 0.0507(15) 0.052(2) -0.0126(14) -0.0154(14) -0.0156(12) I3 0.080(2) 0.0411(12) 0.050(2) -0.0241(13) -0.0041(16) 0.0072(13) I1 0.0652(17) 0.0482(14) 0.055(2) -0.0141(14) -0.0239(15) -0.0165(12) I2 0.0658(16) 0.0643(15) 0.0271(13) -0.0083(11) 0.0026(11) -0.0050(12) I5 0.0606(18) 0.108(2) 0.0342(19) -0.0215(18) -0.0106(15) 0.0392(18) O1 0.031(8) 0.047(9) 0.043(12) -0.034(9) 0.022(6) -0.025(7) O2 0.086(17) 0.078(15) 0.048(16) -0.010(12) 0.005(12) -0.041(13) C3 0.031(10) 0.056(13) 0.052(15) -0.019(12) -0.015(10) -0.001(9) C5 0.053(13) 0.044(12) 0.021(13) 0.014(8) -0.012(9) -0.017(9) C7 0.058(14) 0.038(12) 0.033(15) -0.007(10) 0.010(9) -0.023(10) O4 0.089(15) 0.087(14) 0.010(9) -0.008(8) -0.027(9) 0.008(11) N4 0.055(13) 0.062(14) 0.022(10) -0.003(8) -0.016(8) -0.007(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 I3 3.106(4) . ? Pb1 I1 3.114(3) . ? Pb1 I4 3.158(3) . ? Pb1 I2 3.185(3) . ? Pb1 I5 3.233(4) . ? Pb3 I8 3.124(3) . ? Pb3 I3 3.149(3) 1_564 ? Pb3 I2 3.172(4) 1_564 ? Pb3 I7 3.185(4) . ? Pb3 I1 3.302(4) 1_564 ? Pb3 I6 3.316(4) . ? Pb2 O2 2.74(2) 1_445 ? Pb2 I8 3.106(3) . ? Pb2 I5 3.156(3) . ? Pb2 I6 3.156(3) . ? Pb2 I7 3.173(3) . ? Pb2 I4 3.234(4) . ? I3 Pb3 3.149(3) 1_546 ? I1 Pb3 3.302(4) 1_546 ? I2 Pb3 3.172(4) 1_546 ? N1 C4 1.45(2) . ? N1 C5 1.468(16) . ? N1 C1 1.62(3) . ? N1 H1N 0.9100 . ? N2 C7 1.42(3) . ? N2 C6 1.464(16) . ? N2 C10 1.54(2) . ? N2 H2N 0.9100 . ? O1 C2 1.36(3) . ? O1 C3 1.54(3) . ? O2 C9 1.31(3) . ? O2 C8 1.56(4) . ? O2 Pb2 2.74(2) 1_665 ? O3 C11 1.31(3) . ? N3 C11 1.360(18) . ? N3 C13 1.43(4) . ? N3 C12 1.58(5) . ? C1 C2 1.37(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.52(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.545(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.68(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.49(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O4 C14 1.04(6) . ? N4 C14 1.27(5) . ? N4 C15 1.39(5) . ? N4 C16 1.39(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 90.17(10) . . ? I3 Pb1 I4 93.17(9) . . ? I1 Pb1 I4 101.74(11) . . ? I3 Pb1 I2 85.04(9) . . ? I1 Pb1 I2 84.36(9) . . ? I4 Pb1 I2 173.67(11) . . ? I3 Pb1 I5 157.74(11) . . ? I1 Pb1 I5 108.80(12) . . ? I4 Pb1 I5 94.17(11) . . ? I2 Pb1 I5 85.36(9) . . ? I8 Pb3 I3 179.86(14) . 1_564 ? I8 Pb3 I2 95.57(10) . 1_564 ? I3 Pb3 I2 84.54(10) 1_564 1_564 ? I8 Pb3 I7 84.61(9) . . ? I3 Pb3 I7 95.28(10) 1_564 . ? I2 Pb3 I7 179.41(14) 1_564 . ? I8 Pb3 I1 94.01(9) . 1_564 ? I3 Pb3 I1 86.10(10) 1_564 1_564 ? I2 Pb3 I1 81.56(10) 1_564 1_564 ? I7 Pb3 I1 99.00(10) . 1_564 ? I8 Pb3 I6 86.96(9) . . ? I3 Pb3 I6 92.94(9) 1_564 . ? I2 Pb3 I6 98.24(10) 1_564 . ? I7 Pb3 I6 81.20(10) . . ? I1 Pb3 I6 179.03(10) 1_564 . ? O2 Pb2 I8 77.8(7) 1_445 . ? O2 Pb2 I5 82.6(8) 1_445 . ? I8 Pb2 I5 93.73(9) . . ? O2 Pb2 I6 167.5(7) 1_445 . ? I8 Pb2 I6 90.14(9) . . ? I5 Pb2 I6 101.39(10) . . ? O2 Pb2 I7 92.0(8) 1_445 . ? I8 Pb2 I7 85.11(9) . . ? I5 Pb2 I7 174.58(11) . . ? I6 Pb2 I7 83.92(9) . . ? O2 Pb2 I4 83.4(7) 1_445 . ? I8 Pb2 I4 158.44(11) . . ? I5 Pb2 I4 94.20(10) . . ? I6 Pb2 I4 107.86(11) . . ? I7 Pb2 I4 85.10(9) . . ? Pb2 I7 Pb3 76.82(8) . . ? Pb1 I4 Pb2 85.79(8) . . ? Pb2 I8 Pb3 78.70(8) . . ? Pb2 I6 Pb3 75.19(7) . . ? Pb1 I3 Pb3 78.26(8) . 1_546 ? Pb1 I1 Pb3 75.89(7) . 1_546 ? Pb3 I2 Pb1 76.77(8) 1_546 . ? Pb2 I5 Pb1 85.83(8) . . ? C4 N1 C5 111.8(19) . . ? C4 N1 C1 104.3(14) . . ? C5 N1 C1 112(2) . . ? C4 N1 H1N 109.6 . . ? C5 N1 H1N 109.6 . . ? C1 N1 H1N 109.6 . . ? C7 N2 C6 109.4(18) . . ? C7 N2 C10 110.1(15) . . ? C6 N2 C10 111.1(16) . . ? C7 N2 H2N 108.7 . . ? C6 N2 H2N 108.7 . . ? C10 N2 H2N 108.7 . . ? C2 O1 C3 109.6(16) . . ? C9 O2 C8 112(2) . . ? C9 O2 Pb2 130.2(18) . 1_665 ? C8 O2 Pb2 113.9(17) . 1_665 ? C11 N3 C13 121(3) . . ? C11 N3 C12 94(3) . . ? C13 N3 C12 145(3) . . ? C2 C1 N1 112.2(18) . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? N1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O1 C2 C1 113(2) . . ? O1 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? O1 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 O1 106.0(17) . . ? C4 C3 H3A 110.5 . . ? O1 C3 H3A 110.5 . . ? C4 C3 H3B 110.5 . . ? O1 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? N1 C4 C3 111.1(16) . . ? N1 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 113.2(17) . . ? N1 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N1 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N2 C6 C5 109.1(15) . . ? N2 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N2 C6 H6B 109.9 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C8 107.4(19) . . ? N2 C7 H7A 110.2 . . ? C8 C7 H7A 110.3 . . ? N2 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O2 C8 C7 105(2) . . ? O2 C8 H8A 110.8 . . ? C7 C8 H8A 110.8 . . ? O2 C8 H8B 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? O2 C9 C10 115(2) . . ? O2 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? O2 C9 H9B 108.5 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C9 C10 N2 108.7(15) . . ? C9 C10 H10A 110.0 . . ? N2 C10 H10A 109.9 . . ? C9 C10 H10B 109.9 . . ? N2 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O3 C11 N3 118(2) . . ? O3 C11 H11 120.9 . . ? N3 C11 H11 120.9 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.4 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 N4 C15 129(4) . . ? C14 N4 C16 136(4) . . ? C15 N4 C16 95(3) . . ? O4 C14 N4 146(6) . . ? O4 C14 H14A 107.2 . . ? N4 C14 H14A 107.3 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.4 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.974 _refine_diff_density_min -2.752 _refine_diff_density_rms 0.318 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chen, Zhi Rong' _publ_contact_author_email zrchen@fzu.edu.cn _publ_section_title ; Hybrid Polymeric Iodoplumbates Constructed from Morpholine and Its Derivatives: Structures and Properties ; loop_ _publ_author_name 'Hao-Hong Li' 'Zhi Rong Chen' 'Li-Chuan Cheng' 'Yun-Jie Wang' ; Miao Feng ; 'Min Wang' data_lihh _database_code_depnum_ccdc_archive 'CCDC 681701' #TrackingRef '- CIF-3(681701).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I6 Pb2,C6 H12 N O,C5 H10 N O,C3 H7 N O' _chemical_formula_sum 'C14 H29 I6 N3 O3 Pb2' _chemical_formula_weight 1463.20 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8467(18) _cell_length_b 12.084(2) _cell_length_c 15.236(3) _cell_angle_alpha 109.71(3) _cell_angle_beta 96.64(3) _cell_angle_gamma 98.58(3) _cell_volume 1491.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 17.497 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.021 _exptl_absorpt_correction_T_max 0.043 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 14424 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.1136 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6758 _reflns_number_gt 4163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.0788P)^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 6758 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.52171(6) 0.94701(6) 0.33973(4) 0.03830(18) Uani 1 1 d . . . Pb2 Pb -0.00970(6) 0.80840(6) 0.40177(4) 0.03814(18) Uani 1 1 d . . . I1 I 0.78661(12) 1.18378(11) 0.42038(8) 0.0502(3) Uani 1 1 d . . . I2 I 0.44395(14) 1.02925(12) 0.18266(8) 0.0559(3) Uani 1 1 d . . . I3 I 0.70534(12) 0.76016(11) 0.22382(7) 0.0495(3) Uani 1 1 d . . . I4 I 0.21995(12) 0.72155(10) 0.26393(8) 0.0446(3) Uani 1 1 d . . . I5 I 0.25894(12) 1.08883(10) 0.45617(8) 0.0453(3) Uani 1 1 d . . . I6 I -0.12301(18) 0.56836(16) 0.38029(12) 0.0802(5) Uani 1 1 d . . . O1 O 0.1663(13) 0.3497(12) 0.2387(9) 0.056(4) Uani 1 1 d . . . O2 O 0.5972(14) 0.3192(13) 0.1148(9) 0.063(4) Uani 1 1 d . . . O3 O 1.0153(14) 0.7708(11) 0.0298(9) 0.057(4) Uani 1 1 d . . . N1 N 0.4108(14) 0.4777(13) 0.4043(9) 0.042(3) Uani 1 1 d . . . N2 N 0.8296(14) 0.4043(11) 0.0235(8) 0.036(3) Uani 1 1 d . . . N3 N 0.9360(13) 0.9418(12) 0.1014(9) 0.038(3) Uani 1 1 d . . . C1 C 0.1489(18) 0.3478(18) 0.3255(12) 0.053(5) Uani 1 1 d . . . H1A H 0.1800 0.2767 0.3316 0.063 Uiso 1 1 calc R . . H1B H 0.0400 0.3420 0.3305 0.063 Uiso 1 1 calc R . . C2 C 0.2422(19) 0.4566(17) 0.4058(11) 0.049(5) Uani 1 1 d . . . H2A H 0.2032 0.5267 0.4036 0.059 Uiso 1 1 calc R . . H2B H 0.2266 0.4478 0.4652 0.059 Uiso 1 1 calc R . . C3 C 0.4354(19) 0.4688(18) 0.3036(10) 0.050(5) Uani 1 1 d . . . H3A H 0.4187 0.5419 0.2942 0.060 Uiso 1 1 calc R . . H3B H 0.5420 0.4621 0.2979 0.060 Uiso 1 1 calc R . . C4 C 0.326(2) 0.3608(19) 0.2259(14) 0.064(6) Uani 1 1 d . . . H4A H 0.3317 0.3684 0.1649 0.077 Uiso 1 1 calc R . . H4B H 0.3605 0.2881 0.2247 0.077 Uiso 1 1 calc R . . C5 C 0.5016(18) 0.6049(16) 0.4698(11) 0.043(4) Uani 1 1 d . . . H5A H 0.6075 0.6164 0.4586 0.051 Uiso 1 1 calc R . . H5B H 0.4527 0.6655 0.4562 0.051 Uiso 1 1 calc R . . C6 C 0.502(2) 0.6173(18) 0.5717(11) 0.057(5) Uani 1 1 d . . . H6A H 0.3955 0.6041 0.5823 0.069 Uiso 1 1 calc R . . H6B H 0.5532 0.6979 0.6131 0.069 Uiso 1 1 calc R . . C7 C 0.751(3) 0.3231(19) 0.1388(14) 0.064(6) Uani 1 1 d . . . H7A H 0.7731 0.2460 0.1029 0.077 Uiso 1 1 calc R . . H7B H 0.7727 0.3335 0.2053 0.077 Uiso 1 1 calc R . . C8 C 0.8614(18) 0.4189(17) 0.1234(11) 0.048(5) Uani 1 1 d . . . H8A H 0.8478 0.4975 0.1626 0.058 Uiso 1 1 calc R . . H8B H 0.9677 0.4122 0.1408 0.058 Uiso 1 1 calc R . . C9 C 0.6580(18) 0.394(2) -0.0069(12) 0.053(5) Uani 1 1 d . . . H9A H 0.6282 0.4699 0.0253 0.064 Uiso 1 1 calc R . . H9B H 0.6343 0.3765 -0.0746 0.064 Uiso 1 1 calc R . . C10 C 0.570(2) 0.296(2) 0.0177(14) 0.065(6) Uani 1 1 d . . . H10A H 0.4596 0.2869 -0.0038 0.078 Uiso 1 1 calc R . . H10B H 0.6001 0.2211 -0.0153 0.078 Uiso 1 1 calc R . . C11 C 0.9155(18) 0.5016(17) 0.0025(13) 0.052(5) Uani 1 1 d . . . H11A H 0.9099 0.5769 0.0506 0.063 Uiso 1 1 calc R . . H11B H 0.8645 0.5007 -0.0577 0.063 Uiso 1 1 calc R . . C12 C 1.0189(18) 0.8617(15) 0.0954(12) 0.045(4) Uani 1 1 d . . . H12 H 1.0916 0.8758 0.1492 0.054 Uiso 1 1 calc R . . C13 C 0.816(2) 0.929(2) 0.0220(10) 0.059(6) Uani 1 1 d . . . H13A H 0.7668 0.9968 0.0385 0.088 Uiso 1 1 calc R . . H13B H 0.7402 0.8569 0.0079 0.088 Uiso 1 1 calc R . . H13C H 0.8630 0.9245 -0.0326 0.088 Uiso 1 1 calc R . . C14 C 0.940(3) 1.0483(18) 0.1840(14) 0.074(7) Uani 1 1 d . . . H14A H 0.8669 1.0930 0.1686 0.111 Uiso 1 1 calc R . . H14B H 1.0426 1.0974 0.2024 0.111 Uiso 1 1 calc R . . H14C H 0.9136 1.0246 0.2353 0.111 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 0.0339(3) 0.0416(4) 0.0383(3) 0.0117(3) 0.0041(2) 0.0124(3) Pb2 0.0318(3) 0.0397(4) 0.0386(3) 0.0085(3) 0.0078(2) 0.0065(2) I1 0.0432(6) 0.0528(7) 0.0428(6) 0.0099(5) -0.0033(4) 0.0005(5) I2 0.0573(7) 0.0569(8) 0.0536(7) 0.0225(6) -0.0029(5) 0.0158(6) I3 0.0446(6) 0.0581(7) 0.0436(6) 0.0109(5) 0.0035(4) 0.0248(5) I4 0.0411(5) 0.0432(6) 0.0491(6) 0.0146(5) 0.0142(4) 0.0075(5) I5 0.0504(6) 0.0399(6) 0.0478(6) 0.0129(5) 0.0189(4) 0.0142(5) I6 0.0736(10) 0.0791(11) 0.0829(10) 0.0263(9) 0.0144(7) 0.0067(8) O1 0.042(6) 0.056(8) 0.055(7) 0.009(6) -0.015(5) 0.009(6) O2 0.051(8) 0.071(10) 0.059(8) 0.017(7) 0.024(6) 0.000(7) O3 0.069(8) 0.039(7) 0.056(8) 0.002(6) 0.017(6) 0.022(6) N1 0.035(7) 0.050(8) 0.040(7) 0.018(6) -0.004(5) 0.013(6) N2 0.044(7) 0.029(7) 0.033(7) 0.007(6) 0.016(5) 0.003(6) N3 0.029(6) 0.043(8) 0.044(7) 0.017(6) 0.013(5) 0.009(6) C1 0.032(8) 0.057(12) 0.045(10) 0.000(9) -0.003(7) -0.011(8) C2 0.054(10) 0.047(11) 0.039(9) 0.009(8) 0.008(7) -0.002(8) C3 0.042(9) 0.067(12) 0.032(8) 0.009(8) -0.006(6) 0.008(8) C4 0.048(10) 0.071(14) 0.054(11) 0.000(10) 0.001(8) 0.014(10) C5 0.043(9) 0.047(10) 0.038(8) 0.012(7) 0.005(6) 0.020(8) C6 0.052(10) 0.060(12) 0.035(9) 0.004(9) -0.018(7) -0.011(9) C7 0.095(16) 0.055(12) 0.051(11) 0.019(10) 0.038(10) 0.019(11) C8 0.035(8) 0.056(11) 0.041(9) 0.005(8) -0.010(6) 0.014(8) C9 0.036(9) 0.077(14) 0.046(10) 0.024(9) 0.017(7) 0.000(9) C10 0.060(12) 0.068(14) 0.057(12) 0.017(11) 0.011(9) -0.005(10) C11 0.042(9) 0.053(12) 0.053(10) 0.010(9) 0.000(7) 0.011(8) C12 0.039(9) 0.040(10) 0.047(9) 0.006(8) 0.005(7) 0.007(7) C13 0.049(10) 0.095(16) 0.026(8) 0.014(9) 0.002(6) 0.018(10) C14 0.113(18) 0.042(12) 0.048(12) 0.000(9) 0.013(11) -0.003(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 2.9352(16) . ? Pb1 I3 3.1504(15) . ? Pb1 I1 3.1860(19) . ? Pb1 I4 3.2982(19) . ? Pb1 I5 3.4029(15) . ? Pb2 I6 2.818(2) . ? Pb2 I4 3.1266(14) . ? Pb2 I1 3.1275(16) 2_676 ? Pb2 I3 3.3109(17) 1_455 ? Pb2 I5 3.3461(15) 2_576 ? I1 Pb2 3.1275(16) 2_676 ? I3 Pb2 3.3109(17) 1_655 ? I5 Pb2 3.3461(15) 2_576 ? O1 C1 1.36(2) . ? O1 C4 1.44(2) . ? O2 C7 1.36(2) . ? O2 C10 1.39(2) . ? O3 C12 1.203(17) . ? N1 C2 1.48(2) . ? N1 C3 1.54(2) . ? N1 C5 1.55(2) . ? N1 C6 1.59(2) 2_666 ? N2 C11 1.45(3) . ? N2 C8 1.46(2) . ? N2 C9 1.51(2) . ? N3 C12 1.28(2) . ? N3 C14 1.46(2) . ? N3 C13 1.462(19) . ? C1 C2 1.51(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.54(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.51(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.59(2) 2_666 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.50(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.50(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C11 1.51(3) 2_765 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 93.28(4) . . ? I2 Pb1 I1 84.60(5) . . ? I3 Pb1 I1 100.56(4) . . ? I2 Pb1 I4 93.75(5) . . ? I3 Pb1 I4 85.66(4) . . ? I1 Pb1 I4 173.63(3) . . ? I2 Pb1 I5 90.78(4) . . ? I3 Pb1 I5 166.26(4) . . ? I1 Pb1 I5 92.87(4) . . ? I4 Pb1 I5 80.98(4) . . ? I6 Pb2 I4 89.47(5) . . ? I6 Pb2 I1 84.94(6) . 2_676 ? I4 Pb2 I1 93.70(4) . 2_676 ? I6 Pb2 I3 85.07(6) . 1_455 ? I4 Pb2 I3 92.11(4) . 1_455 ? I1 Pb2 I3 168.38(4) 2_676 1_455 ? I6 Pb2 I5 92.72(5) . 2_576 ? I4 Pb2 I5 177.08(4) . 2_576 ? I1 Pb2 I5 88.42(4) 2_676 2_576 ? I3 Pb2 I5 86.16(4) 1_455 2_576 ? Pb2 I1 Pb1 111.69(5) 2_676 . ? Pb1 I3 Pb2 96.14(4) . 1_655 ? Pb2 I4 Pb1 103.72(4) . . ? Pb2 I5 Pb1 167.78(5) 2_576 . ? C1 O1 C4 112.7(13) . . ? C7 O2 C10 106.1(14) . . ? C2 N1 C3 109.0(11) . . ? C2 N1 C5 114.4(12) . . ? C3 N1 C5 104.7(14) . . ? C2 N1 C6 114.6(15) . 2_666 ? C3 N1 C6 105.9(12) . 2_666 ? C5 N1 C6 107.5(11) . 2_666 ? C11 N2 C8 113.4(13) . . ? C11 N2 C9 109.0(14) . . ? C8 N2 C9 109.5(11) . . ? C12 N3 C14 126.9(16) . . ? C12 N3 C13 120.8(14) . . ? C14 N3 C13 112.2(15) . . ? O1 C1 C2 113.4(17) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C1 114.1(13) . . ? N1 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 N1 112.6(17) . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N1 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? O1 C4 C3 113.5(13) . . ? O1 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? O1 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 N1 109.0(15) . . ? C6 C5 H5A 109.9 . . ? N1 C5 H5A 109.9 . . ? C6 C5 H5B 109.9 . . ? N1 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 C6 N1 110.1(13) . 2_666 ? C5 C6 H6A 109.6 . . ? N1 C6 H6A 109.6 2_666 . ? C5 C6 H6B 109.6 . . ? N1 C6 H6B 109.6 2_666 . ? H6A C6 H6B 108.2 . . ? O2 C7 C8 116.6(19) . . ? O2 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? O2 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? N2 C8 C7 108.6(13) . . ? N2 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? N2 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 N2 108.6(17) . . ? C10 C9 H9A 110.0 . . ? N2 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? N2 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O2 C10 C9 112.2(16) . . ? O2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? O2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N2 C11 C11 116(2) . 2_765 ? N2 C11 H11A 108.4 . . ? C11 C11 H11A 108.4 2_765 . ? N2 C11 H11B 108.4 . . ? C11 C11 H11B 108.4 2_765 . ? H11A C11 H11B 107.5 . . ? O3 C12 N3 128.8(16) . . ? O3 C12 H12 115.6 . . ? N3 C12 H12 115.6 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.801 _refine_diff_density_min -5.020 _refine_diff_density_rms 0.338 # Attachment '- new cif of 2(733611).cif' data_b _database_code_depnum_ccdc_archive 'CCDC 733611' #TrackingRef '- new cif of 2(733611).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 I8 N2 O2 Pb3, 2(C3 H7 N O)' _chemical_formula_sum 'C16 H36 I8 N4 O4 Pb3' _chemical_formula_weight 1985.29 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4126(19) _cell_length_b 9.941(2) _cell_length_c 12.019(2) _cell_angle_alpha 66.53(3) _cell_angle_beta 76.86(3) _cell_angle_gamma 86.97(3) _cell_volume 1003.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 18.726 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 9822 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4546 _reflns_number_gt 3726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.0786P)^2^+3.4050P] 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 4546 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.0000 0.0000 1.0000 0.03820(16) Uani 1 2 d S . . Pb2 Pb 0.02010(4) 0.34416(4) 0.68342(4) 0.03410(14) Uani 1 1 d . . . I1 I -0.16773(9) 0.05359(9) 0.77276(9) 0.0552(2) Uani 1 1 d . . . I2 I 0.27143(9) 0.12826(10) 0.77061(9) 0.0566(2) Uani 1 1 d . . . I3 I -0.05409(10) 0.33031(9) 0.95331(9) 0.0532(2) Uani 1 1 d . . . I4 I 0.20929(11) 0.41508(13) 0.40422(9) 0.0710(3) Uani 1 1 d . . . N1 N 0.3555(8) 0.8461(9) 0.5845(8) 0.0300(17) Uani 1 1 d . . . H1C H 0.3872 0.8188 0.6563 0.036 Uiso 1 1 calc R . . N2 N 0.5398(11) 0.7128(11) 0.9544(10) 0.049(2) Uani 1 1 d . . . O1 O 0.1783(9) 0.5912(10) 0.6448(10) 0.058(3) Uani 1 1 d . . . O2 O 0.4758(12) 0.7518(12) 0.7767(10) 0.067(3) Uani 1 1 d . . . C1 C 0.4021(11) 0.7330(12) 0.5291(13) 0.043(3) Uani 1 1 d . . . H1A H 0.3723 0.7613 0.4510 0.052 Uiso 1 1 calc R . . H1B H 0.5075 0.7271 0.5129 0.052 Uiso 1 1 calc R . . C2 C 0.3321(14) 0.5872(14) 0.6192(16) 0.060(4) Uani 1 1 d . . . H2A H 0.3624 0.5140 0.5851 0.072 Uiso 1 1 calc R . . H2B H 0.3648 0.5585 0.6962 0.072 Uiso 1 1 calc R . . C3 C 0.1318(14) 0.6937(17) 0.6998(15) 0.066(4) Uani 1 1 d . . . H3A H 0.1633 0.6636 0.7773 0.079 Uiso 1 1 calc R . . H3B H 0.0260 0.6938 0.7188 0.079 Uiso 1 1 calc R . . C4 C 0.1916(10) 0.8444(13) 0.6162(14) 0.049(3) Uani 1 1 d . . . H4A H 0.1593 0.9110 0.6570 0.059 Uiso 1 1 calc R . . H4B H 0.1556 0.8774 0.5405 0.059 Uiso 1 1 calc R . . C5 C 0.4189(10) 0.9942(11) 0.4997(11) 0.039(2) Uani 1 1 d . . . H5A H 0.3657 1.0669 0.5257 0.047 Uiso 1 1 calc R . . H5B H 0.4095 1.0142 0.4159 0.047 Uiso 1 1 calc R . . C6 C 0.4582(14) 0.7658(15) 0.8727(16) 0.057(3) Uani 1 1 d . . . H6A H 0.3792 0.8193 0.8916 0.068 Uiso 1 1 calc R . . C7 C 0.498(3) 0.746(4) 1.063(2) 0.140(11) Uani 1 1 d . . . H7A H 0.4110 0.8007 1.0594 0.209 Uiso 1 1 calc R . . H7B H 0.5754 0.8040 1.0651 0.209 Uiso 1 1 calc R . . H7C H 0.4810 0.6568 1.1361 0.209 Uiso 1 1 calc R . . C8 C 0.6656(18) 0.634(2) 0.939(2) 0.095(7) Uani 1 1 d . . . H8A H 0.6789 0.6209 0.8623 0.142 Uiso 1 1 calc R . . H8B H 0.6547 0.5391 1.0072 0.142 Uiso 1 1 calc R . . H8C H 0.7490 0.6865 0.9374 0.142 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 0.0485(3) 0.0333(3) 0.0261(3) -0.0054(2) -0.0068(2) -0.0013(2) Pb2 0.0397(2) 0.0336(2) 0.0240(2) -0.00674(16) -0.00549(16) -0.00191(15) I1 0.0616(5) 0.0501(4) 0.0529(6) -0.0135(4) -0.0195(4) -0.0160(4) I2 0.0542(4) 0.0605(5) 0.0476(6) -0.0164(4) -0.0075(4) 0.0062(4) I3 0.0743(5) 0.0456(4) 0.0391(5) -0.0195(4) -0.0069(4) 0.0038(4) I4 0.0664(5) 0.1071(8) 0.0343(5) -0.0250(5) -0.0163(4) 0.0438(6) N1 0.027(3) 0.036(4) 0.027(5) -0.012(4) -0.005(3) -0.007(3) N2 0.056(5) 0.054(5) 0.033(6) -0.009(5) -0.017(5) -0.006(5) O1 0.053(4) 0.059(5) 0.061(7) -0.036(5) 0.017(4) -0.029(4) O2 0.081(6) 0.078(6) 0.033(6) -0.006(5) -0.024(5) -0.005(5) C1 0.040(5) 0.041(5) 0.054(8) -0.025(6) -0.009(5) 0.002(4) C2 0.056(7) 0.051(7) 0.080(12) -0.028(7) -0.022(7) -0.007(6) C3 0.051(6) 0.087(10) 0.062(11) -0.046(9) 0.020(6) -0.029(7) C4 0.019(4) 0.059(7) 0.074(10) -0.041(7) 0.008(5) -0.009(4) C5 0.039(5) 0.037(5) 0.036(7) -0.007(5) -0.009(5) -0.005(4) C6 0.047(6) 0.060(7) 0.062(11) -0.025(7) -0.010(6) 0.007(6) C7 0.15(2) 0.23(3) 0.069(17) -0.10(2) 0.001(15) -0.02(2) C8 0.064(9) 0.092(12) 0.106(18) -0.006(11) -0.042(10) 0.025(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 I3 3.1371(11) . ? Pb1 I3 3.1371(11) 2_557 ? Pb1 I2 3.1775(17) . ? Pb1 I2 3.1775(17) 2_557 ? Pb1 I1 3.3087(12) . ? Pb1 I1 3.3087(12) 2_557 ? Pb2 I3 3.1069(12) . ? Pb2 I1 3.1351(14) . ? Pb2 I4 3.1590(14) 2_566 ? Pb2 I2 3.1779(14) . ? Pb2 I4 3.2343(16) . ? I4 Pb2 3.1590(14) 2_566 ? N1 C5 1.478(12) . ? N1 C4 1.502(11) . ? N1 C1 1.521(13) . ? N1 H1C 0.9100 . ? N2 C6 1.311(18) . ? N2 C8 1.404(19) . ? N2 C7 1.43(2) . ? O1 C2 1.412(15) . ? O1 C3 1.422(15) . ? O2 C6 1.191(18) . ? C1 C2 1.495(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.485(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C5 1.539(19) 2_676 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 I3 180.0 . 2_557 ? I3 Pb1 I2 84.56(4) . . ? I3 Pb1 I2 95.44(4) 2_557 . ? I3 Pb1 I2 95.44(4) . 2_557 ? I3 Pb1 I2 84.56(4) 2_557 2_557 ? I2 Pb1 I2 180.0 . 2_557 ? I3 Pb1 I1 86.55(4) . . ? I3 Pb1 I1 93.45(4) 2_557 . ? I2 Pb1 I1 81.40(3) . . ? I2 Pb1 I1 98.60(3) 2_557 . ? I3 Pb1 I1 93.45(4) . 2_557 ? I3 Pb1 I1 86.55(4) 2_557 2_557 ? I2 Pb1 I1 98.60(3) . 2_557 ? I2 Pb1 I1 81.40(3) 2_557 2_557 ? I1 Pb1 I1 180.0 . 2_557 ? I3 Pb2 I1 90.17(4) . . ? I3 Pb2 I4 93.42(4) . 2_566 ? I1 Pb2 I4 101.59(4) . 2_566 ? I3 Pb2 I2 85.05(4) . . ? I1 Pb2 I2 84.15(3) . . ? I4 Pb2 I2 174.08(3) 2_566 . ? I3 Pb2 I4 158.11(3) . . ? I1 Pb2 I4 108.28(5) . . ? I4 Pb2 I4 94.22(4) 2_566 . ? I2 Pb2 I4 85.25(4) . . ? Pb2 I1 Pb1 75.52(3) . . ? Pb1 I2 Pb2 76.82(4) . . ? Pb2 I3 Pb1 78.45(4) . . ? Pb2 I4 Pb2 85.78(4) 2_566 . ? C5 N1 C4 111.5(8) . . ? C5 N1 C1 112.0(9) . . ? C4 N1 C1 108.2(7) . . ? C5 N1 H1C 108.3 . . ? C4 N1 H1C 108.3 . . ? C1 N1 H1C 108.3 . . ? C6 N2 C8 124.5(14) . . ? C6 N2 C7 115.9(16) . . ? C8 N2 C7 119.5(17) . . ? C2 O1 C3 110.0(10) . . ? C2 C1 N1 108.8(10) . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O1 C2 C1 111.6(11) . . ? O1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O1 C3 C4 111.8(11) . . ? O1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? O1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 N1 110.0(10) . . ? C3 C4 H4A 109.7 . . ? N1 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? N1 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N1 C5 C5 110.6(11) . 2_676 ? N1 C5 H5A 109.5 . . ? C5 C5 H5A 109.5 2_676 . ? N1 C5 H5B 109.5 . . ? C5 C5 H5B 109.5 2_676 . ? H5A C5 H5B 108.1 . . ? O2 C6 N2 126.0(13) . . ? O2 C6 H6A 117.0 . . ? N2 C6 H6A 117.0 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.007 _refine_diff_density_min -3.151 _refine_diff_density_rms 0.322 # Attachment '- CIF-1(757317).cif' data_wyj001 _database_code_depnum_ccdc_archive 'CCDC 757317' #TrackingRef '- CIF-1(757317).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I15 Pb4, 5(C4 H12 N O)' _chemical_formula_sum 'C20 H60 I15 N5 O5 Pb4' _chemical_formula_weight 3183.03 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' P P 0.1023 0.0942 '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 Pnma _symmetry_space_group_name_Hall -P2ac2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 34.7456(17) _cell_length_b 23.7703(10) _cell_length_c 9.0704(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7491.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5512 _exptl_absorpt_coefficient_mu 15.168 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 52697 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8775 _reflns_number_gt 7859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.1035P)^2^+44.0815P] 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 8775 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1992 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.007 _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 0.116358(14) 0.661672(18) 0.15933(5) 0.04281(15) Uani 1 1 d . . . Pb2 Pb 0.123302(15) 0.48896(2) 0.18651(6) 0.04872(16) Uani 1 1 d . . . I1 I 0.04320(3) 0.7500 0.12191(15) 0.0494(3) Uani 1 2 d S . . I2 I 0.07930(3) 0.57181(4) -0.06533(10) 0.0547(2) Uani 1 1 d . . . I3 I 0.19202(3) 0.58681(4) 0.15220(11) 0.0552(2) Uani 1 1 d . . . I4 I 0.08539(3) 0.58477(4) 0.42171(10) 0.0553(2) Uani 1 1 d . . . I5 I 0.15260(4) 0.7500 -0.08570(15) 0.0575(3) Uani 1 2 d S . . I6 I 0.14293(5) 0.7500 0.41031(16) 0.0630(4) Uani 1 2 d S . . I7 I 0.04349(3) 0.42635(4) 0.20482(12) 0.0661(3) Uani 1 1 d . . . I8 I 0.15553(3) 0.41632(5) -0.06486(12) 0.0675(3) Uani 1 1 d . . . I9 I 0.17025(4) 0.43068(5) 0.43395(13) 0.0763(3) Uani 1 1 d . . . O1 O -0.0614(4) 0.6277(6) 0.3570(15) 0.087(4) Uani 1 1 d . . . H21A H -0.0425 0.6383 0.4304 0.104 Uiso 1 1 calc R . . H21B H -0.0851 0.6479 0.3781 0.104 Uiso 1 1 calc R . . O2 O 0.2358(4) 0.6146(6) -0.3766(18) 0.102(4) Uani 1 1 d . . . H22A H 0.2435 0.6289 -0.2808 0.122 Uiso 1 1 calc R . . H22B H 0.2518 0.6328 -0.4503 0.122 Uiso 1 1 calc R . . O3 O 0.0646(7) 0.7500 0.695(3) 0.157(13) Uani 1 2 d S . . H23A H 0.0822 0.7500 0.6117 0.188 Uiso 1 2 calc SR . . H23B H 0.0799 0.7500 0.7842 0.188 Uiso 1 2 calc SR . . N1 N -0.0145(4) 0.5537(6) 0.1952(15) 0.067(3) Uani 1 1 d . . . H31A H 0.0082 0.5363 0.1819 0.081 Uiso 1 1 calc R . . H31B H -0.0306 0.5417 0.1242 0.081 Uiso 1 1 calc R . . N2 N 0.1792(5) 0.5397(7) -0.2804(19) 0.087(5) Uani 1 1 d . . . H32A H 0.1697 0.5233 -0.3620 0.104 Uiso 1 1 calc R . . H32B H 0.1667 0.5253 -0.2022 0.104 Uiso 1 1 calc R . . N3 N -0.0086(5) 0.7500 0.569(2) 0.079(6) Uani 1 2 d S . . H33A H -0.0246 0.7500 0.4909 0.095 Uiso 1 2 calc SR . . H33B H -0.0229 0.7500 0.6514 0.095 Uiso 1 2 calc SR . . C1 C -0.0089(5) 0.6144(6) 0.1785(17) 0.063(4) Uani 1 1 d . . . H1A H -0.0008 0.6232 0.0788 0.076 Uiso 1 1 calc R . . H1B H 0.0107 0.6276 0.2464 0.076 Uiso 1 1 calc R . . C2 C -0.0477(5) 0.6430(8) 0.212(2) 0.081(5) Uani 1 1 d . . . H2A H -0.0447 0.6835 0.2067 0.097 Uiso 1 1 calc R . . H2B H -0.0665 0.6318 0.1389 0.097 Uiso 1 1 calc R . . C3 C -0.0683(6) 0.5692(9) 0.364(2) 0.085(6) Uani 1 1 d . . . H3A H -0.0867 0.5584 0.2891 0.102 Uiso 1 1 calc R . . H3B H -0.0790 0.5596 0.4598 0.102 Uiso 1 1 calc R . . C4 C -0.0304(5) 0.5372(7) 0.3407(19) 0.071(4) Uani 1 1 d . . . H4A H -0.0122 0.5465 0.4182 0.085 Uiso 1 1 calc R . . H4B H -0.0350 0.4969 0.3431 0.085 Uiso 1 1 calc R . . C5 C 0.2208(7) 0.5263(8) -0.268(2) 0.090(6) Uani 1 1 d . . . H5A H 0.2302 0.5383 -0.1722 0.108 Uiso 1 1 calc R . . H5B H 0.2243 0.4859 -0.2748 0.108 Uiso 1 1 calc R . . C6 C 0.2429(6) 0.5534(8) -0.381(3) 0.093(6) Uani 1 1 d . . . H6A H 0.2355 0.5387 -0.4770 0.111 Uiso 1 1 calc R . . H6B H 0.2700 0.5459 -0.3668 0.111 Uiso 1 1 calc R . . C7 C 0.1965(7) 0.6291(10) -0.403(2) 0.103(8) Uani 1 1 d . . . H7A H 0.1888 0.6167 -0.5002 0.124 Uiso 1 1 calc R . . H7B H 0.1933 0.6696 -0.3974 0.124 Uiso 1 1 calc R . . C8 C 0.1717(5) 0.6010(10) -0.288(2) 0.091(7) Uani 1 1 d . . . H8A H 0.1768 0.6178 -0.1922 0.109 Uiso 1 1 calc R . . H8B H 0.1448 0.6073 -0.3111 0.109 Uiso 1 1 calc R . . C9 C 0.0411(9) 0.6980(9) 0.690(2) 0.125(11) Uani 1 1 d . . . H9A H 0.0578 0.6655 0.6824 0.150 Uiso 1 1 calc R . . H9B H 0.0263 0.6947 0.7804 0.150 Uiso 1 1 calc R . . C10 C 0.0152(7) 0.6993(7) 0.565(2) 0.098(7) Uani 1 1 d . . . H10A H -0.0012 0.6663 0.5670 0.118 Uiso 1 1 calc R . . H10B H 0.0299 0.6985 0.4743 0.118 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 0.0497(3) 0.0391(3) 0.0397(3) -0.00127(16) -0.00128(19) 0.00099(17) Pb2 0.0516(3) 0.0514(3) 0.0432(3) -0.00014(19) -0.0031(2) 0.0014(2) I1 0.0461(6) 0.0472(6) 0.0550(7) 0.000 0.0030(5) 0.000 I2 0.0612(5) 0.0603(5) 0.0427(5) -0.0032(3) -0.0126(4) 0.0011(4) I3 0.0464(5) 0.0631(5) 0.0560(5) -0.0007(4) -0.0020(4) 0.0064(4) I4 0.0648(5) 0.0599(5) 0.0412(5) 0.0004(4) 0.0080(4) -0.0035(4) I5 0.0637(7) 0.0621(7) 0.0466(7) 0.000 0.0142(6) 0.000 I6 0.0876(10) 0.0503(7) 0.0510(7) 0.000 -0.0269(7) 0.000 I7 0.0661(6) 0.0716(6) 0.0606(6) 0.0022(4) -0.0041(5) -0.0176(5) I8 0.0744(7) 0.0723(6) 0.0558(6) -0.0115(5) -0.0005(5) 0.0083(5) I9 0.0876(8) 0.0874(8) 0.0538(6) 0.0101(5) -0.0096(5) 0.0225(6) O1 0.082(8) 0.095(9) 0.083(9) -0.027(7) 0.026(7) 0.002(7) O2 0.090(9) 0.096(10) 0.119(12) 0.026(9) 0.013(9) -0.014(8) O3 0.093(18) 0.27(4) 0.11(2) 0.000 -0.047(15) 0.000 N1 0.075(8) 0.067(8) 0.060(8) -0.012(6) -0.004(6) -0.005(7) N2 0.086(10) 0.085(10) 0.089(12) -0.017(9) 0.024(9) -0.030(8) N3 0.053(10) 0.131(19) 0.054(12) 0.000 -0.020(9) 0.000 C1 0.072(9) 0.061(9) 0.056(9) 0.001(6) 0.002(7) -0.017(7) C2 0.075(11) 0.079(11) 0.088(14) 0.015(10) 0.003(10) -0.002(9) C3 0.076(12) 0.113(16) 0.065(11) 0.021(10) 0.001(9) -0.036(10) C4 0.073(10) 0.075(10) 0.066(10) -0.003(8) -0.006(8) -0.021(8) C5 0.127(18) 0.073(11) 0.069(12) 0.017(9) 0.014(12) 0.026(11) C6 0.077(12) 0.093(14) 0.107(16) 0.012(12) 0.038(11) 0.016(10) C7 0.126(18) 0.120(17) 0.065(12) 0.017(11) -0.014(12) 0.061(14) C8 0.067(10) 0.149(19) 0.055(10) -0.003(11) -0.008(8) 0.055(12) C9 0.22(3) 0.093(15) 0.057(11) -0.017(10) -0.035(15) 0.086(18) C10 0.18(2) 0.048(9) 0.070(12) -0.004(8) 0.001(13) -0.031(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 I3 3.1752(10) . ? Pb1 I4 3.1880(10) . ? Pb1 I2 3.2207(10) . ? Pb1 I6 3.2315(11) . ? Pb1 I5 3.3066(11) . ? Pb1 I1 3.3144(10) . ? Pb2 I8 3.0715(11) . ? Pb2 I9 3.1012(12) . ? Pb2 I7 3.1518(11) . ? Pb2 I3 3.3478(11) . ? Pb2 I2 3.3813(10) . ? Pb2 I4 3.3873(10) . ? I1 Pb1 3.3144(10) 7_575 ? I5 Pb1 3.3066(11) 7_575 ? I6 Pb1 3.2315(11) 7_575 ? O1 C3 1.41(2) . ? O1 C2 1.44(2) . ? O1 H21A 0.9700 . ? O1 H21B 0.9700 . ? O2 C7 1.43(2) . ? O2 C6 1.48(2) . ? O2 H22A 0.9700 . ? O2 H22B 0.9700 . ? O3 C9 1.48(3) . ? O3 C9 1.48(3) 7_575 ? O3 H23A 0.9700 . ? O3 H23B 0.9700 . ? N1 C1 1.46(2) . ? N1 C4 1.48(2) . ? N1 H31A 0.9000 . ? N1 H31B 0.9000 . ? N2 C8 1.48(3) . ? N2 C5 1.49(3) . ? N2 H32A 0.9000 . ? N2 H32B 0.9000 . ? N3 C10 1.46(2) 7_575 ? N3 C10 1.46(2) . ? N3 H33A 0.9000 . ? N3 H33B 0.9000 . ? C1 C2 1.54(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.54(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.44(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.51(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.45(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 I4 88.47(3) . . ? I3 Pb1 I2 86.93(3) . . ? I4 Pb1 I2 87.54(3) . . ? I3 Pb1 I6 98.16(3) . . ? I4 Pb1 I6 86.74(3) . . ? I2 Pb1 I6 172.23(4) . . ? I3 Pb1 I5 91.54(3) . . ? I4 Pb1 I5 173.93(3) . . ? I2 Pb1 I5 98.52(3) . . ? I6 Pb1 I5 87.26(3) . . ? I3 Pb1 I1 171.09(3) . . ? I4 Pb1 I1 100.42(3) . . ? I2 Pb1 I1 92.80(3) . . ? I6 Pb1 I1 83.09(3) . . ? I5 Pb1 I1 79.69(3) . . ? I8 Pb2 I9 95.41(3) . . ? I8 Pb2 I7 95.42(3) . . ? I9 Pb2 I7 102.35(4) . . ? I8 Pb2 I3 93.53(3) . . ? I9 Pb2 I3 90.14(3) . . ? I7 Pb2 I3 163.85(3) . . ? I8 Pb2 I2 89.47(3) . . ? I9 Pb2 I2 170.71(3) . . ? I7 Pb2 I2 85.00(3) . . ? I3 Pb2 I2 81.66(3) . . ? I8 Pb2 I4 170.86(3) . . ? I9 Pb2 I4 92.82(3) . . ? I7 Pb2 I4 86.68(3) . . ? I3 Pb2 I4 82.46(3) . . ? I2 Pb2 I4 81.84(3) . . ? Pb1 I1 Pb1 78.62(3) 7_575 . ? Pb1 I2 Pb2 77.18(2) . . ? Pb1 I3 Pb2 78.29(2) . . ? Pb1 I4 Pb2 77.53(2) . . ? Pb1 I5 Pb1 78.84(3) . 7_575 ? Pb1 I6 Pb1 81.04(3) . 7_575 ? C3 O1 C2 110.2(14) . . ? C3 O1 H21A 109.6 . . ? C2 O1 H21A 109.6 . . ? C3 O1 H21B 109.6 . . ? C2 O1 H21B 109.6 . . ? H21A O1 H21B 108.1 . . ? C7 O2 C6 113.0(16) . . ? C7 O2 H22A 109.0 . . ? C6 O2 H22A 109.0 . . ? C7 O2 H22B 109.0 . . ? C6 O2 H22B 109.0 . . ? H22A O2 H22B 107.8 . . ? C9 O3 C9 113(3) . 7_575 ? C9 O3 H23A 109.0 . . ? C9 O3 H23A 109.0 7_575 . ? C9 O3 H23B 109.0 . . ? C9 O3 H23B 109.0 7_575 . ? H23A O3 H23B 107.8 . . ? C1 N1 C4 113.7(13) . . ? C1 N1 H31A 108.8 . . ? C4 N1 H31A 108.8 . . ? C1 N1 H31B 108.8 . . ? C4 N1 H31B 108.8 . . ? H31A N1 H31B 107.7 . . ? C8 N2 C5 112.7(14) . . ? C8 N2 H32A 109.0 . . ? C5 N2 H32A 109.0 . . ? C8 N2 H32B 109.0 . . ? C5 N2 H32B 109.0 . . ? H32A N2 H32B 107.8 . . ? C10 N3 C10 111(2) 7_575 . ? C10 N3 H33A 109.4 7_575 . ? C10 N3 H33A 109.4 . . ? C10 N3 H33B 109.4 7_575 . ? C10 N3 H33B 109.4 . . ? H33A N3 H33B 108.0 . . ? N1 C1 C2 107.3(13) . . ? N1 C1 H1A 110.3 . . ? C2 C1 H1A 110.3 . . ? N1 C1 H1B 110.3 . . ? C2 C1 H1B 110.3 . . ? H1A C1 H1B 108.5 . . ? O1 C2 C1 111.1(15) . . ? O1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? O1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O1 C3 C4 109.7(14) . . ? O1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N1 C4 C3 108.1(14) . . ? N1 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N1 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C6 C5 N2 111.6(17) . . ? C6 C5 H5A 109.3 . . ? N2 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? N2 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 O2 109.5(15) . . ? C5 C6 H6A 109.8 . . ? O2 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? O2 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? O2 C7 C8 109.1(14) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N2 C8 C7 111.4(14) . . ? N2 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 O3 110.4(19) . . ? C10 C9 H9A 109.6 . . ? O3 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? O3 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C9 C10 N3 110.5(15) . . ? C9 C10 H10A 109.5 . . ? N3 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.776 _refine_diff_density_min -2.039 _refine_diff_density_rms 0.289