# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Using alcohols as alkylation reagents for 4-cyanopyridinium and N,N'-dialkyl-4,4'-bipyridinium and their one-dimensional iodoplumbates ; loop_ _publ_author_name 'Yang Chen' 'Zhou Yang' 'Cheng-Xin Guo' 'Chun-Yan Ni' 'Hong-Xi Li' ; Zhi-Gang Ren ; 'Jian-Ping Lang' #===END #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 765929' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I9 Pb3, C14 H18 N2, C7 H9 N' _chemical_formula_sum 'C21 H27 I9 N3 Pb3' _chemical_formula_weight 2085.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.026(2) _cell_length_b 14.039(3) _cell_length_c 24.770(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.44(3) _cell_angle_gamma 90.00 _cell_volume 4181.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11960 _cell_measurement_theta_min 3.0163 _cell_measurement_theta_max 27.6021 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3588 _exptl_absorpt_coefficient_mu 18.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1431 _exptl_absorpt_correction_T_max 0.1657 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19117 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9316 _reflns_number_gt 6458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0462P)^2^+25.5108P] 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 SHELXL _refine_ls_extinction_coef 0.000128(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9316 _refine_ls_number_parameters 326 _refine_ls_number_restraints 206 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.088 _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 0.66879(5) 0.99913(5) 0.05618(2) 0.04446(17) Uani 1 1 d . . . Pb2 Pb 0.33942(6) 0.84203(6) 0.11912(3) 0.0618(2) Uani 1 1 d . . . Pb3 Pb 1.00489(5) 0.82585(5) 0.00086(3) 0.0527(2) Uani 1 1 d . . . I1 I 0.88656(12) 0.66385(11) -0.05465(7) 0.0896(5) Uani 1 1 d . . . I2 I 0.45947(13) 0.66680(12) 0.15693(8) 0.1079(6) Uani 1 1 d . . . I3 I 0.22331(14) 0.87719(16) 0.22416(6) 0.1129(7) Uani 1 1 d . . . I4 I 0.83779(9) 0.84509(9) 0.10524(5) 0.0578(3) Uani 1 1 d . . . I5 I 0.49869(9) 0.84479(8) -0.00161(4) 0.0504(3) Uani 1 1 d . . . I6 I 0.83181(8) 0.99372(8) -0.05071(4) 0.0469(3) Uani 1 1 d . . . I7 I 0.81241(10) 1.17644(9) 0.09547(5) 0.0607(3) Uani 1 1 d . . . I8 I 0.52985(10) 0.99120(10) 0.16293(5) 0.0645(4) Uani 1 1 d . . . I9 I 0.14862(10) 0.69439(10) 0.07447(6) 0.0752(4) Uani 1 1 d . . . N1 N 1.1007(14) 0.9074(17) -0.2455(8) 0.097(5) Uani 1 1 d U . . N2 N 0.5684(12) 0.7412(12) -0.1843(7) 0.068(4) Uani 1 1 d U . . N3 N 0.2363(13) 0.0246(12) 0.4411(8) 0.080(4) Uani 1 1 d U . . C1 C 1.057(2) 0.8349(19) -0.2743(11) 0.117(8) Uani 1 1 d U . . H1A H 1.0978 0.8084 -0.3028 0.141 Uiso 1 1 calc R . . C2 C 0.9555(18) 0.7997(17) -0.2629(10) 0.103(7) Uani 1 1 d U . . H2A H 0.9271 0.7487 -0.2833 0.123 Uiso 1 1 calc R . . C3 C 0.8940(14) 0.8364(13) -0.2227(7) 0.057(4) Uani 1 1 d U . . C4 C 0.9401(15) 0.9110(16) -0.1939(7) 0.076(5) Uani 1 1 d U . . H4A H 0.9000 0.9399 -0.1658 0.091 Uiso 1 1 calc R . . C5 C 1.0434(16) 0.9422(19) -0.2062(7) 0.086(6) Uani 1 1 d U . . H5A H 1.0748 0.9913 -0.1853 0.103 Uiso 1 1 calc R . . C6 C 0.6295(15) 0.7822(14) -0.1467(8) 0.070(5) Uani 1 1 d U . . H6A H 0.6007 0.7916 -0.1119 0.084 Uiso 1 1 calc R . . C7 C 0.7366(14) 0.8115(12) -0.1586(6) 0.059(4) Uani 1 1 d U . . H7A H 0.7812 0.8373 -0.1309 0.071 Uiso 1 1 calc R . . C8 C 0.7799(13) 0.8037(13) -0.2102(7) 0.053(4) Uani 1 1 d U . . C9 C 0.7109(18) 0.7609(17) -0.2470(8) 0.092(6) Uani 1 1 d U . . H9A H 0.7352 0.7529 -0.2827 0.110 Uiso 1 1 calc R . . C10 C 0.6038(18) 0.7282(17) -0.2327(8) 0.092(6) Uani 1 1 d U . . H10A H 0.5586 0.6973 -0.2584 0.110 Uiso 1 1 calc R . . C11 C 1.2124(18) 0.945(2) -0.2602(12) 0.128(9) Uani 1 1 d U . . H11A H 1.2480 0.9714 -0.2278 0.154 Uiso 1 1 calc R . . H11B H 1.2585 0.8921 -0.2728 0.154 Uiso 1 1 calc R . . C12 C 1.209(2) 1.019(2) -0.3022(12) 0.127(10) Uani 1 1 d U . . H12A H 1.2841 1.0413 -0.3093 0.190 Uiso 1 1 calc R . . H12B H 1.1641 1.0721 -0.2900 0.190 Uiso 1 1 calc R . . H12C H 1.1772 0.9929 -0.3351 0.190 Uiso 1 1 calc R . . C13 C 0.4556(16) 0.7075(16) -0.1711(11) 0.094(6) Uani 1 1 d U . . H13A H 0.4269 0.7442 -0.1406 0.112 Uiso 1 1 calc R . . H13B H 0.4061 0.7181 -0.2021 0.112 Uiso 1 1 calc R . . C14 C 0.4559(18) 0.6074(17) -0.1575(10) 0.104(8) Uani 1 1 d U . . H14A H 0.3809 0.5872 -0.1491 0.156 Uiso 1 1 calc R . . H14B H 0.5039 0.5969 -0.1264 0.156 Uiso 1 1 calc R . . H14C H 0.4832 0.5708 -0.1879 0.156 Uiso 1 1 calc R . . C15 C 0.3040(17) 0.0979(14) 0.4422(11) 0.099(7) Uani 1 1 d U . . H15A H 0.2824 0.1563 0.4268 0.119 Uiso 1 1 calc R . . C16 C 0.4066(17) 0.0880(15) 0.4662(10) 0.096(7) Uani 1 1 d U . . H16A H 0.4534 0.1416 0.4674 0.116 Uiso 1 1 calc R . . C17 C 0.4439(14) 0.0071(13) 0.4877(9) 0.070(5) Uani 1 1 d U . . C18 C 0.3678(16) -0.0690(16) 0.4848(10) 0.098(6) Uani 1 1 d U . . H18A H 0.3876 -0.1285 0.4994 0.118 Uiso 1 1 calc R . . C19 C 0.2625(16) -0.0575(16) 0.4603(10) 0.089(6) Uani 1 1 d U . . H19A H 0.2125 -0.1088 0.4581 0.107 Uiso 1 1 calc R . . C20 C 0.1227(17) 0.0318(16) 0.4159(11) 0.100(7) Uani 1 1 d U . . H20A H 0.0991 0.0985 0.4150 0.120 Uiso 1 1 calc R . . H20B H 0.0693 -0.0041 0.4376 0.120 Uiso 1 1 calc R . . C21 C 0.124(2) -0.007(2) 0.3593(11) 0.132(10) Uani 1 1 d U . . H21A H 0.0502 -0.0034 0.3436 0.198 Uiso 1 1 calc R . . H21B H 0.1478 -0.0735 0.3602 0.198 Uiso 1 1 calc R . . H21C H 0.1756 0.0292 0.3376 0.198 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 0.0515(4) 0.0467(4) 0.0351(3) 0.0041(3) -0.0005(3) 0.0087(3) Pb2 0.0621(4) 0.0752(5) 0.0481(4) 0.0203(4) -0.0050(3) 0.0102(4) Pb3 0.0517(4) 0.0496(4) 0.0567(4) 0.0039(3) -0.0031(3) 0.0090(3) I1 0.0766(9) 0.0743(11) 0.1176(13) -0.0260(10) -0.0063(8) -0.0045(8) I2 0.0872(10) 0.0821(12) 0.1537(17) 0.0396(11) -0.0430(11) 0.0103(9) I3 0.1075(12) 0.181(2) 0.0501(8) 0.0155(11) 0.0143(8) -0.0029(13) I4 0.0587(7) 0.0630(8) 0.0516(6) 0.0216(6) 0.0008(5) 0.0158(6) I5 0.0604(6) 0.0414(6) 0.0492(6) 0.0004(5) -0.0055(5) 0.0107(5) I6 0.0591(6) 0.0518(7) 0.0297(5) 0.0000(5) -0.0022(4) 0.0120(5) I7 0.0652(7) 0.0584(8) 0.0584(7) -0.0119(6) 0.0036(6) 0.0038(6) I8 0.0703(8) 0.0828(10) 0.0404(6) 0.0053(6) 0.0060(5) 0.0051(7) I9 0.0557(7) 0.0691(9) 0.1006(11) 0.0293(8) -0.0133(7) 0.0057(6) N1 0.069(9) 0.132(15) 0.090(12) 0.021(10) 0.008(8) -0.003(9) N2 0.059(7) 0.058(9) 0.089(9) -0.007(8) -0.003(7) 0.001(6) N3 0.058(8) 0.054(8) 0.128(13) -0.017(9) 0.016(8) -0.001(6) C1 0.114(14) 0.107(18) 0.132(18) -0.009(12) 0.072(13) -0.014(12) C2 0.102(13) 0.092(15) 0.116(16) -0.035(11) 0.058(11) -0.007(11) C3 0.055(7) 0.070(11) 0.045(8) -0.013(8) -0.002(6) 0.008(7) C4 0.076(10) 0.112(15) 0.039(9) -0.013(9) -0.001(8) -0.025(10) C5 0.075(10) 0.139(17) 0.044(10) 0.010(10) -0.020(7) -0.031(10) C6 0.079(10) 0.070(12) 0.062(10) -0.028(10) 0.027(8) -0.015(9) C7 0.077(9) 0.061(11) 0.038(7) -0.023(8) 0.008(7) -0.017(9) C8 0.056(7) 0.061(10) 0.042(7) -0.014(8) 0.000(6) 0.008(7) C9 0.115(12) 0.119(16) 0.042(8) -0.012(11) -0.002(8) -0.054(12) C10 0.104(12) 0.112(16) 0.059(9) 0.000(11) -0.022(8) -0.046(12) C11 0.070(12) 0.16(2) 0.15(2) 0.027(16) 0.015(12) -0.011(13) C12 0.097(18) 0.13(2) 0.15(3) 0.013(17) 0.026(17) -0.038(16) C13 0.063(9) 0.076(12) 0.142(18) -0.001(14) -0.003(10) -0.007(10) C14 0.096(16) 0.100(15) 0.115(19) 0.047(16) -0.011(14) -0.020(12) C15 0.082(11) 0.037(9) 0.18(2) -0.010(12) -0.025(12) -0.003(8) C16 0.085(11) 0.046(9) 0.157(19) -0.002(12) -0.028(12) -0.011(9) C17 0.057(9) 0.038(9) 0.115(15) -0.006(9) 0.016(9) -0.007(7) C18 0.072(11) 0.065(11) 0.157(19) 0.022(13) 0.004(11) -0.016(9) C19 0.065(9) 0.067(10) 0.136(18) 0.015(12) 0.017(10) -0.027(9) C20 0.076(11) 0.071(13) 0.153(18) -0.044(13) -0.011(12) -0.002(10) C21 0.096(17) 0.16(3) 0.14(2) -0.04(2) 0.001(14) -0.002(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I8 3.1406(15) . ? Pb1 I7 3.1783(15) . ? Pb1 I4 3.2009(13) . ? Pb1 I5 3.2625(13) 3_675 ? Pb1 I5 3.2991(14) . ? Pb1 I6 3.3076(15) . ? Pb2 I2 2.9988(17) . ? Pb2 I3 3.0031(18) . ? Pb2 I9 3.2781(17) . ? Pb2 I8 3.2816(17) . ? Pb3 I1 3.0096(17) . ? Pb3 I9 3.1097(15) 1_655 ? Pb3 I7 3.2561(16) 3_775 ? Pb3 I4 3.2980(16) . ? Pb3 I6 3.3879(13) . ? Pb3 I6 3.4295(15) 3_775 ? I5 Pb1 3.2625(13) 3_675 ? I6 Pb3 3.4295(15) 3_775 ? I7 Pb3 3.2561(16) 3_775 ? I9 Pb3 3.1097(15) 1_455 ? N1 C5 1.29(2) . ? N1 C1 1.35(3) . ? N1 C11 1.49(3) . ? N2 C10 1.29(2) . ? N2 C6 1.31(2) . ? N2 C13 1.48(2) . ? N3 C19 1.29(2) . ? N3 C15 1.31(2) . ? N3 C20 1.50(2) . ? C1 C2 1.35(3) . ? C1 H1A 0.9400 . ? C2 C3 1.35(2) . ? C2 H2A 0.9400 . ? C3 C4 1.38(2) . ? C3 C8 1.48(2) . ? C4 C5 1.36(2) . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C6 C7 1.39(2) . ? C6 H6A 0.9400 . ? C7 C8 1.39(2) . ? C7 H7A 0.9400 . ? C8 C9 1.37(2) . ? C9 C10 1.41(3) . ? C9 H9A 0.9400 . ? C10 H10A 0.9400 . ? C11 C12 1.47(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.45(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.37(3) . ? C15 H15A 0.9400 . ? C16 C17 1.33(3) . ? C16 H16A 0.9400 . ? C17 C18 1.41(2) . ? C17 C17 1.49(4) 3_656 ? C18 C19 1.41(3) . ? C18 H18A 0.9400 . ? C19 H19A 0.9400 . ? C20 C21 1.51(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 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 I8 Pb1 I7 93.52(4) . . ? I8 Pb1 I4 89.81(4) . . ? I7 Pb1 I4 94.07(4) . . ? I8 Pb1 I5 92.40(4) . 3_675 ? I7 Pb1 I5 86.16(4) . 3_675 ? I4 Pb1 I5 177.75(3) . 3_675 ? I8 Pb1 I5 90.57(4) . . ? I7 Pb1 I5 168.81(4) . . ? I4 Pb1 I5 96.36(4) . . ? I5 Pb1 I5 83.26(4) 3_675 . ? I8 Pb1 I6 174.63(4) . . ? I7 Pb1 I6 86.50(3) . . ? I4 Pb1 I6 84.83(3) . . ? I5 Pb1 I6 92.95(3) 3_675 . ? I5 Pb1 I6 90.39(3) . . ? I2 Pb2 I3 95.17(6) . . ? I2 Pb2 I9 85.45(5) . . ? I3 Pb2 I9 93.86(5) . . ? I2 Pb2 I8 95.00(5) . . ? I3 Pb2 I8 86.37(5) . . ? I9 Pb2 I8 179.48(4) . . ? I1 Pb3 I9 94.48(5) . 1_655 ? I1 Pb3 I7 88.69(4) . 3_775 ? I9 Pb3 I7 92.79(4) 1_655 3_775 ? I1 Pb3 I4 97.54(4) . . ? I9 Pb3 I4 85.88(4) 1_655 . ? I7 Pb3 I4 173.71(4) 3_775 . ? I1 Pb3 I6 93.81(5) . . ? I9 Pb3 I6 166.18(4) 1_655 . ? I7 Pb3 I6 98.43(4) 3_775 . ? I4 Pb3 I6 82.09(3) . . ? I1 Pb3 I6 171.94(4) . 3_775 ? I9 Pb3 I6 85.01(4) 1_655 3_775 ? I7 Pb3 I6 83.30(3) 3_775 3_775 ? I4 Pb3 I6 90.45(3) . 3_775 ? I6 Pb3 I6 88.31(4) . 3_775 ? Pb1 I4 Pb3 98.43(3) . . ? Pb1 I5 Pb1 96.74(4) 3_675 . ? Pb1 I6 Pb3 94.61(3) . . ? Pb1 I6 Pb3 92.07(3) . 3_775 ? Pb3 I6 Pb3 91.69(4) . 3_775 ? Pb1 I7 Pb3 97.82(4) . 3_775 ? Pb1 I8 Pb2 96.81(4) . . ? Pb3 I9 Pb2 101.95(5) 1_455 . ? C5 N1 C1 118(2) . . ? C5 N1 C11 122(2) . . ? C1 N1 C11 119(2) . . ? C10 N2 C6 122.3(18) . . ? C10 N2 C13 118.1(19) . . ? C6 N2 C13 119.6(18) . . ? C19 N3 C15 123(2) . . ? C19 N3 C20 115.7(18) . . ? C15 N3 C20 121(2) . . ? N1 C1 C2 121(2) . . ? N1 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 C2 C1 121(2) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 116.9(19) . . ? C2 C3 C8 123.3(18) . . ? C4 C3 C8 119.7(15) . . ? C5 C4 C3 119.6(19) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? N1 C5 C4 123(2) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? N2 C6 C7 119.7(16) . . ? N2 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C6 C7 C8 121.9(16) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 114.7(17) . . ? C9 C8 C3 123.8(16) . . ? C7 C8 C3 121.4(15) . . ? C8 C9 C10 121.6(18) . . ? C8 C9 H9A 119.2 . . ? C10 C9 H9A 119.2 . . ? N2 C10 C9 119.7(19) . . ? N2 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C12 C11 N1 114(2) . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? N1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N2 111.3(18) . . ? C14 C13 H13A 109.4 . . ? N2 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? N2 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 119(2) . . ? N3 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C17 C16 C15 124(2) . . ? C17 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? C16 C17 C18 114.2(19) . . ? C16 C17 C17 125(2) . 3_656 ? C18 C17 C17 120(2) . 3_656 ? C17 C18 C19 121(2) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? N3 C19 C18 119(2) . . ? N3 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? N3 C20 C21 110.3(19) . . ? N3 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? N3 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.444 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.246 #===END #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 765930' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I9 Pb3, C16 H22 N2, C8 H11 N' _chemical_formula_sum 'C24 H33 I9 N3 Pb3' _chemical_formula_weight 2127.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.328(3) _cell_length_b 14.341(3) _cell_length_c 24.982(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(3) _cell_angle_gamma 90.00 _cell_volume 4416.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13791 _cell_measurement_theta_min 3.2619 _cell_measurement_theta_max 27.4894 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3684 _exptl_absorpt_coefficient_mu 17.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2460 _exptl_absorpt_correction_T_max 0.2460 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20775 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10019 _reflns_number_gt 7579 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0347P)^2^+20.0000P] 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 10019 _refine_ls_number_parameters 380 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.005 _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 Pb2 Pb 0.16425(5) 0.84044(4) 0.11146(2) 0.04167(16) Uani 1 1 d . . . Pb1 Pb -0.16750(5) 0.99361(4) 0.05315(2) 0.03568(14) Uani 1 1 d . . . Pb3 Pb -0.50378(5) 0.83357(4) 0.00129(2) 0.03729(15) Uani 1 1 d . . . I4 I -0.33342(8) 0.84483(7) 0.10204(4) 0.0469(3) Uani 1 1 d . . . I8 I -0.03127(9) 0.97381(7) 0.15848(4) 0.0462(3) Uani 1 1 d . . . I7 I -0.30409(9) 1.17139(7) 0.09043(4) 0.0460(3) Uani 1 1 d . . . I5 I 0.00206(8) 1.15202(6) 0.00654(4) 0.0398(2) Uani 1 1 d . . . I6 I -0.33398(8) 0.99348(6) -0.05123(4) 0.0368(2) Uani 1 1 d . . . I9 I 0.36425(9) 0.70027(7) 0.07516(4) 0.0480(3) Uani 1 1 d . . . I2 I 0.05091(10) 0.66573(7) 0.14507(5) 0.0567(3) Uani 1 1 d . . . I1 I -0.38701(10) 0.68611(8) -0.06197(5) 0.0569(3) Uani 1 1 d . . . I3 I 0.27312(10) 0.88070(8) 0.21615(5) 0.0580(3) Uani 1 1 d . . . N1 N 0.6067(10) 1.1095(9) 0.2389(6) 0.053(4) Uani 1 1 d . B . N2 N 0.0637(10) 1.2314(8) 0.1988(5) 0.044(3) Uani 1 1 d . . . N3 N -0.2696(11) 0.5119(10) 0.0423(5) 0.051(4) Uani 1 1 d . . . C1 C 0.5609(13) 1.1727(10) 0.2705(7) 0.050(4) Uani 1 1 d . . . H1A H 0.6023 1.1991 0.2983 0.060 Uiso 1 1 calc R . . C2 C 0.4558(14) 1.2008(13) 0.2639(7) 0.064(5) Uani 1 1 d . . . H2A H 0.4261 1.2455 0.2871 0.077 Uiso 1 1 calc R . . C3 C 0.3933(13) 1.1639(11) 0.2235(6) 0.045(4) Uani 1 1 d . . . C4 C 0.4435(13) 1.0948(11) 0.1910(6) 0.048(4) Uani 1 1 d . . . H4A H 0.4037 1.0665 0.1632 0.058 Uiso 1 1 calc R . . C5 C 0.5494(13) 1.0690(12) 0.1998(6) 0.050(4) Uani 1 1 d . . . H5A H 0.5815 1.0230 0.1783 0.060 Uiso 1 1 calc R . . C6 C 0.1117(13) 1.2525(11) 0.2453(7) 0.053(4) Uani 1 1 d . . . H6A H 0.0724 1.2832 0.2723 0.063 Uiso 1 1 calc R . . C7 C 0.2177(14) 1.2296(12) 0.2536(7) 0.059(5) Uani 1 1 d . . . H7A H 0.2505 1.2432 0.2867 0.071 Uiso 1 1 calc R . . C8 C 0.2775(12) 1.1869(10) 0.2142(6) 0.042(4) Uani 1 1 d . . . C9 C 0.2271(12) 1.1679(10) 0.1654(6) 0.047(4) Uani 1 1 d . . . H9A H 0.2651 1.1387 0.1375 0.057 Uiso 1 1 calc R . . C10 C 0.1213(13) 1.1928(10) 0.1593(6) 0.045(4) Uani 1 1 d . . . H10A H 0.0874 1.1827 0.1260 0.054 Uiso 1 1 calc R . . C11 C -0.2283(14) 0.4294(12) 0.0298(7) 0.058(5) Uani 1 1 d . . . H11A H -0.2704 0.3752 0.0338 0.069 Uiso 1 1 calc R . . C12 C -0.1240(13) 0.4231(11) 0.0111(7) 0.055(5) Uani 1 1 d . . . H12A H -0.0962 0.3648 0.0008 0.066 Uiso 1 1 calc R . . C13 C -0.0571(11) 0.5040(10) 0.0071(7) 0.042(4) Uani 1 1 d . . . C14 C -0.1062(12) 0.5875(10) 0.0228(7) 0.049(4) Uani 1 1 d . . . H14A H -0.0655 0.6430 0.0226 0.059 Uiso 1 1 calc R . . C15 C -0.2131(13) 0.5897(11) 0.0385(7) 0.057(5) Uani 1 1 d . . . H15A H -0.2460 0.6471 0.0466 0.069 Uiso 1 1 calc R . . C16 C 0.7225(14) 1.0809(13) 0.2469(8) 0.069(5) Uani 1 1 d DU . . H16A H 0.7678 1.1341 0.2572 0.082 Uiso 1 1 calc R A 1 H16B H 0.7521 1.0522 0.2145 0.082 Uiso 1 1 calc R A 1 C17 C 0.713(4) 1.011(3) 0.2916(15) 0.067(9) Uani 0.45(3) 1 d PDU B 1 H17A H 0.7694 0.9712 0.2763 0.080 Uiso 0.45(3) 1 calc PR B 1 H17B H 0.7543 1.0512 0.3164 0.080 Uiso 0.45(3) 1 calc PR B 1 C18 C 0.697(4) 0.970(4) 0.318(2) 0.076(13) Uani 0.45(3) 1 d PU B 1 H18A H 0.7515 0.9734 0.3458 0.114 Uiso 0.45(3) 1 calc PR B 1 H18B H 0.6972 0.9073 0.3025 0.114 Uiso 0.45(3) 1 calc PR B 1 H18C H 0.6264 0.9834 0.3322 0.114 Uiso 0.45(3) 1 calc PR B 1 C17' C 0.735(2) 0.978(2) 0.2598(15) 0.069(8) Uani 0.55(3) 1 d PDU B 2 H17C H 0.7532 0.9458 0.2263 0.082 Uiso 0.55(3) 1 calc PR B 2 H17D H 0.7987 0.9717 0.2834 0.082 Uiso 0.55(3) 1 calc PR B 2 C18' C 0.644(3) 0.925(3) 0.2854(19) 0.096(13) Uani 0.55(3) 1 d PDU B 2 H18D H 0.6668 0.8609 0.2923 0.143 Uiso 0.55(3) 1 calc PR B 2 H18E H 0.5817 0.9242 0.2615 0.143 Uiso 0.55(3) 1 calc PR B 2 H18F H 0.6244 0.9542 0.3189 0.143 Uiso 0.55(3) 1 calc PR B 2 C19 C -0.0495(14) 1.2586(13) 0.1897(8) 0.072(5) Uani 1 1 d U B . H19A H -0.0873 1.2607 0.2241 0.086 Uiso 1 1 calc R . . H19B H -0.0850 1.2112 0.1674 0.086 Uiso 1 1 calc R . . C20 C -0.060(2) 1.3504(18) 0.1632(12) 0.116(9) Uani 1 1 d U . . H20A H -0.0474 1.3362 0.1253 0.139 Uiso 1 1 calc R B 1 H20B H -0.1371 1.3647 0.1659 0.139 Uiso 1 1 calc R B 1 C21 C -0.021(5) 1.417(4) 0.169(3) 0.117(18) Uani 0.45(3) 1 d PU B 1 H21A H -0.0490 1.4606 0.1422 0.176 Uiso 0.45(3) 1 calc PR B 1 H21B H 0.0566 1.4102 0.1641 0.176 Uiso 0.45(3) 1 calc PR B 1 H21C H -0.0361 1.4401 0.2042 0.176 Uiso 0.45(3) 1 calc PR B 1 C21' C 0.025(3) 1.392(3) 0.126(2) 0.091(13) Uani 0.55(3) 1 d PU B 2 H21D H -0.0011 1.4517 0.1131 0.137 Uiso 0.55(3) 1 calc PR B 2 H21E H 0.0370 1.3502 0.0966 0.137 Uiso 0.55(3) 1 calc PR B 2 H21F H 0.0918 1.4011 0.1461 0.137 Uiso 0.55(3) 1 calc PR B 2 C22 C -0.3843(15) 0.5165(14) 0.0640(9) 0.081(6) Uani 1 1 d U . . H22A H -0.4313 0.4735 0.0442 0.097 Uiso 1 1 calc R . . H22B H -0.4132 0.5798 0.0598 0.097 Uiso 1 1 calc R . . C23 C -0.382(2) 0.490(2) 0.1238(11) 0.123(9) Uani 1 1 d U . . H23A H -0.4561 0.4933 0.1380 0.148 Uiso 1 1 calc R . . H23B H -0.3575 0.4250 0.1273 0.148 Uiso 1 1 calc R . . C24 C -0.312(2) 0.5493(19) 0.1549(11) 0.142(10) Uani 1 1 d U . . H24A H -0.3127 0.5292 0.1920 0.213 Uiso 1 1 calc R . . H24B H -0.3381 0.6131 0.1526 0.213 Uiso 1 1 calc R . . H24C H -0.2390 0.5458 0.1411 0.213 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 Pb2 0.0470(3) 0.0426(3) 0.0354(3) 0.0050(3) 0.0015(3) -0.0025(3) Pb1 0.0396(3) 0.0358(3) 0.0316(3) 0.0004(2) -0.0003(2) 0.0011(3) Pb3 0.0423(3) 0.0347(3) 0.0349(3) -0.0005(2) 0.0044(2) 0.0003(3) I4 0.0519(6) 0.0515(6) 0.0371(6) 0.0103(5) -0.0054(5) -0.0120(5) I8 0.0499(6) 0.0516(6) 0.0369(6) -0.0008(5) -0.0053(5) 0.0094(5) I7 0.0523(6) 0.0469(6) 0.0388(6) -0.0068(5) -0.0061(5) 0.0094(5) I5 0.0503(6) 0.0310(5) 0.0382(5) -0.0022(4) 0.0052(4) -0.0015(4) I6 0.0511(6) 0.0340(5) 0.0254(5) -0.0022(4) 0.0019(4) -0.0019(4) I9 0.0523(6) 0.0453(6) 0.0467(6) 0.0055(5) 0.0136(5) -0.0018(5) I2 0.0676(8) 0.0467(6) 0.0559(7) 0.0025(5) 0.0078(6) -0.0115(6) I1 0.0699(8) 0.0480(6) 0.0529(7) -0.0069(5) 0.0148(6) 0.0082(6) I3 0.0696(8) 0.0602(7) 0.0442(7) -0.0009(6) -0.0082(6) -0.0034(6) N1 0.046(8) 0.052(9) 0.061(10) 0.007(7) -0.007(7) -0.003(7) N2 0.042(7) 0.040(7) 0.050(9) 0.001(6) -0.001(6) 0.012(6) N3 0.042(8) 0.067(10) 0.042(8) 0.008(7) -0.001(6) -0.008(7) C1 0.058(11) 0.039(9) 0.054(11) -0.015(8) -0.009(9) -0.013(8) C2 0.059(11) 0.079(13) 0.053(12) -0.020(10) -0.015(9) 0.008(10) C3 0.052(10) 0.051(10) 0.033(8) -0.001(7) 0.000(7) 0.004(8) C4 0.050(10) 0.064(11) 0.030(8) -0.019(8) -0.001(7) -0.008(9) C5 0.050(10) 0.064(11) 0.036(9) -0.006(8) -0.003(8) -0.008(9) C6 0.057(11) 0.060(11) 0.041(10) -0.009(8) 0.015(8) 0.000(9) C7 0.058(11) 0.081(13) 0.038(10) -0.009(9) 0.004(8) 0.003(10) C8 0.045(9) 0.042(9) 0.039(9) -0.015(7) -0.005(7) -0.008(8) C9 0.051(10) 0.054(10) 0.037(9) -0.027(8) 0.014(7) -0.005(8) C10 0.067(11) 0.039(8) 0.031(8) 0.004(7) 0.005(7) 0.012(8) C11 0.055(11) 0.049(10) 0.070(13) 0.000(9) 0.004(10) -0.009(9) C12 0.058(11) 0.049(10) 0.059(12) -0.018(9) 0.011(9) -0.010(9) C13 0.034(8) 0.039(8) 0.052(10) -0.016(7) -0.003(7) -0.014(7) C14 0.045(9) 0.036(9) 0.067(12) -0.001(8) 0.000(8) -0.013(8) C15 0.051(10) 0.040(9) 0.081(14) 0.009(9) 0.013(10) 0.008(8) C16 0.052(10) 0.074(11) 0.079(14) 0.013(10) -0.001(10) -0.001(9) C17 0.058(19) 0.07(2) 0.07(2) 0.005(14) 0.016(18) 0.026(18) C18 0.07(3) 0.10(3) 0.06(3) 0.011(18) 0.02(2) 0.01(3) C17' 0.072(17) 0.088(15) 0.046(17) 0.022(15) 0.027(14) 0.041(14) C18' 0.12(3) 0.08(2) 0.09(3) 0.06(2) 0.03(2) 0.030(19) C19 0.053(10) 0.079(12) 0.083(15) 0.013(11) -0.003(10) 0.019(10) C20 0.091(16) 0.104(16) 0.15(2) 0.051(16) 0.032(15) 0.064(14) C21 0.10(4) 0.10(2) 0.14(4) 0.07(3) 0.02(3) 0.04(3) C21' 0.07(2) 0.06(2) 0.14(3) 0.01(2) -0.041(19) -0.044(19) C22 0.048(11) 0.079(14) 0.116(16) 0.021(13) 0.020(11) 0.004(10) C23 0.106(18) 0.15(2) 0.111(17) 0.007(16) 0.038(16) -0.041(15) C24 0.19(3) 0.13(2) 0.109(19) -0.014(19) 0.017(19) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb2 I2 2.9907(13) . ? Pb2 I3 2.9909(15) . ? Pb2 I8 3.2971(13) . ? Pb2 I9 3.3108(13) . ? Pb1 I8 3.1285(14) . ? Pb1 I7 3.1963(12) . ? Pb1 I4 3.2014(13) . ? Pb1 I5 3.2819(13) 3_575 ? Pb1 I5 3.3024(12) . ? Pb1 I6 3.3117(15) . ? Pb3 I1 3.0102(13) . ? Pb3 I9 3.1196(13) 1_455 ? Pb3 I4 3.2752(15) . ? Pb3 I7 3.2893(15) 3_475 ? Pb3 I6 3.3742(12) . ? Pb3 I6 3.4249(12) 3_475 ? I7 Pb3 3.2894(15) 3_475 ? I5 Pb1 3.2819(13) 3_575 ? I6 Pb3 3.4249(12) 3_475 ? I9 Pb3 3.1196(13) 1_655 ? N1 C1 1.329(19) . ? N1 C5 1.337(18) . ? N1 C16 1.497(19) . ? N2 C6 1.336(19) . ? N2 C10 1.339(18) . ? N2 C19 1.466(19) . ? N3 C15 1.319(19) . ? N3 C11 1.33(2) . ? N3 C22 1.52(2) . ? C1 C2 1.37(2) . ? C1 H1A 0.9400 . ? C2 C3 1.37(2) . ? C2 H2A 0.9400 . ? C3 C4 1.423(19) . ? C3 C8 1.48(2) . ? C4 C5 1.37(2) . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C6 C7 1.36(2) . ? C6 H6A 0.9400 . ? C7 C8 1.38(2) . ? C7 H7A 0.9400 . ? C8 C9 1.393(19) . ? C9 C10 1.36(2) . ? C9 H9A 0.9400 . ? C10 H10A 0.9400 . ? C11 C12 1.37(2) . ? C11 H11A 0.9400 . ? C12 C13 1.43(2) . ? C12 H12A 0.9400 . ? C13 C14 1.398(19) . ? C13 C13 1.46(3) 3_565 ? C14 C15 1.38(2) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 C17 1.502(10) . ? C16 C17' 1.52(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 0.91(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C17' C18' 1.506(10) . ? C17' H17C 0.9800 . ? C17' H17D 0.9800 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 C20 1.48(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.07(6) . ? C20 C21' 1.51(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 C23 1.54(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.44(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 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 I2 Pb2 I3 97.16(4) . . ? I2 Pb2 I8 92.46(4) . . ? I3 Pb2 I8 84.41(4) . . ? I2 Pb2 I9 85.28(4) . . ? I3 Pb2 I9 91.42(4) . . ? I8 Pb2 I9 174.98(3) . . ? I8 Pb1 I7 96.25(3) . . ? I8 Pb1 I4 87.72(3) . . ? I7 Pb1 I4 94.72(4) . . ? I8 Pb1 I5 89.54(3) . 3_575 ? I7 Pb1 I5 165.73(3) . 3_575 ? I4 Pb1 I5 98.54(4) . 3_575 ? I8 Pb1 I5 91.18(3) . . ? I7 Pb1 I5 83.63(3) . . ? I4 Pb1 I5 177.91(3) . . ? I5 Pb1 I5 83.23(3) 3_575 . ? I8 Pb1 I6 172.28(3) . . ? I7 Pb1 I6 84.51(3) . . ? I4 Pb1 I6 84.56(3) . . ? I5 Pb1 I6 91.50(3) 3_575 . ? I5 Pb1 I6 96.54(3) . . ? I1 Pb3 I9 97.58(4) . 1_455 ? I1 Pb3 I4 97.56(4) . . ? I9 Pb3 I4 84.84(3) 1_455 . ? I1 Pb3 I7 87.91(4) . 3_475 ? I9 Pb3 I7 91.32(3) 1_455 3_475 ? I4 Pb3 I7 173.67(3) . 3_475 ? I1 Pb3 I6 88.54(4) . . ? I9 Pb3 I6 166.52(3) 1_455 . ? I4 Pb3 I6 82.44(3) . . ? I7 Pb3 I6 100.95(3) 3_475 . ? I1 Pb3 I6 168.91(4) . 3_475 ? I9 Pb3 I6 85.49(3) 1_455 3_475 ? I4 Pb3 I6 93.32(3) . 3_475 ? I7 Pb3 I6 81.35(3) 3_475 3_475 ? I6 Pb3 I6 90.79(3) . 3_475 ? Pb1 I4 Pb3 98.53(3) . . ? Pb1 I8 Pb2 98.26(4) . . ? Pb1 I7 Pb3 99.12(3) . 3_475 ? Pb1 I5 Pb1 96.77(3) 3_575 . ? Pb1 I6 Pb3 94.45(3) . . ? Pb1 I6 Pb3 94.23(3) . 3_475 ? Pb3 I6 Pb3 89.21(3) . 3_475 ? Pb3 I9 Pb2 100.42(4) 1_655 . ? C1 N1 C5 120.4(14) . . ? C1 N1 C16 121.0(15) . . ? C5 N1 C16 118.6(15) . . ? C6 N2 C10 120.1(14) . . ? C6 N2 C19 119.5(15) . . ? C10 N2 C19 120.1(15) . . ? C15 N3 C11 122.2(15) . . ? C15 N3 C22 118.8(15) . . ? C11 N3 C22 118.9(15) . . ? N1 C1 C2 122.3(15) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 120.3(17) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C2 C3 C4 116.3(15) . . ? C2 C3 C8 124.4(15) . . ? C4 C3 C8 119.1(14) . . ? C5 C4 C3 120.7(14) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? N1 C5 C4 119.9(16) . . ? N1 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? N2 C6 C7 119.9(15) . . ? N2 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C6 C7 C8 121.0(16) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C7 C8 C9 118.3(15) . . ? C7 C8 C3 120.4(14) . . ? C9 C8 C3 121.3(14) . . ? C10 C9 C8 118.1(14) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 122.4(15) . . ? N2 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? N3 C11 C12 120.0(16) . . ? N3 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 120.8(15) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C14 C13 C12 115.2(14) . . ? C14 C13 C13 123.7(16) . 3_565 ? C12 C13 C13 120.7(17) . 3_565 ? C15 C14 C13 121.0(14) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? N3 C15 C14 120.5(15) . . ? N3 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? N1 C16 C17 102(2) . . ? N1 C16 C17' 113.1(17) . . ? N1 C16 H16A 111.4 . . ? C17 C16 H16A 111.4 . . ? C17' C16 H16A 129.9 . . ? N1 C16 H16B 111.4 . . ? C17 C16 H16B 111.4 . . ? C17' C16 H16B 74.2 . . ? H16A C16 H16B 109.3 . . ? C18 C17 C16 172(7) . . ? C18 C17 H17A 94.00 . . ? C16 C17 H17A 92.5 . . ? C18 C17 H17B 92.5 . . ? C16 C17 H17B 92.6 . . ? H17A C17 H17B 103.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 108.00 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 111.00 . . ? H18B C18 H18C 109.5 . . ? C18' C17' C16 120(2) . . ? C18' C17' H17C 107.2 . . ? C16 C17' H17C 107.2 . . ? C18' C17' H17D 107.2 . . ? C16 C17' H17D 107.2 . . ? H17C C17' H17D 106.9 . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? N2 C19 C20 112.7(17) . . ? N2 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N2 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C21' 55(4) . . ? C21 C20 C19 134(5) . . ? C21' C20 C19 125(2) . . ? C21 C20 H20A 103.6 . . ? C21' C20 H20A 52.2 . . ? C19 C20 H20A 103.6 . . ? C21 C20 H20B 103.6 . . ? C21' C20 H20B 129.2 . . ? C19 C20 H20B 103.6 . . ? H20A C20 H20B 105.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C21' H21D 109.5 . . ? C20 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C20 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? N3 C22 C23 108.9(17) . . ? N3 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? N3 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 C22 112(2) . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 1.256 _refine_diff_density_min -2.152 _refine_diff_density_rms 0.294 #===END #============================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 765931' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I12 Pb4, C16 H22 N2, 2(C8 H11 N)' _chemical_formula_sum 'C32 H44 I12 N4 Pb4' _chemical_formula_weight 2836.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.182(3) _cell_length_b 21.323(4) _cell_length_c 17.966(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.44(3) _cell_angle_gamma 90.00 _cell_volume 6029(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18847 _cell_measurement_theta_min 3.0145 _cell_measurement_theta_max 27.6491 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4912 _exptl_absorpt_coefficient_mu 17.305 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.121 _exptl_absorpt_correction_T_max 0.135 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19681 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.1353 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10380 _reflns_number_gt 4568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0691P)^2^+28.1904P] 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 10380 _refine_ls_number_parameters 304 _refine_ls_number_restraints 488 _refine_ls_R_factor_all 0.1803 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.2363 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.28624(16) 0.61196(13) 0.26007(15) 0.0479(6) Uani 0.826(5) 1 d PU . 1 Pb1' Pb -0.2542(10) 0.6318(5) 0.2512(6) 0.051(3) Uani 0.174(5) 1 d PU . 2 Pb2 Pb -0.03575(14) 0.63257(7) 0.26161(10) 0.0418(5) Uani 0.826(5) 1 d PU . 1 Pb2' Pb -0.0007(6) 0.6409(4) 0.2494(4) 0.033(2) Uiso 0.174(5) 1 d PU . 2 Pb3 Pb 0.21579(14) 0.63044(7) 0.26364(10) 0.0456(5) Uani 0.826(5) 1 d PU . 1 Pb3' Pb 0.2493(7) 0.6311(4) 0.2478(5) 0.036(2) Uiso 0.174(5) 1 d PU . 2 Pb4 Pb 0.46309(15) 0.61074(11) 0.25821(14) 0.0420(5) Uani 0.826(5) 1 d PU . 1 Pb4' Pb 0.4975(8) 0.6219(4) 0.2502(7) 0.044(3) Uani 0.174(5) 1 d PU . 2 I1 I -0.1517(2) 0.70554(14) 0.36457(18) 0.0644(10) Uani 0.826(5) 1 d PU . 1 I1' I -0.0951(12) 0.7220(6) 0.3507(8) 0.060(4) Uani 0.174(5) 1 d PU . 2 I2 I -0.1999(2) 0.64707(17) 0.11928(18) 0.0480(8) Uani 0.826(5) 1 d PU . 1 I2' I -0.1637(14) 0.6640(8) 0.1074(9) 0.057(3) Uani 0.174(5) 1 d PU . 2 I3 I -0.13658(14) 0.51193(9) 0.30355(13) 0.0520(6) Uani 1 1 d U . . I4 I 0.1286(3) 0.67574(17) 0.3983(2) 0.0553(9) Uani 0.826(5) 1 d PU . 1 I4' I 0.1694(12) 0.6665(7) 0.3901(9) 0.048(3) Uani 0.174(5) 1 d PU . 2 I5 I 0.06781(19) 0.71467(10) 0.15155(14) 0.0729(8) Uani 1 1 d U . . I6 I 0.08227(15) 0.52012(10) 0.22229(14) 0.0612(7) Uani 1 1 d U . . I7 I 0.35385(18) 0.53819(10) 0.36777(13) 0.0682(7) Uani 1 1 d U . . I8 I 0.2954(2) 0.5977(2) 0.1182(2) 0.0474(9) Uani 0.826(5) 1 d PU . 1 I8' I 0.3296(13) 0.5944(8) 0.1073(10) 0.049(3) Uani 0.174(5) 1 d PU . 2 I9 I 0.3668(3) 0.73206(18) 0.3052(3) 0.0518(9) Uani 0.826(5) 1 d PU . 1 I9' I 0.3920(13) 0.7394(7) 0.2844(13) 0.045(3) Uani 0.174(5) 1 d PU . 2 I10 I 0.58230(17) 0.72567(11) 0.21309(13) 0.0670(7) Uani 1 1 d U . . I11 I 0.6249(2) 0.57187(17) 0.39619(17) 0.0483(8) Uani 0.826(5) 1 d PU . 1 I11' I 0.6579(12) 0.5988(6) 0.3897(9) 0.046(3) Uani 0.174(5) 1 d PU . 2 I12 I 0.56178(18) 0.52794(10) 0.15072(14) 0.0681(7) Uani 1 1 d U . . N1 N 0.3735(11) 0.6616(8) 0.5733(10) 0.0553(19) Uani 1 1 d GDU . . C1 C 0.4406(12) 0.6361(6) 0.5471(11) 0.0553(19) Uani 1 1 d GU . . H1A H 0.4506 0.5927 0.5504 0.066 Uiso 1 1 calc R . . C2 C 0.4928(11) 0.6749(9) 0.5159(12) 0.0553(19) Uani 1 1 d GU . . H2A H 0.5381 0.6577 0.4982 0.066 Uiso 1 1 calc R . . C3 C 0.4780(12) 0.7392(8) 0.5110(12) 0.0553(19) Uani 1 1 d GU . . C4 C 0.4110(13) 0.7646(6) 0.5373(12) 0.0553(19) Uani 1 1 d GU . . H4A H 0.4010 0.8081 0.5340 0.066 Uiso 1 1 calc R . . C5 C 0.3587(11) 0.7258(8) 0.5684(11) 0.0553(19) Uani 1 1 d GU . . H5A H 0.3134 0.7431 0.5862 0.066 Uiso 1 1 calc R . . N2 N 0.6387(11) 0.8652(8) 0.4194(10) 0.0553(19) Uani 1 1 d GU . . C6 C 0.5850(12) 0.8891(6) 0.4627(11) 0.0553(19) Uani 1 1 d GU . . H6A H 0.5835 0.9325 0.4716 0.066 Uiso 1 1 calc R . . C7 C 0.5336(12) 0.8489(9) 0.4928(11) 0.0553(19) Uani 1 1 d GU . . H7A H 0.4973 0.8650 0.5220 0.066 Uiso 1 1 calc R . . C8 C 0.5358(12) 0.7847(8) 0.4796(12) 0.0553(19) Uani 1 1 d GU . . C9 C 0.5894(13) 0.7608(6) 0.4363(12) 0.0553(19) Uani 1 1 d GU . . H9A H 0.5909 0.7174 0.4274 0.066 Uiso 1 1 calc R . . C10 C 0.6409(12) 0.8011(8) 0.4062(11) 0.0553(19) Uani 1 1 d GU . . H10A H 0.6772 0.7849 0.3770 0.066 Uiso 1 1 calc R . . C11 C 0.3302(15) 0.6120(12) 0.6101(15) 0.0553(19) Uani 1 1 d DU . . H11A H 0.3205 0.5731 0.5791 0.066 Uiso 1 1 calc R . . C12 C 0.3837(19) 0.6000(14) 0.6892(15) 0.0553(19) Uani 1 1 d DU . . H12A H 0.4367 0.5803 0.6856 0.083 Uiso 1 1 calc R . . H12B H 0.3532 0.5725 0.7166 0.083 Uiso 1 1 calc R . . H12C H 0.3957 0.6395 0.7165 0.083 Uiso 1 1 calc R . . C13 C 0.2470(17) 0.6422(14) 0.6168(18) 0.0553(19) Uani 1 1 d DU . . H13A H 0.2146 0.6126 0.6396 0.083 Uiso 1 1 calc R . . H13B H 0.2145 0.6540 0.5663 0.083 Uiso 1 1 calc R . . H13C H 0.2590 0.6793 0.6488 0.083 Uiso 1 1 calc R . . C14 C 0.685(2) 0.9122(15) 0.3826(18) 0.0553(19) Uani 1 1 d U . . H14A H 0.6822 0.9551 0.4028 0.066 Uiso 1 1 calc R . . C15 C 0.654(2) 0.9090(14) 0.2965(16) 0.0553(19) Uani 1 1 d U . . H15A H 0.5946 0.9218 0.2823 0.083 Uiso 1 1 calc R . . H15B H 0.6590 0.8664 0.2793 0.083 Uiso 1 1 calc R . . H15C H 0.6874 0.9369 0.2727 0.083 Uiso 1 1 calc R . . C16 C 0.778(2) 0.8890(14) 0.3917(18) 0.0553(19) Uani 1 1 d U . . H16A H 0.8079 0.8910 0.4451 0.083 Uiso 1 1 calc R . . H16B H 0.8070 0.9154 0.3616 0.083 Uiso 1 1 calc R . . H16C H 0.7778 0.8460 0.3739 0.083 Uiso 1 1 calc R . . N3 N 0.1385(12) 0.5975(8) -0.0740(11) 0.062(3) Uani 1 1 d GU . . C17 C 0.1415(12) 0.5329(8) -0.0841(11) 0.062(3) Uani 1 1 d GU . . H17A H 0.1798 0.5157 -0.1106 0.075 Uiso 1 1 calc R . . C18 C 0.0877(14) 0.4939(6) -0.0551(12) 0.062(3) Uani 1 1 d GU . . H18A H 0.0897 0.4503 -0.0620 0.075 Uiso 1 1 calc R . . C19 C 0.0310(13) 0.5194(8) -0.0160(12) 0.062(3) Uani 1 1 d GU . . C20 C 0.0280(12) 0.5839(8) -0.0059(12) 0.062(3) Uani 1 1 d GU . . H20A H -0.0103 0.6011 0.0206 0.075 Uiso 1 1 calc R . . C21 C 0.0818(13) 0.6229(6) -0.0348(12) 0.062(3) Uani 1 1 d GU . . H21A H 0.0798 0.6666 -0.0280 0.075 Uiso 1 1 calc R . . C22 C 0.198(2) 0.6364(14) -0.110(2) 0.062(3) Uani 1 1 d U . . H22A H 0.2130 0.6738 -0.0775 0.075 Uiso 1 1 calc R . . C23 C 0.280(2) 0.6064(13) -0.1164(19) 0.062(3) Uani 1 1 d U . . H23A H 0.3122 0.6355 -0.1405 0.093 Uiso 1 1 calc R . . H23B H 0.2687 0.5685 -0.1469 0.093 Uiso 1 1 calc R . . H23C H 0.3134 0.5960 -0.0656 0.093 Uiso 1 1 calc R . . C24 C 0.136(2) 0.6606(14) -0.1881(18) 0.062(3) Uani 1 1 d U . . H24A H 0.1683 0.6844 -0.2173 0.093 Uiso 1 1 calc R . . H24B H 0.0920 0.6871 -0.1759 0.093 Uiso 1 1 calc R . . H24C H 0.1095 0.6249 -0.2179 0.093 Uiso 1 1 calc R . . N4 N -0.1193(14) 0.6125(9) 0.5776(12) 0.079(4) Uani 1 1 d GDU . . C25 C -0.0475(15) 0.6311(7) 0.5533(13) 0.079(4) Uani 1 1 d GU . . H25A H -0.0302 0.6733 0.5577 0.094 Uiso 1 1 calc R . . C26 C -0.0014(13) 0.5872(10) 0.5224(14) 0.079(4) Uani 1 1 d GU . . H26A H 0.0472 0.5998 0.5060 0.094 Uiso 1 1 calc R . . C27 C -0.0270(15) 0.5249(9) 0.5159(14) 0.079(4) Uani 1 1 d GU . . C28 C -0.0987(15) 0.5063(7) 0.5402(14) 0.079(4) Uani 1 1 d GU . . H28A H -0.1160 0.4641 0.5358 0.094 Uiso 1 1 calc R . . C29 C -0.1449(13) 0.5502(10) 0.5711(13) 0.079(4) Uani 1 1 d GU . . H29A H -0.1935 0.5376 0.5875 0.094 Uiso 1 1 calc R . . C30 C -0.158(2) 0.6623(14) 0.6182(17) 0.079(4) Uani 1 1 d DU . . H30A H -0.1406 0.7029 0.6005 0.094 Uiso 1 1 calc R . . C31 C -0.252(2) 0.6604(15) 0.592(2) 0.079(4) Uani 1 1 d DU . . H31A H -0.2770 0.6934 0.6167 0.118 Uiso 1 1 calc R . . H31B H -0.2730 0.6200 0.6042 0.118 Uiso 1 1 calc R . . H31C H -0.2681 0.6667 0.5367 0.118 Uiso 1 1 calc R . . C32 C -0.125(2) 0.6616(16) 0.7025(17) 0.079(4) Uani 1 1 d DU . . H32A H -0.1522 0.6948 0.7253 0.118 Uiso 1 1 calc R . . H32B H -0.0643 0.6683 0.7145 0.118 Uiso 1 1 calc R . . H32C H -0.1377 0.6214 0.7227 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 0.0424(12) 0.0482(15) 0.0512(12) -0.0021(10) 0.0068(9) 0.0089(8) Pb1' 0.088(9) 0.026(6) 0.038(5) -0.003(4) 0.012(5) 0.024(5) Pb2 0.0385(11) 0.0404(9) 0.0467(10) -0.0029(7) 0.0102(8) -0.0026(7) Pb3 0.0376(10) 0.0543(10) 0.0471(10) -0.0007(7) 0.0140(8) -0.0057(7) Pb4 0.0348(12) 0.0420(11) 0.0460(10) 0.0028(8) 0.0030(9) 0.0025(9) Pb4' 0.054(7) 0.016(4) 0.058(6) -0.018(3) 0.007(5) -0.001(4) I1 0.062(2) 0.0629(18) 0.0610(19) -0.0156(15) -0.0002(16) 0.0149(16) I1' 0.084(9) 0.049(6) 0.040(6) -0.012(6) 0.000(6) 0.022(6) I2 0.056(2) 0.047(2) 0.0397(16) -0.0018(13) 0.0076(14) 0.0057(14) I2' 0.097(8) 0.035(8) 0.032(6) -0.005(5) 0.002(6) 0.011(7) I3 0.0459(13) 0.0482(12) 0.0573(14) 0.0046(10) 0.0029(11) 0.0103(9) I4 0.068(2) 0.0583(19) 0.0419(16) -0.0030(13) 0.0186(17) -0.0186(17) I4' 0.067(8) 0.039(7) 0.037(6) 0.003(5) 0.011(6) -0.025(6) I5 0.102(2) 0.0553(13) 0.0531(14) 0.0027(12) 0.0005(14) 0.0011(14) I6 0.0580(15) 0.0458(12) 0.0768(17) -0.0174(11) 0.0098(13) -0.0025(10) I7 0.093(2) 0.0518(13) 0.0523(14) 0.0096(11) 0.0010(13) -0.0071(12) I8 0.0419(19) 0.0576(19) 0.0420(17) 0.0004(13) 0.0081(14) 0.0009(16) I8' 0.079(8) 0.027(6) 0.040(6) 0.002(5) 0.015(6) -0.004(7) I9 0.052(2) 0.0411(17) 0.060(3) -0.0024(15) 0.0086(16) 0.0002(14) I9' 0.056(9) 0.018(5) 0.060(12) -0.005(5) 0.010(6) -0.002(5) I10 0.0699(17) 0.0604(14) 0.0610(15) 0.0000(12) -0.0048(13) 0.0224(12) I11 0.0510(19) 0.053(2) 0.0392(15) -0.0020(15) 0.0076(13) 0.0182(14) I11' 0.075(9) 0.014(6) 0.051(6) 0.001(5) 0.018(6) 0.015(6) I12 0.089(2) 0.0515(13) 0.0577(15) -0.0070(12) 0.0056(13) 0.0129(13) N1 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C1 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C2 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C3 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C4 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C5 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) N2 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C6 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C7 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C8 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C9 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C10 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C11 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C12 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C13 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C14 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C15 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) C16 0.055(5) 0.065(4) 0.054(4) 0.006(4) 0.029(4) -0.010(4) N3 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C17 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C18 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C19 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C20 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C21 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C22 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C23 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) C24 0.078(8) 0.044(6) 0.067(7) -0.021(5) 0.020(6) 0.014(5) N4 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C25 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C26 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C27 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C28 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C29 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C30 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C31 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) C32 0.091(9) 0.058(6) 0.083(8) -0.022(6) 0.013(7) -0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I3 3.185(3) . ? Pb1 I10 3.206(4) 1_455 ? Pb1 I1 3.217(4) . ? Pb1 I11 3.227(4) 1_455 ? Pb1 I2 3.249(4) . ? Pb1 I12 3.297(4) 1_455 ? Pb1' I3 3.195(12) . ? Pb1' I11' 3.219(19) 1_455 ? Pb1' I10 3.260(13) 1_455 ? Pb1' I2' 3.32(2) . ? Pb1' I1' 3.37(2) . ? Pb2 I3 3.228(3) . ? Pb2 I6 3.244(3) . ? Pb2 I2 3.245(4) . ? Pb2 I4 3.304(4) . ? Pb2 I1 3.313(4) . ? Pb2 I5 3.365(4) . ? Pb2' I5 2.776(10) . ? Pb2' I6 2.995(8) . ? Pb2' I1' 3.150(16) . ? Pb2' I2' 3.254(19) . ? Pb2' I4' 3.321(18) . ? Pb3 I6 3.163(3) . ? Pb3 I4 3.219(4) . ? Pb3 I9 3.221(4) . ? Pb3 I7 3.227(3) . ? Pb3 I8 3.247(4) . ? Pb3 I5 3.282(3) . ? Pb3' I7 3.121(8) . ? Pb3' I8' 3.194(18) . ? Pb3' I4' 3.210(18) . ? Pb3' I9' 3.224(19) . ? Pb4 I9 3.232(4) . ? Pb4 I8 3.255(4) . ? Pb4 I11 3.267(4) . ? Pb4 I12 3.291(3) . ? Pb4 I7 3.318(4) . ? Pb4 I10 3.333(4) . ? Pb4' I10 2.766(12) . ? Pb4' I12 3.025(11) . ? Pb4' I9' 3.17(2) . ? Pb4' I11' 3.200(19) . ? Pb4' I8' 3.33(2) . ? I10 Pb1 3.206(4) 1_655 ? I10 Pb1' 3.260(13) 1_655 ? I11 Pb1 3.227(4) 1_655 ? I11' Pb1' 3.219(19) 1_655 ? I12 Pb1 3.297(4) 1_655 ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? N1 C11 1.504(17) . ? C1 C2 1.3900 . ? C1 H1A 0.9400 . ? C2 C3 1.3900 . ? C2 H2A 0.9400 . ? C3 C4 1.3900 . ? C3 C8 1.54260 . ? C4 C5 1.3900 . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? N2 C14 1.50(3) . ? C6 C7 1.3900 . ? C6 H6A 0.9400 . ? C7 C8 1.3900 . ? C7 H7A 0.9400 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 H9A 0.9400 . ? C10 H10A 0.9400 . ? C11 C12 1.50(4) . ? C11 C13 1.52(4) . ? C11 H11A 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.51(4) . ? C14 C16 1.56(4) . ? C14 H14A 0.9900 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? N3 C17 1.3900 . ? N3 C21 1.3900 . ? N3 C22 1.52(4) . ? C17 C18 1.3900 . ? C17 H17A 0.9400 . ? C18 C19 1.3900 . ? C18 H18A 0.9400 . ? C19 C20 1.3900 . ? C19 C19 1.51318 3_565 ? C20 C21 1.3900 . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 C23 1.51(4) . ? C22 C24 1.60(4) . ? C22 H22A 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? N4 C25 1.3900 . ? N4 C29 1.3900 . ? N4 C30 1.51(4) . ? C25 C26 1.3900 . ? C25 H25A 0.9400 . ? C26 C27 1.3900 . ? C26 H26A 0.9400 . ? C27 C28 1.3900 . ? C27 C27 1.56514 3_566 ? C28 C29 1.3900 . ? C28 H28A 0.9400 . ? C29 H29A 0.9400 . ? C30 C31 1.49(5) . ? C30 C32 1.48(4) . ? C30 H30A 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 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 I10 172.30(11) . 1_455 ? I3 Pb1 I1 84.22(9) . . ? I10 Pb1 I1 90.12(10) 1_455 . ? I3 Pb1 I11 94.82(10) . 1_455 ? I10 Pb1 I11 90.84(10) 1_455 1_455 ? I1 Pb1 I11 94.73(11) . 1_455 ? I3 Pb1 I2 84.55(10) . . ? I10 Pb1 I2 90.00(11) 1_455 . ? I1 Pb1 I2 87.48(10) . . ? I11 Pb1 I2 177.64(11) 1_455 . ? I3 Pb1 I12 101.63(9) . 1_455 ? I10 Pb1 I12 84.07(9) 1_455 1_455 ? I1 Pb1 I12 174.14(12) . 1_455 ? I11 Pb1 I12 84.58(9) 1_455 1_455 ? I2 Pb1 I12 93.31(10) . 1_455 ? I3 Pb1' I11' 86.4(4) . 1_455 ? I3 Pb1' I10 162.1(5) . 1_455 ? I11' Pb1' I10 79.3(4) 1_455 1_455 ? I3 Pb1' I2' 93.1(4) . . ? I11' Pb1' I2' 179.3(5) 1_455 . ? I10 Pb1' I2' 101.1(4) 1_455 . ? I3 Pb1' I1' 88.3(4) . . ? I11' Pb1' I1' 97.7(5) 1_455 . ? I10 Pb1' I1' 104.1(4) 1_455 . ? I2' Pb1' I1' 82.8(5) . . ? I3 Pb2 I6 79.45(7) . . ? I3 Pb2 I2 83.94(8) . . ? I6 Pb2 I2 108.31(9) . . ? I3 Pb2 I4 114.32(9) . . ? I6 Pb2 I4 87.41(9) . . ? I2 Pb2 I4 158.30(10) . . ? I3 Pb2 I1 82.04(9) . . ? I6 Pb2 I1 155.12(9) . . ? I2 Pb2 I1 85.95(9) . . ? I4 Pb2 I1 85.22(9) . . ? I3 Pb2 I5 154.10(8) . . ? I6 Pb2 I5 81.82(8) . . ? I2 Pb2 I5 85.15(8) . . ? I4 Pb2 I5 82.36(9) . . ? I1 Pb2 I5 120.52(9) . . ? I5 Pb2' I6 97.1(3) . . ? I5 Pb2' I1' 111.9(4) . . ? I6 Pb2' I1' 149.5(4) . . ? I5 Pb2' I2' 77.7(4) . . ? I6 Pb2' I2' 108.4(4) . . ? I1' Pb2' I2' 87.5(5) . . ? I5 Pb2' I4' 90.4(3) . . ? I6 Pb2' I4' 86.7(4) . . ? I1' Pb2' I4' 84.1(4) . . ? I2' Pb2' I4' 161.7(5) . . ? I6 Pb3 I4 90.28(10) . . ? I6 Pb3 I9 174.03(10) . . ? I4 Pb3 I9 93.76(10) . . ? I6 Pb3 I7 91.48(8) . . ? I4 Pb3 I7 96.46(10) . . ? I9 Pb3 I7 83.70(10) . . ? I6 Pb3 I8 91.61(10) . . ? I4 Pb3 I8 174.05(12) . . ? I9 Pb3 I8 84.81(10) . . ? I7 Pb3 I8 89.13(10) . . ? I6 Pb3 I5 84.37(8) . . ? I4 Pb3 I5 84.96(9) . . ? I9 Pb3 I5 100.36(10) . . ? I7 Pb3 I5 175.62(8) . . ? I8 Pb3 I5 89.61(9) . . ? I7 Pb3' I8' 97.7(4) . . ? I7 Pb3' I4' 81.6(4) . . ? I8' Pb3' I4' 179.3(6) . . ? I7 Pb3' I9' 93.8(5) . . ? I8' Pb3' I9' 86.1(5) . . ? I4' Pb3' I9' 94.1(5) . . ? I9 Pb4 I8 84.50(12) . . ? I9 Pb4 I11 110.81(13) . . ? I8 Pb4 I11 160.38(12) . . ? I9 Pb4 I12 155.76(11) . . ? I8 Pb4 I12 86.08(10) . . ? I11 Pb4 I12 84.06(9) . . ? I9 Pb4 I7 82.10(9) . . ? I8 Pb4 I7 87.44(9) . . ? I11 Pb4 I7 82.83(9) . . ? I12 Pb4 I7 119.75(10) . . ? I9 Pb4 I10 79.43(9) . . ? I8 Pb4 I10 107.49(10) . . ? I11 Pb4 I10 87.93(8) . . ? I12 Pb4 I10 82.21(9) . . ? I7 Pb4 I10 154.86(10) . . ? I10 Pb4' I12 97.4(4) . . ? I10 Pb4' I9' 74.6(4) . . ? I12 Pb4' I9' 155.8(6) . . ? I10 Pb4' I11' 87.4(4) . . ? I12 Pb4' I11' 91.9(4) . . ? I9' Pb4' I11' 110.2(6) . . ? I10 Pb4' I8' 108.5(5) . . ? I12 Pb4' I8' 76.0(4) . . ? I9' Pb4' I8' 84.8(6) . . ? I11' Pb4' I8' 161.0(5) . . ? Pb1 I1 Pb2 77.12(8) . . ? Pb2' I1' Pb1' 78.1(4) . . ? Pb2 I2 Pb1 77.64(9) . . ? Pb2' I2' Pb1' 77.4(4) . . ? Pb1 I3 Pb2 78.81(7) . . ? Pb1' I3 Pb2 65.9(3) . . ? Pb3 I4 Pb2 77.03(9) . . ? Pb3' I4' Pb2' 76.8(4) . . ? Pb2' I5 Pb3 69.07(17) . . ? Pb3 I5 Pb2 75.33(7) . . ? Pb2' I6 Pb3 68.29(18) . . ? Pb3 I6 Pb2 78.68(6) . . ? Pb3' I7 Pb4 64.7(2) . . ? Pb3 I7 Pb4 76.38(7) . . ? Pb3 I8 Pb4 76.99(9) . . ? Pb3' I8' Pb4' 75.9(4) . . ? Pb3 I9 Pb4 77.70(10) . . ? Pb4' I9' Pb3' 77.7(4) . . ? Pb4' I10 Pb1 70.6(2) . 1_655 ? Pb4' I10 Pb1' 83.2(3) . 1_655 ? Pb1 I10 Pb4 76.47(8) 1_655 . ? Pb1' I10 Pb4 89.1(3) 1_655 . ? Pb1 I11 Pb4 77.14(9) 1_655 . ? Pb4' I11' Pb1' 77.5(4) . 1_655 ? Pb4' I12 Pb1 66.4(2) . 1_655 ? Pb4 I12 Pb1 75.84(8) . 1_655 ? C1 N1 C5 120.0 . . ? C1 N1 C11 110.7(16) . . ? C5 N1 C11 129.1(16) . . ? N1 C1 C2 120.0 . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C8 122.20 . . ? C4 C3 C8 117.81 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5A 120.0 . . ? N1 C5 H5A 120.0 . . ? C6 N2 C10 120.0 . . ? C6 N2 C14 116.4(17) . . ? C10 N2 C14 123.3(17) . . ? C7 C6 N2 120.0 . . ? C7 C6 H6A 120.0 . . ? N2 C6 H6A 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 C3 118.98 . . ? C7 C8 C3 120.99 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 H10A 120.0 . . ? N2 C10 H10A 120.0 . . ? C12 C11 N1 108(2) . . ? C12 C11 C13 109(2) . . ? N1 C11 C13 104.3(19) . . ? C12 C11 H11A 111.8 . . ? N1 C11 H11A 111.8 . . ? C13 C11 H11A 111.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 110(2) . . ? N2 C14 C16 108(2) . . ? C15 C14 C16 100(2) . . ? N2 C14 H14A 112.6 . . ? C15 C14 H14A 112.6 . . ? C16 C14 H14A 112.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 N3 C21 120.0 . . ? C17 N3 C22 116.0(16) . . ? C21 N3 C22 123.9(16) . . ? C18 C17 N3 120.0 . . ? C18 C17 H17A 120.0 . . ? N3 C17 H17A 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 C19 116(2) . 3_565 ? C18 C19 C19 124(2) . 3_565 ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 N3 120.0 . . ? C20 C21 H21A 120.0 . . ? N3 C21 H21A 120.0 . . ? C23 C22 N3 117(2) . . ? C23 C22 C24 117(3) . . ? N3 C22 C24 103(3) . . ? C23 C22 H22A 106.2 . . ? N3 C22 H22A 106.2 . . ? C24 C22 H22A 106.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 N4 C29 120.0 . . ? C25 N4 C30 115(2) . . ? C29 N4 C30 124(2) . . ? C26 C25 N4 120.0 . . ? C26 C25 H25A 120.0 . . ? N4 C25 H25A 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 C27 120(3) . 3_566 ? C26 C27 C27 120(3) . 3_566 ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C29 N4 120.0 . . ? C28 C29 H29A 120.0 . . ? N4 C29 H29A 120.0 . . ? C31 C30 C32 115(3) . . ? C31 C30 N4 110(2) . . ? C32 C30 N4 113(3) . . ? C31 C30 H30A 105.9 . . ? C32 C30 H30A 105.9 . . ? N4 C30 H30A 105.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.544 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.305 #===END # Attachment '- JPLangCIF.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 776895' #TrackingRef '- JPLangCIF.CIF' _audit_creation_date 2009-06-15 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(I6 Pb2), 4(C8 H9 N2), 4(C H1.50 N0.50)' _chemical_formula_sum 'C38 H45 I12 N11 Pb4' _chemical_formula_weight 3007.45 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.743(3) _cell_length_b 14.793(3) _cell_length_c 28.814(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.97(3) _cell_angle_gamma 90.00 _cell_volume 7110(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10549 _cell_measurement_theta_min 3.0984 _cell_measurement_theta_max 27.4932 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5256.0 _exptl_absorpt_coefficient_mu 14.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2022 _exptl_absorpt_correction_T_max 0.2167 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16517 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7997 _reflns_number_gt 4774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0462P)^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 7997 _refine_ls_number_parameters 286 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.043 _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 Pb3 Pb 0.2500 0.2500 0.0000 0.0352(2) Uani 1 2 d S . . Pb1 Pb 0.0000 0.25419(6) -0.2500 0.0343(2) Uani 1 2 d S . . Pb2 Pb 0.13277(3) 0.25009(4) -0.126361(16) 0.03468(17) Uani 1 1 d . . . I4 I 0.12713(5) 0.39630(7) -0.04605(3) 0.0410(3) Uani 1 1 d . . . I3 I 0.11882(6) 0.09742(7) -0.20926(3) 0.0453(3) Uani 1 1 d . . . I5 I 0.32308(6) 0.24569(7) -0.10033(3) 0.0458(3) Uani 1 1 d . . . I6 I 0.37342(5) 0.40105(7) 0.04611(3) 0.0405(3) Uani 1 1 d . . . I2 I 0.05953(5) 0.26383(7) -0.35266(3) 0.0410(3) Uani 1 1 d . . . I1 I -0.13936(6) 0.39671(8) -0.29063(3) 0.0507(3) Uani 1 1 d . . . N1 N 0.7033(6) 0.4461(8) 0.1206(4) 0.037(3) Uani 1 1 d . . . N2 N 0.4272(8) 0.6209(11) 0.1267(5) 0.072(5) Uani 1 1 d . . . C1 C 0.6656(9) 0.4802(10) 0.0816(5) 0.046(4) Uani 1 1 d . . . H1A H 0.6901 0.4755 0.0536 0.055 Uiso 1 1 calc R . . C2 C 0.5937(9) 0.5209(11) 0.0813(5) 0.051(5) Uani 1 1 d . . . H2A H 0.5677 0.5434 0.0535 0.062 Uiso 1 1 calc R . . C3 C 0.5589(8) 0.5289(10) 0.1230(5) 0.038(4) Uani 1 1 d . . . C4 C 0.5976(8) 0.4953(10) 0.1632(5) 0.040(4) Uani 1 1 d . . . H4A H 0.5748 0.5011 0.1917 0.048 Uiso 1 1 calc R . . C5 C 0.6710(8) 0.4526(11) 0.1611(5) 0.046(4) Uani 1 1 d . . . H5A H 0.6979 0.4283 0.1882 0.056 Uiso 1 1 calc R . . C6 C 0.4840(9) 0.5783(11) 0.1249(5) 0.046(4) Uani 1 1 d . . . C7 C 0.7820(8) 0.4001(12) 0.1191(5) 0.055(5) Uani 1 1 d . . . H7A H 0.8130 0.4074 0.1492 0.066 Uiso 1 1 calc R . . H7B H 0.8118 0.4294 0.0954 0.066 Uiso 1 1 calc R . . C8 C 0.7737(9) 0.3000(12) 0.1079(6) 0.069(6) Uani 1 1 d . . . H8A H 0.8265 0.2733 0.1074 0.104 Uiso 1 1 calc R . . H8B H 0.7441 0.2923 0.0777 0.104 Uiso 1 1 calc R . . H8C H 0.7452 0.2704 0.1316 0.104 Uiso 1 1 calc R . . N3 N 0.1008(7) 0.4792(8) 0.1471(4) 0.041(3) Uani 1 1 d . . . N4 N 0.2587(8) 0.6247(11) 0.0124(5) 0.069(5) Uani 1 1 d . . . C9 C 0.1777(9) 0.4990(11) 0.1546(5) 0.050(4) Uani 1 1 d . . . H9A H 0.2027 0.4897 0.1847 0.061 Uiso 1 1 calc R . . C10 C 0.2229(8) 0.5318(13) 0.1218(5) 0.058(5) Uani 1 1 d . . . H10A H 0.2778 0.5439 0.1285 0.069 Uiso 1 1 calc R . . C11 C 0.1846(8) 0.5470(11) 0.0775(5) 0.044(4) Uani 1 1 d . . . C12 C 0.1049(8) 0.5284(10) 0.0693(5) 0.046(4) Uani 1 1 d . . . H12A H 0.0784 0.5386 0.0397 0.056 Uiso 1 1 calc R . . C13 C 0.0626(9) 0.4941(11) 0.1052(5) 0.049(4) Uani 1 1 d . . . H13A H 0.0075 0.4817 0.0998 0.059 Uiso 1 1 calc R . . C14 C 0.2291(9) 0.5906(13) 0.0408(5) 0.052(5) Uani 1 1 d . . . C15 C 0.0554(10) 0.4514(13) 0.1860(6) 0.068(6) Uani 1 1 d . . . H15A H 0.0929 0.4385 0.2133 0.082 Uiso 1 1 calc R . . H15B H 0.0207 0.5012 0.1942 0.082 Uiso 1 1 calc R . . C16 C 0.0076(10) 0.3736(16) 0.1752(6) 0.106(9) Uani 1 1 d . . . H16A H -0.0214 0.3578 0.2017 0.159 Uiso 1 1 calc R . . H16B H 0.0419 0.3236 0.1679 0.159 Uiso 1 1 calc R . . H16C H -0.0301 0.3864 0.1485 0.159 Uiso 1 1 calc R . . C17 C 0.0595(11) 0.7022(15) -0.0301(7) 0.075(3) Uani 1 1 d U . . N5 N 0.0612(8) 0.6399(11) -0.0517(5) 0.075(3) Uani 1 1 d U . . C18 C 0.0558(10) 0.7806(13) 0.0007(6) 0.075(3) Uani 1 1 d U . . H18A H 0.0039 0.8095 -0.0049 0.112 Uiso 1 1 calc R . . H18B H 0.0976 0.8232 -0.0056 0.112 Uiso 1 1 calc R . . H18C H 0.0635 0.7609 0.0329 0.112 Uiso 1 1 calc R . . N6 N 0.8096(12) 0.329(2) 0.2357(7) 0.044(5) Uani 0.50 1 d PU . . C20 C 0.8591(14) 0.176(2) 0.2491(9) 0.044(5) Uani 0.50 1 d PU . . H20A H 0.9157 0.1768 0.2444 0.066 Uiso 0.50 1 calc PR . . H20B H 0.8341 0.1234 0.2340 0.066 Uiso 0.50 1 calc PR . . H20C H 0.8526 0.1738 0.2822 0.066 Uiso 0.50 1 calc PR . . C19 C 0.8231(17) 0.253(2) 0.2303(9) 0.044(5) Uani 0.50 1 d PU . . 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 Pb3 0.0354(4) 0.0382(6) 0.0307(4) -0.0033(3) -0.0048(3) 0.0040(4) Pb1 0.0368(4) 0.0349(5) 0.0298(4) 0.000 -0.0043(3) 0.000 Pb2 0.0382(3) 0.0359(4) 0.0288(3) -0.0019(2) -0.0034(2) -0.0008(3) I4 0.0445(5) 0.0374(7) 0.0395(5) -0.0069(4) -0.0049(4) 0.0091(5) I3 0.0558(6) 0.0434(7) 0.0348(5) -0.0064(4) -0.0077(4) 0.0136(5) I5 0.0378(5) 0.0483(8) 0.0521(6) -0.0088(5) 0.0089(4) -0.0015(5) I6 0.0453(5) 0.0383(7) 0.0374(5) 0.0016(4) 0.0003(4) -0.0032(5) I2 0.0382(5) 0.0428(7) 0.0426(5) 0.0088(5) 0.0072(4) 0.0023(5) I1 0.0575(6) 0.0459(8) 0.0472(6) -0.0079(5) -0.0050(4) 0.0137(6) N1 0.041(7) 0.023(7) 0.049(8) -0.003(5) 0.012(5) -0.018(6) N2 0.057(9) 0.065(13) 0.095(13) 0.017(9) 0.005(8) 0.017(9) C1 0.059(10) 0.030(10) 0.050(10) -0.007(7) 0.005(7) 0.007(8) C2 0.055(9) 0.065(14) 0.032(8) 0.007(7) -0.008(6) 0.012(9) C3 0.032(7) 0.033(10) 0.048(9) -0.004(7) 0.008(6) -0.004(7) C4 0.046(8) 0.043(11) 0.032(8) 0.011(7) 0.012(6) -0.002(8) C5 0.048(9) 0.063(13) 0.028(8) -0.002(7) 0.004(6) -0.011(8) C6 0.052(9) 0.035(11) 0.051(10) 0.001(7) 0.005(7) -0.001(8) C7 0.039(8) 0.066(15) 0.060(11) 0.006(9) 0.008(7) 0.008(9) C8 0.041(10) 0.043(13) 0.124(17) 0.011(11) 0.015(9) 0.009(9) N3 0.047(7) 0.036(9) 0.042(7) -0.012(6) 0.006(5) 0.003(6) N4 0.081(11) 0.063(13) 0.064(11) -0.021(8) 0.019(8) -0.007(9) C9 0.055(9) 0.055(12) 0.038(9) -0.010(8) -0.014(7) 0.022(9) C10 0.034(8) 0.086(16) 0.053(11) 0.001(10) 0.003(7) 0.019(9) C11 0.034(7) 0.054(12) 0.041(9) -0.022(7) -0.009(6) 0.017(8) C12 0.055(9) 0.042(11) 0.040(9) -0.017(7) -0.007(7) 0.013(8) C13 0.059(10) 0.050(12) 0.036(9) -0.012(7) -0.012(7) 0.009(8) C14 0.052(10) 0.067(14) 0.038(9) -0.010(9) 0.004(7) 0.016(9) C15 0.067(12) 0.071(16) 0.069(13) -0.025(10) 0.014(9) -0.032(11) C16 0.085(14) 0.17(3) 0.071(15) -0.019(15) 0.042(11) -0.035(16) C17 0.083(7) 0.061(9) 0.079(8) -0.026(5) -0.003(5) -0.001(6) N5 0.083(7) 0.061(9) 0.079(8) -0.026(5) -0.003(5) -0.001(6) C18 0.083(7) 0.061(9) 0.079(8) -0.026(5) -0.003(5) -0.001(6) N6 0.036(8) 0.067(14) 0.033(8) 0.014(9) 0.023(6) 0.005(10) C20 0.036(8) 0.067(14) 0.033(8) 0.014(9) 0.023(6) 0.005(10) C19 0.036(8) 0.067(14) 0.033(8) 0.014(9) 0.023(6) 0.005(10) _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 Pb3 I4 3.1943(11) 7 ? Pb3 I4 3.1943(11) . ? Pb3 I5 3.2361(13) . ? Pb3 I5 3.2361(13) 7 ? Pb3 I6 3.2485(11) 7 ? Pb3 I6 3.2485(11) . ? Pb3 Pb2 3.9838(12) . ? Pb3 Pb2 3.9838(12) 7 ? Pb1 I2 3.2053(12) 2_554 ? Pb1 I2 3.2053(12) . ? Pb1 I3 3.2108(13) 2_554 ? Pb1 I3 3.2108(13) . ? Pb1 I1 3.2843(13) 2_554 ? Pb1 I1 3.2843(13) . ? Pb1 Pb2 4.0330(13) . ? Pb1 Pb2 4.0330(13) 2_554 ? Pb2 I4 3.1750(12) . ? Pb2 I5 3.2102(13) . ? Pb2 I6 3.2245(12) 7 ? Pb2 I2 3.2305(12) 2_554 ? Pb2 I1 3.2378(12) 2_554 ? Pb2 I3 3.2808(12) . ? I6 Pb2 3.2245(12) 7 ? I2 Pb2 3.2305(12) 2_554 ? I1 Pb2 3.2378(12) 2_554 ? N1 C5 1.330(15) . ? N1 C1 1.340(16) . ? N1 C7 1.487(17) . ? N2 C6 1.146(17) . ? C1 C2 1.346(18) . ? C1 H1A 0.9400 . ? C2 C3 1.386(17) . ? C2 H2A 0.9400 . ? C3 C4 1.370(17) . ? C3 C6 1.456(19) . ? C4 C5 1.388(18) . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C7 C8 1.52(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? N3 C9 1.320(17) . ? N3 C13 1.336(16) . ? N3 C15 1.466(18) . ? N4 C14 1.114(18) . ? C9 C10 1.35(2) . ? C9 H9A 0.9400 . ? C10 C11 1.397(17) . ? C10 H10A 0.9400 . ? C11 C12 1.363(17) . ? C11 C14 1.49(2) . ? C12 C13 1.398(19) . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C15 C16 1.42(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N5 1.11(2) . ? C17 C18 1.46(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? N6 C19 1.15(4) . ? C20 C19 1.38(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 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 I4 Pb3 I4 180.00(4) 7 . ? I4 Pb3 I5 94.47(3) 7 . ? I4 Pb3 I5 85.53(3) . . ? I4 Pb3 I5 85.53(3) 7 7 ? I4 Pb3 I5 94.47(3) . 7 ? I5 Pb3 I5 180.00(5) . 7 ? I4 Pb3 I6 93.89(3) 7 7 ? I4 Pb3 I6 86.11(3) . 7 ? I5 Pb3 I6 84.11(3) . 7 ? I5 Pb3 I6 95.89(3) 7 7 ? I4 Pb3 I6 86.11(3) 7 . ? I4 Pb3 I6 93.89(3) . . ? I5 Pb3 I6 95.89(3) . . ? I5 Pb3 I6 84.11(3) 7 . ? I6 Pb3 I6 180.00(4) 7 . ? I4 Pb3 Pb2 128.93(2) 7 . ? I4 Pb3 Pb2 51.07(2) . . ? I5 Pb3 Pb2 51.54(2) . . ? I5 Pb3 Pb2 128.46(2) 7 . ? I6 Pb3 Pb2 51.74(2) 7 . ? I6 Pb3 Pb2 128.26(2) . . ? I4 Pb3 Pb2 51.07(2) 7 7 ? I4 Pb3 Pb2 128.93(2) . 7 ? I5 Pb3 Pb2 128.46(2) . 7 ? I5 Pb3 Pb2 51.54(2) 7 7 ? I6 Pb3 Pb2 128.26(2) 7 7 ? I6 Pb3 Pb2 51.74(2) . 7 ? Pb2 Pb3 Pb2 180.000(18) . 7 ? I2 Pb1 I2 174.90(5) 2_554 . ? I2 Pb1 I3 97.88(3) 2_554 2_554 ? I2 Pb1 I3 85.82(3) . 2_554 ? I2 Pb1 I3 85.82(3) 2_554 . ? I2 Pb1 I3 97.88(3) . . ? I3 Pb1 I3 87.51(5) 2_554 . ? I2 Pb1 I1 84.87(3) 2_554 2_554 ? I2 Pb1 I1 91.85(3) . 2_554 ? I3 Pb1 I1 172.99(3) 2_554 2_554 ? I3 Pb1 I1 86.26(3) . 2_554 ? I2 Pb1 I1 91.85(3) 2_554 . ? I2 Pb1 I1 84.87(3) . . ? I3 Pb1 I1 86.26(3) 2_554 . ? I3 Pb1 I1 172.99(3) . . ? I1 Pb1 I1 100.13(5) 2_554 . ? I2 Pb1 Pb2 51.48(2) 2_554 . ? I2 Pb1 Pb2 128.62(2) . . ? I3 Pb1 Pb2 126.07(3) 2_554 . ? I3 Pb1 Pb2 52.38(2) . . ? I1 Pb1 Pb2 51.29(2) 2_554 . ? I1 Pb1 Pb2 130.15(3) . . ? I2 Pb1 Pb2 128.62(2) 2_554 2_554 ? I2 Pb1 Pb2 51.48(2) . 2_554 ? I3 Pb1 Pb2 52.38(2) 2_554 2_554 ? I3 Pb1 Pb2 126.07(3) . 2_554 ? I1 Pb1 Pb2 130.15(3) 2_554 2_554 ? I1 Pb1 Pb2 51.29(2) . 2_554 ? Pb2 Pb1 Pb2 178.27(3) . 2_554 ? I4 Pb2 I5 86.28(3) . . ? I4 Pb2 I6 86.84(3) . 7 ? I5 Pb2 I6 84.92(3) . 7 ? I4 Pb2 I2 90.08(3) . 2_554 ? I5 Pb2 I2 176.36(3) . 2_554 ? I6 Pb2 I2 94.84(3) 7 2_554 ? I4 Pb2 I1 95.00(4) . 2_554 ? I5 Pb2 I1 95.13(4) . 2_554 ? I6 Pb2 I1 178.16(3) 7 2_554 ? I2 Pb2 I1 85.23(4) 2_554 2_554 ? I4 Pb2 I3 174.19(3) . . ? I5 Pb2 I3 99.37(4) . . ? I6 Pb2 I3 92.30(3) 7 . ? I2 Pb2 I3 84.27(3) 2_554 . ? I1 Pb2 I3 85.88(3) 2_554 . ? I4 Pb2 Pb3 51.50(2) . . ? I5 Pb2 Pb3 52.12(3) . . ? I6 Pb2 Pb3 52.29(2) 7 . ? I2 Pb2 Pb3 125.11(3) 2_554 . ? I1 Pb2 Pb3 129.03(2) 2_554 . ? I3 Pb2 Pb3 131.57(2) . . ? I4 Pb2 Pb1 125.78(3) . . ? I5 Pb2 Pb1 131.81(3) . . ? I6 Pb2 Pb1 126.47(3) 7 . ? I2 Pb2 Pb1 50.92(3) 2_554 . ? I1 Pb2 Pb1 52.32(2) 2_554 . ? I3 Pb2 Pb1 50.82(2) . . ? Pb3 Pb2 Pb1 175.993(15) . . ? Pb2 I4 Pb3 77.43(3) . . ? Pb1 I3 Pb2 76.81(3) . . ? Pb2 I5 Pb3 76.34(3) . . ? Pb2 I6 Pb3 75.97(3) 7 . ? Pb1 I2 Pb2 77.61(3) . 2_554 ? Pb2 I1 Pb1 76.39(3) 2_554 . ? C5 N1 C1 120.7(13) . . ? C5 N1 C7 119.2(12) . . ? C1 N1 C7 120.1(12) . . ? N1 C1 C2 122.0(14) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C1 C2 C3 118.4(13) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 119.8(13) . . ? C4 C3 C6 119.8(13) . . ? C2 C3 C6 120.2(13) . . ? C3 C4 C5 119.0(13) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 C4 120.0(13) . . ? N1 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? N2 C6 C3 176.6(19) . . ? N1 C7 C8 112.8(12) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 N3 C13 119.7(13) . . ? C9 N3 C15 120.0(13) . . ? C13 N3 C15 119.9(13) . . ? N3 C9 C10 124.2(14) . . ? N3 C9 H9A 117.9 . . ? C10 C9 H9A 117.9 . . ? C9 C10 C11 117.2(14) . . ? C9 C10 H10A 121.4 . . ? C11 C10 H10A 121.4 . . ? C12 C11 C10 119.4(15) . . ? C12 C11 C14 120.5(13) . . ? C10 C11 C14 119.9(13) . . ? C11 C12 C13 119.8(14) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? N3 C13 C12 119.7(14) . . ? N3 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? N4 C14 C11 176.4(18) . . ? C16 C15 N3 112.2(14) . . ? C16 C15 H15A 109.2 . . ? N3 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? N3 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 176(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N6 C19 C20 146(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.692 _refine_diff_density_min -2.210 _refine_diff_density_rms 0.301 #===END #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 776896' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H11 N2, I3 Pb' _chemical_formula_sum 'C9 H11 I3 N2 Pb' _chemical_formula_weight 735.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 7.8610(11) _cell_length_b 12.7769(19) _cell_length_c 16.133(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.655(4) _cell_angle_gamma 90.00 _cell_volume 1606.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6671 _cell_measurement_theta_min 3.0058 _cell_measurement_theta_max 27.5087 _exptl_crystal_description Rod _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 16.249 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.276 _exptl_absorpt_correction_T_max 0.377 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9048 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3651 _reflns_number_gt 2354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.1562P)^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 3651 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2694 _refine_ls_wR_factor_gt 0.2498 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 0.5000 0.5000 0.5000 0.0324(3) Uani 1 2 d S . . Pb2 Pb 1.0000 0.5000 0.5000 0.0318(3) Uani 1 2 d S . . I1 I 0.75521(19) 0.69762(11) 0.51180(9) 0.0398(4) Uani 1 1 d . . . I2 I 0.78502(18) 0.38397(12) 0.63203(9) 0.0386(4) Uani 1 1 d . . . I3 I 0.70904(19) 0.41481(12) 0.35511(9) 0.0396(4) Uani 1 1 d . . . N1 N 0.694(3) 0.8931(16) 0.3179(11) 0.044(5) Uani 1 1 d . . . N2 N 0.832(4) 0.5474(19) 0.1550(15) 0.064(7) Uani 1 1 d . . . C1 C 0.843(3) 0.8847(18) 0.2807(15) 0.046(6) Uani 1 1 d . . . H1 H 0.9171 0.9427 0.2814 0.055 Uiso 1 1 calc R . . C2 C 0.884(3) 0.796(2) 0.2439(14) 0.049(6) Uani 1 1 d . . . H2 H 0.9892 0.7901 0.2224 0.058 Uiso 1 1 calc R . . C3 C 0.773(3) 0.7126(18) 0.2377(15) 0.042(5) Uani 1 1 d . . . C4 C 0.623(3) 0.7200(19) 0.2770(13) 0.040(5) Uani 1 1 d . . . H4 H 0.5473 0.6628 0.2774 0.048 Uiso 1 1 calc R . . C5 C 0.590(3) 0.8119(17) 0.3140(14) 0.039(5) Uani 1 1 d . . . H5 H 0.4883 0.8178 0.3382 0.046 Uiso 1 1 calc R . . C6 C 0.807(3) 0.617(2) 0.1954(15) 0.044(5) Uani 1 1 d . . . C7 C 0.658(4) 0.993(2) 0.3555(18) 0.059(8) Uani 1 1 d . . . H7A H 0.5356 0.9974 0.3601 0.071 Uiso 1 1 calc R . . H7B H 0.6853 1.0497 0.3181 0.071 Uiso 1 1 calc R . . C8 C 0.758(4) 1.011(2) 0.4405(19) 0.063(8) Uani 1 1 d . . . H8A H 0.8811 1.0095 0.4363 0.076 Uiso 1 1 calc R . . H8B H 0.7328 0.9550 0.4783 0.076 Uiso 1 1 calc R . . C9 C 0.713(6) 1.116(2) 0.477(2) 0.090(12) Uani 1 1 d . . . H9A H 0.7798 1.1251 0.5314 0.135 Uiso 1 1 calc R . . H9B H 0.5918 1.1171 0.4824 0.135 Uiso 1 1 calc R . . H9C H 0.7391 1.1718 0.4399 0.135 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 0.0263(6) 0.0395(6) 0.0315(6) -0.0004(5) 0.0041(4) 0.0009(4) Pb2 0.0259(6) 0.0367(6) 0.0326(6) 0.0013(5) 0.0035(4) 0.0003(4) I1 0.0469(9) 0.0327(7) 0.0384(8) -0.0006(5) 0.0000(6) 0.0028(6) I2 0.0327(7) 0.0459(8) 0.0369(8) 0.0096(6) 0.0038(6) -0.0002(6) I3 0.0348(7) 0.0501(8) 0.0339(8) -0.0076(6) 0.0044(6) 0.0002(6) N1 0.060(13) 0.049(11) 0.021(9) 0.007(8) -0.003(9) 0.006(10) N2 0.092(19) 0.056(13) 0.046(14) -0.004(11) 0.016(13) 0.024(14) C1 0.059(15) 0.038(12) 0.038(13) 0.009(10) -0.007(11) -0.014(11) C2 0.053(14) 0.063(16) 0.029(12) 0.013(11) 0.003(10) -0.012(12) C3 0.041(13) 0.038(11) 0.046(14) 0.008(10) 0.006(10) -0.003(10) C4 0.039(12) 0.061(14) 0.019(10) -0.002(9) -0.002(9) -0.016(11) C5 0.038(12) 0.049(12) 0.033(11) -0.002(10) 0.018(9) -0.004(10) C6 0.030(11) 0.063(15) 0.040(13) 0.002(12) 0.007(10) 0.003(11) C7 0.071(19) 0.060(16) 0.046(16) 0.007(13) 0.004(14) 0.022(15) C8 0.09(2) 0.043(13) 0.060(18) -0.002(12) 0.020(16) 0.002(15) C9 0.15(4) 0.043(15) 0.08(2) -0.002(15) 0.05(2) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I1 3.2148(15) . ? Pb1 I1 3.2148(15) 3_666 ? Pb1 I3 3.2207(15) 3_666 ? Pb1 I3 3.2207(15) . ? Pb1 I2 3.2378(14) 3_666 ? Pb1 I2 3.2378(14) . ? Pb2 I1 3.1957(15) . ? Pb2 I1 3.1957(15) 3_766 ? Pb2 I3 3.2336(14) . ? Pb2 I3 3.2336(14) 3_766 ? Pb2 I2 3.2480(15) 3_766 ? Pb2 I2 3.2480(15) . ? N1 C5 1.31(3) . ? N1 C1 1.39(3) . ? N1 C7 1.46(3) . ? N2 C6 1.13(3) . ? C1 C2 1.34(4) . ? C1 H1 0.9400 . ? C2 C3 1.37(3) . ? C2 H2 0.9400 . ? C3 C4 1.42(3) . ? C3 C6 1.44(3) . ? C4 C5 1.36(3) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C7 C8 1.50(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.52(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 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 I1 Pb1 I1 180.0 . 3_666 ? I1 Pb1 I3 93.80(4) . 3_666 ? I1 Pb1 I3 86.20(4) 3_666 3_666 ? I1 Pb1 I3 86.20(4) . . ? I1 Pb1 I3 93.80(4) 3_666 . ? I3 Pb1 I3 180.0 3_666 . ? I1 Pb1 I2 92.93(4) . 3_666 ? I1 Pb1 I2 87.08(4) 3_666 3_666 ? I3 Pb1 I2 86.99(4) 3_666 3_666 ? I3 Pb1 I2 93.01(4) . 3_666 ? I1 Pb1 I2 87.08(4) . . ? I1 Pb1 I2 92.92(4) 3_666 . ? I3 Pb1 I2 93.01(4) 3_666 . ? I3 Pb1 I2 86.99(4) . . ? I2 Pb1 I2 180.0 3_666 . ? I1 Pb2 I1 180.0 . 3_766 ? I1 Pb2 I3 86.30(4) . . ? I1 Pb2 I3 93.70(4) 3_766 . ? I1 Pb2 I3 93.70(4) . 3_766 ? I1 Pb2 I3 86.30(4) 3_766 3_766 ? I3 Pb2 I3 180.0 . 3_766 ? I1 Pb2 I2 92.78(4) . 3_766 ? I1 Pb2 I2 87.22(4) 3_766 3_766 ? I3 Pb2 I2 93.40(4) . 3_766 ? I3 Pb2 I2 86.60(4) 3_766 3_766 ? I1 Pb2 I2 87.22(4) . . ? I1 Pb2 I2 92.78(4) 3_766 . ? I3 Pb2 I2 86.60(4) . . ? I3 Pb2 I2 93.40(4) 3_766 . ? I2 Pb2 I2 180.00(5) 3_766 . ? Pb2 I1 Pb1 75.63(3) . . ? Pb1 I2 Pb2 74.60(3) . . ? Pb1 I3 Pb2 75.03(3) . . ? C5 N1 C1 118(2) . . ? C5 N1 C7 124(2) . . ? C1 N1 C7 118(2) . . ? C2 C1 N1 121(2) . . ? C2 C1 H1 119.3 . . ? N1 C1 H1 119.3 . . ? C1 C2 C3 120(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 119(2) . . ? C2 C3 C6 122(2) . . ? C4 C3 C6 119(2) . . ? C5 C4 C3 118(2) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 124(2) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C3 173(3) . . ? N1 C7 C8 114(2) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 112(3) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.710 _refine_diff_density_min -2.232 _refine_diff_density_rms 0.544 #===END #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 776897' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I6 Pb2, 3(C9 H11 N2), I3 Pb' _chemical_formula_sum 'C27 H33 I9 N6 Pb3' _chemical_formula_weight 2205.29 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' 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 Trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.208(3) _cell_length_b 19.208(3) _cell_length_c 7.8129(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2496.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4826 _cell_measurement_theta_min 3.2402 _cell_measurement_theta_max 27.4739 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 15.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2548 _exptl_absorpt_correction_T_max 0.3031 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12015 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3804 _reflns_number_gt 2813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0182P)^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 SHELXL _refine_ls_extinction_coef 0.00110(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3804 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 0.6667 0.3333 0.35201(6) 0.03040(16) Uani 1 3 d S . . Pb2 Pb 0.6667 0.3333 0.85782(6) 0.03355(17) Uani 1 3 d S . . Pb3 Pb 1.0000 0.0000 1.0000 0.0294(2) Uani 1 6 d S . . Pb4 Pb 1.0000 0.0000 1.5000 0.0324(2) Uani 1 6 d S . . I1 I 0.51606(4) 0.29067(4) 0.10822(7) 0.0490(2) Uani 1 1 d . . . I2 I 0.62739(3) 0.44194(3) 0.60736(7) 0.03532(17) Uani 1 1 d . . . I3 I 1.15267(3) 0.09818(3) 1.24836(7) 0.03521(17) Uani 1 1 d . . . N1 N 1.3478(4) 0.3095(5) 1.8316(9) 0.0395(19) Uani 1 1 d . . . N2 N 1.3251(6) 0.0677(6) 1.4633(12) 0.089(3) Uani 1 1 d . . . C1 C 1.4085(5) 0.3224(6) 1.7283(11) 0.049(3) Uani 1 1 d . . . H1 H 1.4548 0.3736 1.7233 0.059 Uiso 1 1 calc R . . C2 C 1.4032(5) 0.2615(6) 1.6302(11) 0.047(3) Uani 1 1 d . . . H2 H 1.4459 0.2708 1.5571 0.056 Uiso 1 1 calc R . . C3 C 1.3361(5) 0.1865(5) 1.6370(10) 0.037(2) Uani 1 1 d . . . C4 C 1.2737(6) 0.1735(5) 1.7456(11) 0.048(3) Uani 1 1 d . . . H4 H 1.2272 0.1227 1.7542 0.057 Uiso 1 1 calc R . . C5 C 1.2824(6) 0.2381(6) 1.8411(11) 0.047(3) Uani 1 1 d . . . H5 H 1.2406 0.2309 1.9147 0.056 Uiso 1 1 calc R . . C6 C 1.3294(6) 0.1200(7) 1.5378(12) 0.054(3) Uani 1 1 d . . . C7 C 1.3502(8) 0.3779(6) 1.9376(14) 0.081(4) Uani 1 1 d . . . H7 H 1.2954 0.3689 1.9172 0.098 Uiso 1 1 calc R . . C8 C 1.3986(8) 0.4557(7) 1.8602(14) 0.106(5) Uani 1 1 d . . . H8A H 1.3875 0.4521 1.7384 0.159 Uiso 1 1 calc R . . H8B H 1.4550 0.4735 1.8781 0.159 Uiso 1 1 calc R . . H8C H 1.3858 0.4939 1.9120 0.159 Uiso 1 1 calc R . . C9 C 1.3469(9) 0.3623(8) 2.1172(13) 0.114(5) Uani 1 1 d . . . H9A H 1.4004 0.3778 2.1584 0.171 Uiso 1 1 calc R . . H9B H 1.3113 0.3055 2.1381 0.171 Uiso 1 1 calc R . . H9C H 1.3270 0.3931 2.1769 0.171 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 0.0336(2) 0.0336(2) 0.0240(2) 0.000 0.000 0.01681(12) Pb2 0.0377(2) 0.0377(2) 0.0253(3) 0.000 0.000 0.01883(12) Pb3 0.0306(3) 0.0306(3) 0.0270(4) 0.000 0.000 0.01528(15) Pb4 0.0353(3) 0.0353(3) 0.0267(4) 0.000 0.000 0.01766(16) I1 0.0386(4) 0.0710(5) 0.0409(3) 0.0031(3) -0.0019(3) 0.0299(4) I2 0.0355(4) 0.0313(4) 0.0421(3) 0.0010(3) 0.0041(3) 0.0189(3) I3 0.0275(3) 0.0346(4) 0.0424(3) 0.0009(3) -0.0024(3) 0.0146(3) N1 0.033(5) 0.038(5) 0.048(4) -0.012(4) 0.000(4) 0.018(4) N2 0.087(8) 0.104(9) 0.100(7) -0.058(7) -0.040(6) 0.065(7) C1 0.026(6) 0.035(6) 0.068(6) 0.011(5) 0.013(5) 0.003(5) C2 0.026(6) 0.061(7) 0.052(5) -0.008(5) 0.000(5) 0.021(5) C3 0.034(6) 0.041(6) 0.040(5) -0.011(5) -0.013(4) 0.022(5) C4 0.043(6) 0.027(6) 0.066(6) -0.005(5) 0.010(5) 0.012(5) C5 0.040(6) 0.044(7) 0.057(6) 0.003(5) 0.012(5) 0.021(6) C6 0.035(6) 0.066(8) 0.061(6) -0.016(6) -0.003(5) 0.025(6) C7 0.103(11) 0.029(7) 0.088(8) -0.015(7) 0.006(8) 0.015(7) C8 0.154(14) 0.046(8) 0.127(11) -0.030(8) -0.016(10) 0.057(9) C9 0.175(16) 0.102(12) 0.080(9) -0.045(8) -0.003(10) 0.082(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 I1 3.2089(7) 2_655 ? Pb1 I1 3.2089(7) 3_665 ? Pb1 I1 3.2089(7) . ? Pb1 I2 3.2365(7) 3_665 ? Pb1 I2 3.2365(7) 2_655 ? Pb1 I2 3.2365(7) . ? Pb2 I2 3.2131(7) 2_655 ? Pb2 I2 3.2131(7) 3_665 ? Pb2 I2 3.2131(7) . ? Pb2 I1 3.2398(8) 2_656 ? Pb2 I1 3.2398(8) 3_666 ? Pb2 I1 3.2398(8) 1_556 ? Pb3 I3 3.2235(7) . ? Pb3 I3 3.2235(7) 4_757 ? Pb3 I3 3.2235(7) 3_765 ? Pb3 I3 3.2235(6) 2_645 ? Pb3 I3 3.2235(7) 6_547 ? Pb3 I3 3.2235(7) 5_667 ? Pb4 I3 3.2390(7) 3_765 ? Pb4 I3 3.2390(7) 6_548 ? Pb4 I3 3.2390(7) 5_668 ? Pb4 I3 3.2390(7) 4_758 ? Pb4 I3 3.2390(7) 2_645 ? Pb4 I3 3.2390(7) . ? I1 Pb2 3.2398(8) 1_554 ? N1 C5 1.320(10) . ? N1 C1 1.335(10) . ? N1 C7 1.534(12) . ? N2 C6 1.127(11) . ? C1 C2 1.360(11) . ? C1 H1 0.9400 . ? C2 C3 1.372(11) . ? C2 H2 0.9400 . ? C3 C4 1.385(11) . ? C3 C6 1.445(13) . ? C4 C5 1.384(11) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C7 C9 1.429(12) . ? C7 C8 1.441(13) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 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 I1 Pb1 I1 88.37(2) 2_655 3_665 ? I1 Pb1 I1 88.37(2) 2_655 . ? I1 Pb1 I1 88.37(2) 3_665 . ? I1 Pb1 I2 92.210(18) 2_655 3_665 ? I1 Pb1 I2 93.417(18) 3_665 3_665 ? I1 Pb1 I2 178.139(18) . 3_665 ? I1 Pb1 I2 93.417(18) 2_655 2_655 ? I1 Pb1 I2 178.139(18) 3_665 2_655 ? I1 Pb1 I2 92.210(18) . 2_655 ? I2 Pb1 I2 85.99(2) 3_665 2_655 ? I1 Pb1 I2 178.139(18) 2_655 . ? I1 Pb1 I2 92.210(18) 3_665 . ? I1 Pb1 I2 93.417(18) . . ? I2 Pb1 I2 85.99(2) 3_665 . ? I2 Pb1 I2 85.99(2) 2_655 . ? I2 Pb2 I2 86.77(2) 2_655 3_665 ? I2 Pb2 I2 86.77(2) 2_655 . ? I2 Pb2 I2 86.77(2) 3_665 . ? I2 Pb2 I1 93.565(18) 2_655 2_656 ? I2 Pb2 I1 92.361(18) 3_665 2_656 ? I2 Pb2 I1 179.051(17) . 2_656 ? I2 Pb2 I1 179.051(16) 2_655 3_666 ? I2 Pb2 I1 93.565(18) 3_665 3_666 ? I2 Pb2 I1 92.361(18) . 3_666 ? I1 Pb2 I1 87.31(2) 2_656 3_666 ? I2 Pb2 I1 92.360(18) 2_655 1_556 ? I2 Pb2 I1 179.051(16) 3_665 1_556 ? I2 Pb2 I1 93.565(18) . 1_556 ? I1 Pb2 I1 87.31(2) 2_656 1_556 ? I1 Pb2 I1 87.31(2) 3_666 1_556 ? I3 Pb3 I3 180.000(18) . 4_757 ? I3 Pb3 I3 87.506(17) . 3_765 ? I3 Pb3 I3 92.494(17) 4_757 3_765 ? I3 Pb3 I3 87.506(17) . 2_645 ? I3 Pb3 I3 92.494(17) 4_757 2_645 ? I3 Pb3 I3 87.505(17) 3_765 2_645 ? I3 Pb3 I3 92.494(17) . 6_547 ? I3 Pb3 I3 87.505(17) 4_757 6_547 ? I3 Pb3 I3 180.000(15) 3_765 6_547 ? I3 Pb3 I3 92.494(17) 2_645 6_547 ? I3 Pb3 I3 92.494(17) . 5_667 ? I3 Pb3 I3 87.506(17) 4_757 5_667 ? I3 Pb3 I3 92.495(17) 3_765 5_667 ? I3 Pb3 I3 180.0 2_645 5_667 ? I3 Pb3 I3 87.506(17) 6_547 5_667 ? I3 Pb4 I3 180.0 3_765 6_548 ? I3 Pb4 I3 93.018(17) 3_765 5_668 ? I3 Pb4 I3 86.982(17) 6_548 5_668 ? I3 Pb4 I3 93.018(17) 3_765 4_758 ? I3 Pb4 I3 86.982(17) 6_548 4_758 ? I3 Pb4 I3 86.982(17) 5_668 4_758 ? I3 Pb4 I3 86.982(17) 3_765 2_645 ? I3 Pb4 I3 93.018(17) 6_548 2_645 ? I3 Pb4 I3 180.0 5_668 2_645 ? I3 Pb4 I3 93.018(17) 4_758 2_645 ? I3 Pb4 I3 86.982(17) 3_765 . ? I3 Pb4 I3 93.018(17) 6_548 . ? I3 Pb4 I3 93.018(17) 5_668 . ? I3 Pb4 I3 180.000(18) 4_758 . ? I3 Pb4 I3 86.982(17) 2_645 . ? Pb1 I1 Pb2 73.56(2) . 1_554 ? Pb2 I2 Pb1 75.57(2) . . ? Pb3 I3 Pb4 74.382(18) . . ? C5 N1 C1 121.0(8) . . ? C5 N1 C7 117.7(8) . . ? C1 N1 C7 121.2(8) . . ? N1 C1 C2 119.9(9) . . ? N1 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C1 C2 C3 120.5(9) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 119.2(8) . . ? C2 C3 C6 121.9(9) . . ? C4 C3 C6 118.9(9) . . ? C5 C4 C3 117.6(9) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 121.8(8) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N2 C6 C3 178.4(12) . . ? C9 C7 C8 124.5(10) . . ? C9 C7 N1 111.8(10) . . ? C8 C7 N1 112.9(9) . . ? C9 C7 H7 101.0 . . ? C8 C7 H7 101.0 . . ? N1 C7 H7 101.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.803 _refine_diff_density_min -2.054 _refine_diff_density_rms 0.233 #===END #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 776898' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H11 N2, I3 Pb' _chemical_formula_sum 'C13 H11 I3 N2 Pb' _chemical_formula_weight 783.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.0356(16) _cell_length_b 14.126(3) _cell_length_c 16.065(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.41(3) _cell_angle_gamma 90.00 _cell_volume 1820.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5616 _cell_measurement_theta_min 3.1243 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Orange-red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 14.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1445 _exptl_absorpt_correction_T_max 0.1615 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17293 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3323 _reflns_number_gt 2709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0451P)^2^+17.0530P] 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 SHELXL _refine_ls_extinction_coef 0.00116(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3323 _refine_ls_number_parameters 170 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.016 _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 0.5000 0.5000 0.0000 0.0508(2) Uani 1 2 d S . . Pb2 Pb 1.0000 0.5000 0.0000 0.0512(2) Uani 1 2 d S . . I1 I 0.75339(11) 0.67849(6) 0.02003(6) 0.0618(3) Uani 1 1 d . . . I2 I 0.76170(11) 0.39566(6) 0.12753(6) 0.0599(3) Uani 1 1 d . . . I3 I 0.27167(11) 0.56193(7) 0.14966(6) 0.0601(3) Uani 1 1 d . . . N1 N 0.6437(15) 0.6204(9) 0.3253(8) 0.072(3) Uani 1 1 d . . . N2 N 0.959(3) 0.8948(14) 0.1799(11) 0.134(7) Uani 1 1 d . . . C1 C 0.584(2) 0.7044(13) 0.3236(10) 0.080(5) Uani 1 1 d . . . H1A H 0.4830 0.7158 0.3476 0.096 Uiso 1 1 calc R . . C2 C 0.662(2) 0.7760(12) 0.2882(10) 0.081(5) Uani 1 1 d . . . H2A H 0.6172 0.8366 0.2893 0.098 Uiso 1 1 calc R . . C3 C 0.8112(19) 0.7606(10) 0.2497(8) 0.060(3) Uani 1 1 d . . . C4 C 0.875(2) 0.6705(11) 0.2538(9) 0.071(4) Uani 1 1 d . . . H4A H 0.9758 0.6567 0.2310 0.085 Uiso 1 1 calc R . . C5 C 0.788(2) 0.6017(11) 0.2915(9) 0.071(4) Uani 1 1 d . . . H5A H 0.8299 0.5403 0.2938 0.085 Uiso 1 1 calc R . . C6 C 0.892(2) 0.8336(14) 0.2112(11) 0.090(5) Uani 1 1 d . . . C7 C 0.549(2) 0.5397(12) 0.3633(13) 0.095(4) Uani 1 1 d U . . H7A H 0.4627 0.5667 0.3959 0.115 Uiso 1 1 calc R . . H7B H 0.4931 0.5038 0.3183 0.115 Uiso 1 1 calc R . . C8 C 0.645(2) 0.4759(12) 0.4150(11) 0.095(4) Uani 1 1 d DU . . C9 C 0.646(3) 0.3772(14) 0.4059(14) 0.119(6) Uani 1 1 d U . . H9A H 0.5834 0.3497 0.3618 0.143 Uiso 1 1 calc R . . C10 C 0.735(3) 0.3220(14) 0.4589(16) 0.120(6) Uani 1 1 d U . . H10A H 0.7352 0.2568 0.4507 0.144 Uiso 1 1 calc R . . C11 C 0.822(3) 0.3591(14) 0.5234(14) 0.109(6) Uani 1 1 d U . . H11A H 0.8791 0.3188 0.5611 0.130 Uiso 1 1 calc R . . C12 C 0.832(2) 0.4491(13) 0.5353(13) 0.105(6) Uani 1 1 d U . . H12A H 0.8996 0.4728 0.5794 0.126 Uiso 1 1 calc R . . C13 C 0.7421(18) 0.5105(11) 0.4836(9) 0.078(4) Uani 1 1 d DU . . H13A H 0.7460 0.5752 0.4942 0.093 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 0.0343(4) 0.0599(5) 0.0582(5) -0.0036(3) 0.0030(3) 0.0007(3) Pb2 0.0347(4) 0.0563(4) 0.0627(5) -0.0013(3) 0.0040(3) -0.0013(3) I1 0.0599(6) 0.0492(5) 0.0749(7) -0.0064(4) -0.0077(5) -0.0013(4) I2 0.0538(5) 0.0625(6) 0.0630(6) 0.0051(4) 0.0007(4) -0.0053(4) I3 0.0536(5) 0.0705(6) 0.0568(6) -0.0089(4) 0.0079(4) 0.0068(4) N1 0.061(8) 0.081(9) 0.073(9) 0.019(7) -0.009(6) 0.003(7) N2 0.171(19) 0.138(16) 0.090(13) 0.026(11) -0.015(12) -0.059(14) C1 0.060(10) 0.103(14) 0.077(11) 0.005(10) 0.005(8) 0.034(9) C2 0.106(14) 0.070(10) 0.066(10) -0.017(8) -0.015(10) 0.038(10) C3 0.076(9) 0.059(8) 0.045(8) 0.000(6) -0.001(7) 0.003(7) C4 0.076(10) 0.078(11) 0.061(10) -0.002(8) 0.016(8) 0.011(8) C5 0.077(11) 0.078(10) 0.058(9) 0.003(8) -0.002(8) 0.032(9) C6 0.105(14) 0.098(13) 0.066(11) 0.019(10) -0.009(10) -0.012(11) C7 0.080(8) 0.090(7) 0.114(9) 0.029(7) -0.014(6) -0.019(6) C8 0.080(8) 0.090(7) 0.114(9) 0.029(7) -0.014(6) -0.019(6) C9 0.159(17) 0.085(8) 0.110(14) 0.000(9) -0.020(11) -0.015(11) C10 0.154(18) 0.069(9) 0.136(16) 0.004(9) -0.004(11) 0.007(10) C11 0.110(14) 0.087(8) 0.128(14) 0.034(10) -0.002(10) -0.004(10) C12 0.106(13) 0.091(9) 0.115(13) 0.027(9) -0.024(10) -0.017(10) C13 0.071(10) 0.067(8) 0.095(11) 0.011(6) 0.005(7) -0.008(7) _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 3.2063(12) . ? Pb1 I2 3.2063(12) 3_665 ? Pb1 I3 3.2305(12) . ? Pb1 I3 3.2305(12) 3_665 ? Pb1 I1 3.2448(10) 3_665 ? Pb1 I1 3.2448(10) . ? Pb2 I1 3.2347(10) 3_765 ? Pb2 I1 3.2347(10) . ? Pb2 I2 3.2408(12) 3_765 ? Pb2 I2 3.2408(12) . ? Pb2 I3 3.2692(13) 1_655 ? Pb2 I3 3.2692(13) 3_665 ? I3 Pb2 3.2692(13) 1_455 ? N1 C1 1.280(19) . ? N1 C5 1.336(18) . ? N1 C7 1.520(19) . ? N2 C6 1.15(2) . ? C1 C2 1.34(2) . ? C1 H1A 0.9300 . ? C2 C3 1.40(2) . ? C2 H2A 0.9300 . ? C3 C4 1.372(19) . ? C3 C6 1.38(2) . ? C4 C5 1.36(2) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.42(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.400(9) . ? C8 C9 1.40(2) . ? C9 C10 1.33(3) . ? C9 H9A 0.9300 . ? C10 C11 1.33(3) . ? C10 H10A 0.9300 . ? C11 C12 1.29(3) . ? C11 H11A 0.9300 . ? C12 C13 1.37(2) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I2 Pb1 I2 180.0 . 3_665 ? I2 Pb1 I3 91.66(3) . . ? I2 Pb1 I3 88.34(3) 3_665 . ? I2 Pb1 I3 88.34(3) . 3_665 ? I2 Pb1 I3 91.66(3) 3_665 3_665 ? I3 Pb1 I3 180.0 . 3_665 ? I2 Pb1 I1 95.17(3) . 3_665 ? I2 Pb1 I1 84.83(3) 3_665 3_665 ? I3 Pb1 I1 84.46(3) . 3_665 ? I3 Pb1 I1 95.54(3) 3_665 3_665 ? I2 Pb1 I1 84.83(3) . . ? I2 Pb1 I1 95.17(3) 3_665 . ? I3 Pb1 I1 95.54(3) . . ? I3 Pb1 I1 84.46(3) 3_665 . ? I1 Pb1 I1 180.000(19) 3_665 . ? I1 Pb2 I1 180.0 3_765 . ? I1 Pb2 I2 84.44(3) 3_765 3_765 ? I1 Pb2 I2 95.56(3) . 3_765 ? I1 Pb2 I2 95.56(3) 3_765 . ? I1 Pb2 I2 84.44(3) . . ? I2 Pb2 I2 180.0 3_765 . ? I1 Pb2 I3 84.00(3) 3_765 1_655 ? I1 Pb2 I3 96.00(3) . 1_655 ? I2 Pb2 I3 87.10(3) 3_765 1_655 ? I2 Pb2 I3 92.90(3) . 1_655 ? I1 Pb2 I3 96.00(3) 3_765 3_665 ? I1 Pb2 I3 84.00(3) . 3_665 ? I2 Pb2 I3 92.90(3) 3_765 3_665 ? I2 Pb2 I3 87.10(3) . 3_665 ? I3 Pb2 I3 180.0 1_655 3_665 ? Pb2 I1 Pb1 76.64(2) . . ? Pb1 I2 Pb2 77.10(2) . . ? Pb1 I3 Pb2 76.36(2) . 1_455 ? C1 N1 C5 120.7(15) . . ? C1 N1 C7 120.3(15) . . ? C5 N1 C7 118.9(14) . . ? N1 C1 C2 121.5(16) . . ? N1 C1 H1A 119.3 . . ? C2 C1 H1A 119.3 . . ? C1 C2 C3 120.7(14) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? C4 C3 C6 121.9(16) . . ? C4 C3 C2 116.7(14) . . ? C6 C3 C2 121.3(15) . . ? C5 C4 C3 119.0(14) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 121.3(14) . . ? N1 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? N2 C6 C3 179(2) . . ? C8 C7 N1 116.1(14) . . ? C8 C7 H7A 108.3 . . ? N1 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? N1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 115.0(17) . . ? C13 C8 C7 119.8(16) . . ? C9 C8 C7 125.1(16) . . ? C10 C9 C8 122(2) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C11 C10 C9 121(2) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 122(2) . . ? C12 C11 H11A 119.0 . . ? C10 C11 H11A 119.0 . . ? C11 C12 C13 121(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C8 C13 C12 120.2(16) . . ? C8 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.170 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.172 #===END #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 776899' #TrackingRef '- JPLangCIF.CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 N4, 2(C10 H8 N2), 2(I6 Pb2)' _chemical_formula_sum 'C40 H32 I12 N8 Pb4' _chemical_formula_weight 2976.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 7.7261(15) _cell_length_b 21.194(4) _cell_length_c 19.674(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.01(3) _cell_angle_gamma 90.00 _cell_volume 3213.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9676 _cell_measurement_theta_min 3.0612 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 16.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2266 _exptl_absorpt_correction_T_max 0.2460 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12948 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7200 _reflns_number_gt 4202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0141P)^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 7200 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.815 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.61742(4) 0.620498(16) -0.25171(2) 0.03687(11) Uani 1 1 d . . . Pb2 Pb 0.12342(4) 0.622534(16) -0.25193(2) 0.03676(10) Uani 1 1 d . . . I1 I 0.39516(9) 0.67441(3) -0.12986(4) 0.0491(2) Uani 1 1 d . . . I2 I 0.35627(8) 0.69215(3) -0.36234(4) 0.04071(18) Uani 1 1 d . . . I3 I 0.36160(7) 0.50055(3) -0.26126(4) 0.04080(18) Uani 1 1 d . . . I4 I 0.86818(8) 0.74350(3) -0.23119(4) 0.04213(19) Uani 1 1 d . . . I5 I 0.89098(8) 0.54352(3) -0.15404(4) 0.03966(17) Uani 1 1 d . . . I6 I -0.14210(8) 0.57721(3) -0.37140(4) 0.04165(18) Uani 1 1 d . . . N1 N -0.3914(10) 0.1265(3) 0.1273(5) 0.037(2) Uani 1 1 d . . . N2 N -0.1150(13) 0.1376(4) 0.3798(6) 0.072(3) Uani 1 1 d . . . N3 N 0.7436(11) 0.6434(4) 0.0587(5) 0.049(2) Uani 1 1 d . . . N4 N 1.0109(18) 0.8448(5) -0.0539(7) 0.124(5) Uani 1 1 d . . . C1 C -0.4627(13) 0.1627(4) 0.1730(6) 0.048(3) Uani 1 1 d . . . H1 H -0.5629 0.1861 0.1599 0.057 Uiso 1 1 calc R . . C2 C -0.3940(13) 0.1666(4) 0.2377(6) 0.051(3) Uani 1 1 d . . . H2 H -0.4447 0.1931 0.2690 0.062 Uiso 1 1 calc R . . C3 C -0.2476(13) 0.1310(4) 0.2582(6) 0.037(2) Uani 1 1 d . . . C4 C -0.1760(12) 0.0930(4) 0.2103(6) 0.045(3) Uani 1 1 d . . . H4 H -0.0774 0.0686 0.2227 0.054 Uiso 1 1 calc R . . C5 C -0.2490(13) 0.0911(4) 0.1442(6) 0.048(3) Uani 1 1 d . . . H5 H -0.2006 0.0655 0.1114 0.057 Uiso 1 1 calc R . . C6 C -0.1721(15) 0.1349(5) 0.3266(7) 0.052(3) Uani 1 1 d . . . C7 C -0.4639(15) 0.1260(4) 0.0551(6) 0.062(3) Uani 1 1 d . . . H7A H -0.3884 0.1511 0.0276 0.074 Uiso 1 1 calc R . . H7B H -0.5784 0.1462 0.0525 0.074 Uiso 1 1 calc R . . C8 C -0.4813(15) 0.0606(4) 0.0253(6) 0.048(3) Uani 1 1 d . . . C9 C -0.3637(13) 0.0376(5) -0.0175(6) 0.050(3) Uani 1 1 d . . . H9 H -0.2712 0.0633 -0.0293 0.060 Uiso 1 1 calc R . . C10 C -0.6207(14) 0.0226(5) 0.0434(6) 0.053(3) Uani 1 1 d . . . H10 H -0.7017 0.0381 0.0727 0.063 Uiso 1 1 calc R . . C11 C 0.7378(14) 0.6986(5) 0.0884(6) 0.060(3) Uani 1 1 d . . . H11 H 0.6819 0.7025 0.1291 0.072 Uiso 1 1 calc R . . C12 C 0.8124(15) 0.7512(5) 0.0609(7) 0.068(4) Uani 1 1 d . . . H12 H 0.8125 0.7900 0.0841 0.081 Uiso 1 1 calc R . . C13 C 0.8864(13) 0.7465(5) -0.0006(6) 0.047(3) Uani 1 1 d . . . C14 C 0.8910(14) 0.6896(5) -0.0322(6) 0.058(3) Uani 1 1 d . . . H14 H 0.9441 0.6848 -0.0734 0.069 Uiso 1 1 calc R . . C15 C 0.8137(15) 0.6383(5) -0.0010(6) 0.066(4) Uani 1 1 d . . . H15 H 0.8113 0.5989 -0.0231 0.079 Uiso 1 1 calc R . . C16 C 0.9587(18) 0.8019(5) -0.0281(7) 0.080(5) Uani 1 1 d . . . C17 C 0.6779(16) 0.5871(5) 0.0931(6) 0.077(4) Uani 1 1 d . . . H17A H 0.5971 0.6007 0.1264 0.093 Uiso 1 1 calc R . . H17B H 0.7755 0.5659 0.1181 0.093 Uiso 1 1 calc R . . C18 C 0.5868(13) 0.5405(5) 0.0448(6) 0.045(3) Uani 1 1 d . . . C19 C 0.6649(13) 0.4854(5) 0.0261(6) 0.058(3) Uani 1 1 d . . . H19 H 0.7775 0.4754 0.0440 0.070 Uiso 1 1 calc R . . C20 C 0.5783(14) 0.4458(4) -0.0183(7) 0.062(4) Uani 1 1 d . . . H20 H 0.6320 0.4083 -0.0312 0.074 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 0.03056(19) 0.0413(2) 0.0389(3) 0.0035(2) 0.00313(17) 0.00058(16) Pb2 0.03005(18) 0.0414(2) 0.0392(3) -0.0014(2) 0.00461(17) 0.00056(16) I1 0.0531(4) 0.0601(4) 0.0342(5) -0.0009(4) 0.0033(4) -0.0086(3) I2 0.0491(4) 0.0414(3) 0.0317(5) 0.0012(3) 0.0036(3) 0.0002(3) I3 0.0448(4) 0.0356(3) 0.0427(5) 0.0026(3) 0.0079(3) 0.0040(3) I4 0.0430(4) 0.0373(3) 0.0466(6) -0.0027(3) 0.0068(3) 0.0012(3) I5 0.0453(4) 0.0434(3) 0.0302(5) 0.0035(3) 0.0019(3) 0.0018(3) I6 0.0526(4) 0.0385(3) 0.0332(5) -0.0030(3) -0.0015(3) -0.0019(3) N1 0.065(5) 0.023(4) 0.023(6) 0.002(4) 0.004(5) 0.002(4) N2 0.106(8) 0.055(6) 0.051(9) -0.008(6) -0.012(7) -0.012(6) N3 0.080(6) 0.051(5) 0.016(6) -0.009(5) 0.004(5) -0.023(5) N4 0.214(14) 0.087(8) 0.077(12) -0.003(8) 0.041(10) -0.066(9) C1 0.060(7) 0.031(5) 0.050(9) -0.003(6) -0.014(6) 0.005(5) C2 0.067(7) 0.048(6) 0.040(9) -0.010(6) 0.011(6) -0.010(6) C3 0.053(6) 0.029(5) 0.029(7) 0.004(5) 0.001(5) -0.005(5) C4 0.051(6) 0.039(6) 0.044(9) 0.013(6) -0.003(6) 0.000(5) C5 0.080(8) 0.035(5) 0.030(8) 0.000(5) 0.015(6) 0.007(5) C6 0.070(8) 0.036(6) 0.049(10) -0.016(6) -0.003(7) -0.021(5) C7 0.112(9) 0.034(5) 0.037(9) 0.009(6) -0.014(8) -0.001(6) C8 0.073(8) 0.042(6) 0.027(7) -0.003(5) -0.008(6) -0.002(6) C9 0.066(7) 0.052(6) 0.033(8) 0.000(6) 0.011(6) -0.003(6) C10 0.075(8) 0.061(7) 0.021(7) -0.001(6) 0.001(6) 0.016(6) C11 0.081(8) 0.056(7) 0.046(9) -0.022(6) 0.029(7) -0.007(6) C12 0.089(9) 0.040(6) 0.075(12) -0.010(7) 0.011(8) -0.001(6) C13 0.053(7) 0.045(6) 0.045(9) -0.003(6) 0.010(6) -0.009(5) C14 0.094(9) 0.058(7) 0.023(7) 0.004(6) 0.019(7) -0.018(6) C15 0.117(11) 0.051(7) 0.030(9) 0.001(6) 0.008(8) -0.016(7) C16 0.128(12) 0.050(7) 0.063(12) -0.001(7) 0.001(9) -0.032(8) C17 0.147(11) 0.061(7) 0.025(8) -0.006(6) 0.012(8) -0.061(8) C18 0.059(7) 0.049(6) 0.025(7) 0.010(5) -0.010(6) -0.019(6) C19 0.052(7) 0.055(7) 0.065(11) 0.011(7) -0.011(6) -0.011(6) C20 0.064(7) 0.035(6) 0.087(12) 0.016(7) -0.001(7) -0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I5 3.2021(11) . ? Pb1 I3 3.2176(8) . ? Pb1 I6 3.2326(12) 1_655 ? Pb1 I2 3.2403(11) . ? Pb1 I1 3.2523(12) . ? Pb1 I4 3.2563(8) . ? Pb2 I6 3.1593(12) . ? Pb2 I3 3.1861(8) . ? Pb2 I5 3.1971(10) 1_455 ? Pb2 I2 3.2677(11) . ? Pb2 I1 3.2679(12) . ? Pb2 I4 3.2773(8) 1_455 ? I4 Pb2 3.2773(8) 1_655 ? I5 Pb2 3.1971(10) 1_655 ? I6 Pb1 3.2326(12) 1_455 ? N1 C1 1.330(12) . ? N1 C5 1.354(11) . ? N1 C7 1.490(12) . ? N2 C6 1.108(14) . ? N3 C11 1.310(11) . ? N3 C15 1.331(13) . ? N3 C17 1.480(11) . ? N4 C16 1.129(13) . ? C1 C2 1.348(14) . ? C1 H1 0.9400 . ? C2 C3 1.395(13) . ? C2 H2 0.9400 . ? C3 C4 1.384(13) . ? C3 C6 1.431(15) . ? C4 C5 1.382(13) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C7 C8 1.508(12) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.371(13) . ? C8 C10 1.411(13) . ? C9 C10 1.376(12) 3_455 ? C9 H9 0.9400 . ? C10 C9 1.376(12) 3_455 ? C10 H10 0.9400 . ? C11 C12 1.383(13) . ? C11 H11 0.9400 . ? C12 C13 1.377(15) . ? C12 H12 0.9400 . ? C13 C14 1.358(12) . ? C13 C16 1.423(14) . ? C14 C15 1.402(13) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C17 C18 1.511(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.375(13) . ? C18 C20 1.375(13) 3_665 ? C19 C20 1.355(14) . ? C19 H19 0.9400 . ? C20 C18 1.375(13) 3_665 ? C20 H20 0.9400 . ? 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 I5 Pb1 I3 90.54(2) . . ? I5 Pb1 I6 84.47(2) . 1_655 ? I3 Pb1 I6 96.62(2) . 1_655 ? I5 Pb1 I2 174.70(2) . . ? I3 Pb1 I2 88.85(3) . . ? I6 Pb1 I2 90.36(3) 1_655 . ? I5 Pb1 I1 95.57(3) . . ? I3 Pb1 I1 88.10(2) . . ? I6 Pb1 I1 175.284(19) 1_655 . ? I2 Pb1 I1 89.68(2) . . ? I5 Pb1 I4 88.36(3) . . ? I3 Pb1 I4 175.96(2) . . ? I6 Pb1 I4 87.15(2) 1_655 . ? I2 Pb1 I4 92.59(3) . . ? I1 Pb1 I4 88.14(2) . . ? I6 Pb2 I3 93.33(2) . . ? I6 Pb2 I5 85.76(2) . 1_455 ? I3 Pb2 I5 87.75(2) . 1_455 ? I6 Pb2 I2 90.10(3) . . ? I3 Pb2 I2 88.91(2) . . ? I5 Pb2 I2 174.52(2) 1_455 . ? I6 Pb2 I1 178.04(2) . . ? I3 Pb2 I1 88.36(2) . . ? I5 Pb2 I1 95.31(3) 1_455 . ? I2 Pb2 I1 88.93(2) . . ? I6 Pb2 I4 88.02(2) . 1_455 ? I3 Pb2 I4 175.51(2) . 1_455 ? I5 Pb2 I4 88.08(3) 1_455 1_455 ? I2 Pb2 I4 95.37(3) . 1_455 ? I1 Pb2 I4 90.38(2) . 1_455 ? Pb1 I1 Pb2 71.66(2) . . ? Pb1 I2 Pb2 71.81(2) . . ? Pb2 I3 Pb1 73.17(2) . . ? Pb1 I4 Pb2 73.51(2) . 1_655 ? Pb2 I5 Pb1 75.32(2) 1_655 . ? Pb2 I6 Pb1 75.41(2) . 1_455 ? C1 N1 C5 121.5(10) . . ? C1 N1 C7 120.1(9) . . ? C5 N1 C7 118.3(9) . . ? C11 N3 C15 119.7(10) . . ? C11 N3 C17 119.4(10) . . ? C15 N3 C17 120.8(9) . . ? N1 C1 C2 121.2(10) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C1 C2 C3 119.9(11) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 118.1(10) . . ? C4 C3 C6 121.2(10) . . ? C2 C3 C6 120.6(10) . . ? C5 C4 C3 120.2(10) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 119.0(10) . . ? N1 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N2 C6 C3 179.3(15) . . ? N1 C7 C8 113.2(8) . . ? N1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C10 120.1(9) . . ? C9 C8 C7 121.4(11) . . ? C10 C8 C7 118.4(11) . . ? C8 C9 C10 120.8(10) . 3_455 ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 3_455 . ? C9 C10 C8 119.1(10) 3_455 . ? C9 C10 H10 120.5 3_455 . ? C8 C10 H10 120.5 . . ? N3 C11 C12 121.1(11) . . ? N3 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 119.7(11) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 119.4(10) . . ? C14 C13 C16 122.4(12) . . ? C12 C13 C16 118.2(11) . . ? C13 C14 C15 117.6(11) . . ? C13 C14 H14 121.2 . . ? C15 C14 H14 121.2 . . ? N3 C15 C14 122.3(11) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? N4 C16 C13 175.5(16) . . ? N3 C17 C18 113.5(9) . . ? N3 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? N3 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C20 119.4(10) . 3_665 ? C19 C18 C17 122.0(10) . . ? C20 C18 C17 118.6(11) 3_665 . ? C20 C19 C18 119.5(10) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C18 121.1(10) . 3_665 ? C19 C20 H20 119.4 . . ? C18 C20 H20 119.4 3_665 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.340 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.228