# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guo-Cong Guo' _publ_contact_author_email gcguo@fjirsm.ac.cn loop_ _publ_author_name 'Guan-E Wang' 'Gang Xu' 'Ming-Sheng Wang' 'Jing Sun' 'Zhong-Ning Xu' 'Guo-Cong Guo' 'Jin-Shun Huang' data_14 _database_code_depnum_ccdc_archive 'CCDC 849193' #TrackingRef 'compound.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 N2,2 (I3 Pb),2 (H2 O)' _chemical_formula_sum 'C12 H18 I6 N2 O2 Pb2' _chemical_formula_weight 1398.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/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 4.5346(13) _cell_length_b 13.251(4) _cell_length_c 22.712(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.203(5) _cell_angle_gamma 90.00 _cell_volume 1364.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3535 _cell_measurement_theta_min 2.3614 _cell_measurement_theta_max 27.5165 _exptl_crystal_description acicular _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 19.116 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1616 _exptl_absorpt_correction_T_max 0.5152 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 Ultrax-Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11339 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2533 _reflns_number_gt 1467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2533 _refine_ls_number_parameters 104 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.25500(6) 0.02724(2) 0.091483(11) 0.04153(8) Uani 1 1 d . . . I1 I -0.24090(10) 0.18544(3) 0.13256(2) 0.05139(16) Uani 1 1 d . . . I2 I -0.24349(9) -0.12800(3) 0.044305(19) 0.04543(15) Uani 1 1 d . . . I3 I 0.25045(9) -0.08175(3) 0.212389(19) 0.04581(14) Uani 1 1 d . . . N1 N 0.7531(11) 0.0879(4) 0.2945(2) 0.072(2) Uani 1 1 d . . . H1A H 0.7372 0.0335 0.2717 0.109 Uiso 1 1 calc R . . H1B H 0.9259 0.1177 0.2881 0.109 Uiso 1 1 calc R . . H1C H 0.6078 0.1307 0.2861 0.109 Uiso 1 1 calc R . . C1 C 0.7336(6) 0.0573(3) 0.35739(9) 0.063(3) Uani 1 1 d G . . C2 C 0.6754(11) -0.0424(3) 0.3726(2) 0.131(3) Uani 1 1 d GU . . H2A H 0.6924 -0.0931 0.3445 0.157 Uiso 1 1 calc R . . C3 C 0.5918(14) -0.0662(5) 0.4297(2) 0.156(3) Uani 1 1 d GU . . H3A H 0.5528 -0.1329 0.4399 0.187 Uiso 1 1 calc R . . C4 C 0.5664(13) 0.0096(7) 0.47171(14) 0.147(3) Uani 1 1 d GDU . . C5 C 0.6246(12) 0.1092(6) 0.45654(14) 0.165(3) Uani 1 1 d GU . . H5A H 0.6076 0.1600 0.4846 0.198 Uiso 1 1 calc R . . C6 C 0.7082(10) 0.1331(4) 0.39938(17) 0.098(2) Uani 1 1 d GU . . H6A H 0.7472 0.1997 0.3892 0.118 Uiso 1 1 calc R . . O1W O 0.7490(10) -0.2932(3) 0.23546(14) 0.084(2) Uani 1 1 d D . . H1WA H 0.748(5) -0.2469(5) 0.2615(3) 0.109 Uiso 1 1 d D . . H1WB H 0.8454(18) -0.2667(8) 0.2072(3) 0.109 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.03587(13) 0.04873(15) 0.03997(15) 0.00122(14) -0.00061(12) 0.00048(14) I1 0.0476(3) 0.0448(3) 0.0618(3) -0.0025(2) -0.0018(3) 0.0016(2) I2 0.0475(3) 0.0422(3) 0.0465(3) 0.0023(2) -0.0003(2) -0.0002(2) I3 0.0453(3) 0.0497(3) 0.0424(3) 0.0058(2) -0.0001(2) 0.0010(2) N1 0.072(4) 0.056(4) 0.089(5) -0.016(4) -0.002(4) 0.000(4) C1 0.095(6) 0.065(5) 0.027(4) 0.001(4) -0.002(4) 0.002(5) C2 0.146(4) 0.115(4) 0.132(4) -0.001(4) 0.012(4) -0.021(4) C3 0.174(5) 0.153(5) 0.140(5) -0.014(4) 0.001(4) -0.004(4) C4 0.152(5) 0.143(4) 0.146(5) 0.000(4) 0.000(4) -0.002(4) C5 0.187(5) 0.151(5) 0.158(5) 0.010(4) 0.012(4) 0.003(4) C6 0.119(4) 0.081(4) 0.096(4) -0.010(3) 0.022(3) 0.005(3) O1W 0.100(4) 0.058(3) 0.094(4) 0.007(3) -0.009(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I3 3.1027(9) . ? Pb1 I1 3.2150(8) . ? Pb1 I2 3.2360(8) . ? Pb1 I1 3.2365(8) 1_655 ? Pb1 I2 3.2509(8) 1_655 ? Pb1 I2 3.3608(9) 3 ? I1 Pb1 3.2365(8) 1_455 ? I2 Pb1 3.2509(8) 1_455 ? I2 Pb1 3.3608(9) 3 ? N1 C1 1.488(6) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 C4 1.444(5) 3_656 ? C5 C6 1.3900 . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? O1W H1WA 0.852(6) . ? O1W H1WB 0.853(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Pb1 I1 92.281(19) . . ? I3 Pb1 I2 89.446(19) . . ? I1 Pb1 I2 91.26(2) . . ? I3 Pb1 I1 93.052(19) . 1_655 ? I1 Pb1 I1 89.32(2) . 1_655 ? I2 Pb1 I1 177.411(15) . 1_655 ? I3 Pb1 I2 90.230(19) . 1_655 ? I1 Pb1 I2 177.488(15) . 1_655 ? I2 Pb1 I2 88.70(2) . 1_655 ? I1 Pb1 I2 90.61(2) 1_655 1_655 ? I3 Pb1 I2 175.487(15) . 3 ? I1 Pb1 I2 89.925(18) . 3 ? I2 Pb1 I2 86.568(18) . 3 ? I1 Pb1 I2 90.910(18) 1_655 3 ? I2 Pb1 I2 87.565(18) 1_655 3 ? Pb1 I1 Pb1 89.32(2) . 1_455 ? Pb1 I2 Pb1 88.70(2) . 1_455 ? Pb1 I2 Pb1 93.432(18) . 3 ? Pb1 I2 Pb1 92.435(18) 1_455 3 ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C2 C1 C6 120.0 . . ? C2 C1 N1 120.6(3) . . ? C6 C1 N1 117.9(3) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C4 121.3(10) . 3_656 ? C5 C4 C4 117.9(10) . 3_656 ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? H1WA O1W H1WB 103.3(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.260 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.212