# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mao, Jiang-Gao' _publ_contact_author_name 'Mao, Jiang-Gao' _publ_contact_author_email mjg@fjirsm.ac.cn _publ_section_title ; PbPt(IO3)6(H2O): A New Polar Material with Two Types of Stereoactive Lone-Pairs and a Very Large SHG Response ; # Attachment '- scf-Chem Comm.CIF' data_s _database_code_depnum_ccdc_archive 'CCDC 863192' #TrackingRef '- scf-Chem Comm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 I6 O19 Pb Pt' _chemical_formula_weight 1469.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source I I -0.4742 1.8119 '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' O O 0.0106 0.0060 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 11.3072(6) _cell_length_b 11.3072(6) _cell_length_c 11.2423(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1244.79(14) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Brick _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 29.812 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4566 _exptl_absorpt_process_details 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 Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 3231 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.43 _reflns_number_total 1218 _reflns_number_gt 1201 _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^)+(0.0000P)^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 0.00231(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.277(6) _refine_ls_number_reflns 1218 _refine_ls_number_parameters 84 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0163 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0350 _refine_ls_wR_factor_gt 0.0350 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 0.3333 0.6667 -0.16058(5) 0.01995(15) Uani 1 3 d S . . Pt1 Pt -0.3333 0.3333 0.05963(4) 0.00722(13) Uani 1 3 d S . . I1 I -0.02262(4) 0.59066(4) -0.03146(4) 0.00888(12) Uani 1 1 d . . . I2 I 0.71999(5) 0.74656(5) -0.12109(4) 0.00968(12) Uani 1 1 d . . . O1 O -0.1681(5) 0.4086(5) -0.0447(5) 0.0154(12) Uani 1 1 d . . . O2 O 0.0679(6) 0.5508(6) -0.1386(6) 0.0188(13) Uani 1 1 d . . . O3 O 0.0445(6) 0.5673(6) 0.1061(5) 0.0151(13) Uani 1 1 d . . . O4 O 0.8313(5) 0.9260(5) -0.1748(5) 0.0142(12) Uani 1 1 d . . . O5 O 0.6029(5) 0.7921(6) -0.0568(6) 0.0159(13) Uani 1 1 d . . . O6 O 0.8174(6) 0.7505(6) 0.0078(5) 0.0196(14) Uani 1 1 d . . . O1W O 0.3333 0.6667 0.0478(10) 0.020(2) Uani 1 3 d S . . H1WA H 0.4150 0.7023 0.0730 0.030 Uiso 0.6667 1 d PR . . 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 0.02027(19) 0.02027(19) 0.0193(3) 0.000 0.000 0.01014(9) Pt1 0.00616(15) 0.00616(15) 0.0093(3) 0.000 0.000 0.00308(7) I1 0.0085(2) 0.0084(2) 0.0106(3) 0.00051(19) 0.00118(18) 0.00483(19) I2 0.0091(2) 0.0087(2) 0.0119(3) 0.00166(18) 0.00262(19) 0.00496(19) O1 0.016(3) 0.010(3) 0.018(3) 0.000(2) 0.009(2) 0.004(2) O2 0.013(3) 0.017(3) 0.029(4) -0.009(3) 0.004(2) 0.009(2) O3 0.019(3) 0.019(3) 0.007(3) 0.000(2) 0.001(2) 0.009(3) O4 0.010(3) 0.009(3) 0.022(3) 0.004(2) 0.010(2) 0.003(2) O5 0.007(3) 0.015(3) 0.024(4) 0.001(2) 0.006(2) 0.005(2) O6 0.021(3) 0.025(3) 0.016(3) 0.006(3) 0.004(2) 0.013(3) O1W 0.014(3) 0.014(3) 0.032(7) 0.000 0.000 0.0072(16) _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 O1W 2.342(11) . ? Pb1 O2 2.618(6) . ? Pb1 O2 2.618(6) 3_565 ? Pb1 O2 2.618(6) 2_665 ? Pt1 O4 1.995(5) 5 ? Pt1 O4 1.995(5) 6_465 ? Pt1 O4 1.995(5) 4_345 ? Pt1 O1 2.000(5) 3_455 ? Pt1 O1 2.000(5) . ? Pt1 O1 2.000(5) 2_565 ? I1 O2 1.779(6) . ? I1 O3 1.799(6) . ? I1 O1 1.892(5) . ? I2 O5 1.795(6) . ? I2 O6 1.807(6) . ? I2 O4 1.874(5) . ? O4 Pt1 1.995(5) 7_654 ? O1W H1WA 0.8500 . ? 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 O1W Pb1 O2 84.58(14) . . ? O1W Pb1 O2 84.58(14) . 3_565 ? O2 Pb1 O2 119.12(5) . 3_565 ? O1W Pb1 O2 84.58(14) . 2_665 ? O2 Pb1 O2 119.12(5) . 2_665 ? O2 Pb1 O2 119.12(5) 3_565 2_665 ? O4 Pt1 O4 91.9(2) 5 6_465 ? O4 Pt1 O4 91.9(2) 5 4_345 ? O4 Pt1 O4 91.9(2) 6_465 4_345 ? O4 Pt1 O1 88.8(2) 5 3_455 ? O4 Pt1 O1 177.8(2) 6_465 3_455 ? O4 Pt1 O1 90.1(2) 4_345 3_455 ? O4 Pt1 O1 90.1(2) 5 . ? O4 Pt1 O1 88.8(2) 6_465 . ? O4 Pt1 O1 177.8(2) 4_345 . ? O1 Pt1 O1 89.1(2) 3_455 . ? O4 Pt1 O1 177.8(2) 5 2_565 ? O4 Pt1 O1 90.1(2) 6_465 2_565 ? O4 Pt1 O1 88.8(2) 4_345 2_565 ? O1 Pt1 O1 89.1(2) 3_455 2_565 ? O1 Pt1 O1 89.1(2) . 2_565 ? O2 I1 O3 101.9(3) . . ? O2 I1 O1 88.2(2) . . ? O3 I1 O1 96.2(3) . . ? O5 I2 O6 101.4(3) . . ? O5 I2 O4 90.7(2) . . ? O6 I2 O4 99.2(3) . . ? I1 O1 Pt1 122.4(3) . . ? I1 O2 Pb1 126.7(3) . . ? I2 O4 Pt1 128.1(3) . 7_654 ? Pb1 O1W H1WA 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.178 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.204