Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mercier, Nicolas' 'Blanchard, Philippe' 'Frere, Pierre' 'Riou, Amedee' 'Zhu, Xu-Hui' _publ_contact_author_name 'Dr Nicolas Mercier' _publ_contact_author_address ; IMMO laboratory 2 Bd lavoisier Angers 49035 FRANCE ; _publ_contact_author_email 'nicolas.mercier@univ-angers.fr' _publ_contact_author_fax '(33)2.41.73.54.05' _publ_contact_author_phone '(33)2.41.73.50.83' _publ_requested_journal 'Chem. Comm.' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM _publ_section_title ; (C4H3SCH2NH3)2(CH3NH3)Pb2I7 : non centrosymmetrical crystal structure of a bilayer hybrid perovskite ; _publ_section_references ; Allen, F.H., Kennard, O. & Taylor, R. (1983). Acc. Chem. Res. 16, 146-153. Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R., Garciia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1996) The DIRDIF96 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Enraf-Nonius (1994). CAD4Express Software. Enraf-Nonius, Delft, The Netherlands. Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565. Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, In the press. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Harms, K. & Wocadlo, S. (1995) XCAD-4. Program for Processing CAD-4 Diffractometer Data. University of Marburg, Germany. Johnson, C.K. (1965). ORTEP. Report ORNL-3794. Oak Ridge National Laboratory, Tennessee, USA. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G., & Taylor, R. (1992). International Tables for Crystallography, Volume C. Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Spek, A.L. (1990). Acta Cryst. A46, C34 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; data_per24b _database_code_CSD 187951 _audit_creation_date 2002-07-15T10:04:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C11 H19 I7 N3 Pb2 S2' _chemical_formula_sum 'C11 H19 I7 N3 Pb2 S2' _chemical_formula_weight 1560.09 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Aba2 _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-x, -y, z' 'x, y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' '-x, -y+1/2, z+1/2' _cell_length_a 8.838(2) _cell_length_b 41.5200(10) _cell_length_c 8.769(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3218(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 3.22 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2692 _exptl_absorpt_coefficient_mu 17.3 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.0152 _exptl_absorpt_correction_T_max 0.2422 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 12 -2 -1 -13 -3 -3 -7 5 _diffrn_reflns_number 5330 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.97 _diffrn_reflns_theta_full 30.97 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 2786 _reflns_number_gt 1854 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.000127(18) _refine_ls_number_reflns 2786 _refine_ls_number_parameters 122 _refine_ls_number_restraints 1 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0933 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(2) _refine_diff_density_max 1.742 _refine_diff_density_min -1.539 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# 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 0 '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' S S 0.1246 0.1234 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly S1 S -0.0331(16) 0.2139(2) -0.3811(14) 0.139(6) Uani 0.64(3) d P . . C3A C -0.0331(16) 0.2139(2) -0.3811(14) 0.139(6) Uani 0.36(3) d P . . N1 N -0.0682(17) 0.1390(4) -0.5735(14) 0.068(4) Uani 1 d . . . H1A H -0.0726 0.1178 -0.5613 0.102 Uiso 1 calc R . . H1B H -0.0417 0.1435 -0.6691 0.102 Uiso 1 calc R . . H1C H -0.1584 0.1476 -0.5539 0.102 Uiso 1 calc R . . C2 C 0.057(2) 0.1888(5) -0.483(3) 0.077(5) Uani 1 d . . . C1 C 0.046(3) 0.1527(4) -0.467(3) 0.087(6) Uani 1 d . . . H1D H 0.1439 0.1431 -0.4876 0.105 Uiso 1 calc R . . H1E H 0.018 0.1474 -0.363 0.105 Uiso 1 calc R . . C3 C 0.163(2) 0.2066(4) -0.600(2) 0.145(8) Uani 0.64(3) d P . . H3 H 0.2275 0.1986 -0.6749 0.174 Uiso 0.64(3) calc PR . . S1A S 0.163(2) 0.2066(4) -0.600(2) 0.145(8) Uani 0.36(3) d P . . C4 C 0.128(5) 0.2416(7) -0.549(4) 0.152(16) Uani 1 d . . . H4 H 0.1759 0.2593 -0.5925 0.183 Uiso 1 calc R . . C5 C 0.026(5) 0.2446(7) -0.440(4) 0.141(15) Uani 1 d . . . H5 H -0.006 0.2645 -0.4042 0.169 Uiso 1 calc R . . C6 C 0 0 0.451(7) 0.22(5) Uani 1 d S . . N2 N -0.062(7) -0.0115(9) 0.552(8) 0.16(3) Uani 0.5 d P . . Pb1 Pb -0.00130(6) 0.078612(10) 0.00119(18) 0.03460(11) Uani 1 d . . . I2 I -0.19537(12) 0.07517(3) -0.30465(11) 0.0523(3) Uani 1 d . . . I1 I 0 0 -0.0041(4) 0.0551(3) Uani 1 d S . . I4 I 0.20085(12) 0.07861(3) 0.29965(11) 0.0574(3) Uani 1 d . . . I3 I -0.03356(12) 0.15378(2) 0.01461(18) 0.0593(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.195(14) 0.053(5) 0.169(10) -0.017(6) 0.037(9) 0.013(6) C3A 0.195(14) 0.053(5) 0.169(10) -0.017(6) 0.037(9) 0.013(6) N1 0.060(9) 0.066(10) 0.078(9) 0.008(7) 0.014(7) -0.002(8) C2 0.068(10) 0.082(12) 0.081(11) -0.021(12) 0.010(11) -0.007(10) C1 0.089(13) 0.049(9) 0.125(18) -0.028(13) -0.025(13) 0.008(10) C3 0.129(14) 0.129(14) 0.177(16) 0.013(11) 0.026(10) -0.046(11) S1A 0.129(14) 0.129(14) 0.177(16) 0.013(11) 0.026(10) -0.046(11) C4 0.21(4) 0.08(2) 0.16(3) 0.05(2) -0.07(3) -0.09(2) C5 0.21(4) 0.057(16) 0.16(3) 0.005(17) 0.04(2) 0.020(19) C6 0.47(14) 0.05(3) 0.13(4) 0 0 -0.12(5) N2 0.21(6) 0.04(2) 0.23(7) -0.04(3) -0.14(5) 0.05(3) Pb1 0.03204(17) 0.0409(2) 0.03088(16) 0.0004(3) 0.00011(13) -0.00094(19) I2 0.0482(6) 0.0617(7) 0.0471(7) 0.0003(5) -0.0225(4) 0.0021(4) I1 0.0677(7) 0.0333(5) 0.0644(7) 0 0 0.0031(7) I4 0.0457(6) 0.0799(9) 0.0464(7) -0.0093(5) -0.0208(4) 0.0114(5) I3 0.0711(7) 0.0347(4) 0.0720(7) 0.0040(6) -0.0033(8) -0.0048(4) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 S1 C5 1.47(4) . ? S1 C2 1.59(2) . ? N1 C1 1.49(2) . ? C2 C1 1.51(3) . ? C2 C3 1.57(3) . ? C3 C4 1.55(4) . ? C4 C5 1.32(5) . ? C6 N2 1.15(8) 4 ? C6 N2 1.15(8) . ? N2 N2 1.46(12) 4 ? Pb1 I3 3.1361(10) . ? Pb1 I4 3.169(2) . ? Pb1 I2 3.1790(16) 7_445 ? Pb1 I2 3.187(2) . ? Pb1 I4 3.1898(17) 7_544 ? Pb1 I1 3.2643(4) . ? I2 Pb1 3.1790(16) 7_444 ? I1 Pb1 3.2643(4) 4 ? I4 Pb1 3.1898(17) 7_545 ? 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 C5 S1 C2 101.0(18) . . ? C1 C2 C3 124.4(18) . . ? C1 C2 S1 124.5(18) . . ? C3 C2 S1 111.0(15) . . ? N1 C1 C2 111.2(17) . . ? C4 C3 C2 98(2) . . ? C5 C4 C3 116(2) . . ? C4 C5 S1 115(3) . . ? N2 C6 N2 79(6) 4 . ? C6 N2 N2 51(3) . 4 ? I3 Pb1 I4 91.17(4) . . ? I3 Pb1 I2 87.02(3) . 7_445 ? I4 Pb1 I2 91.90(7) . 7_445 ? I3 Pb1 I2 91.56(4) . . ? I4 Pb1 I2 176.90(4) . . ? I2 Pb1 I2 89.70(4) 7_445 . ? I3 Pb1 I4 95.54(3) . 7_544 ? I4 Pb1 I4 89.33(4) . 7_544 ? I2 Pb1 I4 177.14(4) 7_445 7_544 ? I2 Pb1 I4 88.96(6) . 7_544 ? I3 Pb1 I1 174.81(3) . . ? I4 Pb1 I1 90.55(5) . . ? I2 Pb1 I1 88.03(4) 7_445 . ? I2 Pb1 I1 86.85(5) . . ? I4 Pb1 I1 89.38(4) 7_544 . ? Pb1 I2 Pb1 154.50(6) 7_444 . ? Pb1 I1 Pb1 178.38(12) . 4 ? Pb1 I4 Pb1 157.97(6) . 7_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A I2 . 0.89 3.06 3.722(14) 132.6 N1 H1A I4 1_554 0.89 3.16 3.631(16) 115.5 N1 H1B I3 1_554 0.89 2.81 3.676(13) 165.7 N1 H1C I3 7_444 0.89 2.8 3.655(15) 161.7 #====end data_per01 _database_code_CSD 187952 _audit_creation_date 2002-04-09T12:16:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C10 H16 I4 N2 Pb S2' _chemical_formula_sum 'C10 H16 I4 N2 Pb S2' _chemical_formula_weight 943.16 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.842(2) _cell_length_b 8.6930(10) _cell_length_c 28.995(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2228.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 14 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 13.29 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '' _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.7072 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -9 3 -3 9 4 4 0 _diffrn_reflns_number 6243 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.7 _diffrn_reflns_theta_max 29.96 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 3215 _reflns_number_gt 1844 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0406P)^2^+1.3137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00037(5) _refine_ls_number_reflns 3215 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0841 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.007 _refine_diff_density_max 1.271 _refine_diff_density_min -0.714 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb Pb -3.3944 10.1111 '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' S S 0.1246 0.1234 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pb Pb 0 -0.5 0.5 0.03635(10) Uani 1 d S . . I1 I 0.19187(4) -0.19094(5) 0.497285(14) 0.04976(14) Uani 1 d . . . I2 I 0.03191(6) -0.51481(5) 0.610092(16) 0.05727(14) Uani 1 d . . . S1 S 0.0383(7) -0.1217(6) 0.69727(15) 0.158(2) Uani 0.667(9) d P . A C3A C 0.0383(7) -0.1217(6) 0.69727(15) 0.158(2) Uani 0.333(9) d P . A C3 C -0.173(2) 0.063(2) 0.6911(7) 0.082(5) Uiso 0.667(9) d P 1 A H3 H -0.2562 0.1166 0.6799 0.098 Uiso 1 calc R 1 A S1A S -0.1477(19) 0.1259(15) 0.6883(6) 0.152(6) Uani 0.333(9) d P 2 A N N 0.0712(7) 0.0716(7) 0.5920(2) 0.0721(17) Uani 1 d . . . H0A H 0.0688 0.0644 0.5614 0.108 Uiso 1 calc R . . H0B H 0.1625 0.045 0.6022 0.108 Uiso 1 calc R . . H0C H 0.0513 0.168 0.6004 0.108 Uiso 1 calc R . . C1 C -0.0445(12) -0.0333(9) 0.6123(3) 0.084(3) Uani 1 d . . A H1A H -0.1417 -0.0114 0.5982 0.101 Uiso 1 calc R . . H1B H -0.0181 -0.1386 0.6047 0.101 Uiso 1 calc R . . C2 C -0.0588(10) -0.0190(8) 0.6631(3) 0.074(2) Uani 1 d . . . C5 C -0.033(2) -0.055(2) 0.7429(5) 0.159(6) Uani 1 d . . . H5 H -0.0028 -0.0894 0.7718 0.19 Uiso 1 calc R . A C4 C -0.132(2) 0.045(2) 0.7379(5) 0.157(7) Uani 1 d . . A H4 H -0.1734 0.1018 0.762 0.188 Uiso 1 calc R 1 B 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 Pb 0.03066(14) 0.03077(15) 0.04762(19) -0.00088(14) 0.00202(12) -0.00018(10) I1 0.0421(2) 0.0410(2) 0.0661(3) 0.00348(19) -0.00772(19) -0.01623(16) I2 0.0641(3) 0.0643(3) 0.0435(3) -0.0043(2) 0.00611(19) -0.0027(2) S1 0.209(5) 0.187(5) 0.078(3) 0.025(3) -0.009(3) 0.055(4) C3A 0.209(5) 0.187(5) 0.078(3) 0.025(3) -0.009(3) 0.055(4) S1A 0.193(13) 0.093(8) 0.170(12) 0.026(8) 0.077(9) 0.032(8) N 0.064(4) 0.072(4) 0.080(5) 0.000(3) -0.006(3) 0.007(3) C1 0.096(6) 0.073(5) 0.083(7) 0.022(5) 0.000(5) -0.002(5) C2 0.072(5) 0.090(5) 0.061(5) 0.002(4) -0.002(4) -0.011(4) C5 0.183(16) 0.240(19) 0.053(8) -0.007(10) -0.004(8) 0.010(14) C4 0.182(17) 0.180(15) 0.109(13) -0.061(11) 0.057(11) -0.064(12) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 Pb I1 3.1785(5) 5_546 ? Pb I1 3.1785(5) . ? Pb I1 3.1912(6) 8_655 ? Pb I1 3.1912(6) 4_446 ? Pb I2 3.2071(7) . ? Pb I2 3.2071(7) 5_546 ? I1 Pb 3.1912(6) 4_546 ? S1 C5 1.573(15) . ? S1 C2 1.586(9) . ? C3 C4 1.41(2) . ? C3 C2 1.48(2) . ? S1A C4 1.61(2) . ? S1A C2 1.655(15) . ? N C1 1.490(11) . ? C1 C2 1.485(12) . ? C5 C4 1.25(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Pb I1 180.000(15) 5_546 . ? I1 Pb I1 90.954(13) 5_546 8_655 ? I1 Pb I1 89.046(13) . 8_655 ? I1 Pb I1 89.046(13) 5_546 4_446 ? I1 Pb I1 90.954(13) . 4_446 ? I1 Pb I1 180 8_655 4_446 ? I1 Pb I2 89.334(10) 5_546 . ? I1 Pb I2 90.666(10) . . ? I1 Pb I2 85.904(11) 8_655 . ? I1 Pb I2 94.096(11) 4_446 . ? I1 Pb I2 90.666(10) 5_546 5_546 ? I1 Pb I2 89.334(10) . 5_546 ? I1 Pb I2 94.096(11) 8_655 5_546 ? I1 Pb I2 85.904(11) 4_446 5_546 ? I2 Pb I2 180 . 5_546 ? Pb I1 Pb 153.474(15) . 4_546 ? C5 S1 C2 95.9(8) . . ? C4 C3 C2 107.4(15) . . ? C4 S1A C2 91.3(8) . . ? C2 C1 N 113.5(8) . . ? C1 C2 C3 130.1(11) . . ? C1 C2 S1 121.8(7) . . ? C3 C2 S1 107.3(10) . . ? C1 C2 S1A 122.9(8) . . ? S1 C2 S1A 114.2(8) . . ? C4 C5 S1 116.2(13) . . ? C5 C4 C3 111.5(15) . . ? C5 C4 S1A 118.1(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N H0A I1 . 0.89 3.09 3.727(6) 129.9 N H0A I1 5_556 0.89 3.07 3.632(6) 123.1 N H0B I2 8_665 0.89 2.76 3.627(6) 164.6 N H0C I2 1_565 0.89 2.78 3.650(6) 167.1