Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nicolas Mercier' _publ_contact_author_address ; Department of Chemistry University of Angers 2 Boulevard Lavoisier Angers 49045 FRANCE ; _publ_contact_author_email NICOLAS.MERCIER@UNIV-ANGERS.FR _publ_section_title ; PbnI4n+2(2n+2)- Ribbons (n= 3, 5) as Dimensional Reduction of 2D Perovskite Layer in Cystamine Cations Based Hybrids also Incorporating Iodine Molecules or Reversible Guest Water Molecules ; loop_ _publ_author_name N.Mercier 'Wenhua Bi.' J.-Y.Buzare G.Corbel C.Legein N.Louvain data_1 _database_code_depnum_ccdc_archive 'CCDC 625234' _audit_creation_date 2007-01-16T12:43:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_sum 'C16 H56 I16 N8 Pb3 S8' _chemical_formula_weight 3269.14 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.607(2) _cell_length_b 8.835(1) _cell_length_c 22.375(3) _cell_angle_alpha 90 _cell_angle_beta 102.81(1) _cell_angle_gamma 90 _cell_volume 3394.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 3.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860 _exptl_absorpt_coefficient_mu 14.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 0.481 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 26874 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 _reflns_number_total 5836 _reflns_number_gt 3684 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _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^)+(0.0196P)^2^+23.8848P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _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 0.000026(12) _refine_ls_number_reflns 5836 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0795 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.588 _refine_diff_density_min -1.681 #------------------ 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 Pb1 Pb 0.5 0.5 0.5 0.03352(17) Uani 1 d S . . Pb2 Pb 0.44070(2) 0.99061(5) 0.69293(2) 0.03169(13) Uani 1 d . . . I1 I 0.52773(6) 0.74427(9) 0.40275(4) 0.0595(3) Uani 1 d . . . I2 I 0.67272(6) 0.55071(11) 0.58067(5) 0.0657(3) Uani 1 d . . . I3 I 0.44769(5) 0.76497(9) 0.57709(4) 0.0509(2) Uani 1 d . . . I4 I 0.62664(4) 0.94194(10) 0.73211(4) 0.0575(3) Uani 1 d . . . I5 I 0.43870(5) 1.23456(10) 0.79306(4) 0.0577(3) Uani 1 d . . . I6 I 0.42497(5) 0.73389(10) 0.78297(4) 0.0610(3) Uani 1 d . . . I7 I 0.25518(4) 0.98620(10) 0.64179(4) 0.0527(2) Uani 1 d . . . I8 I 0.43002(6) 0.48917(12) 0.95674(5) 0.0795(3) Uani 1 d . . . S2 S 0.1886(3) 0.5981(5) 0.5598(2) 0.1085(19) Uani 1 d . . . S3 S 0.7926(2) 1.1591(4) 0.61942(17) 0.0619(10) Uani 1 d . . . S4 S 0.87603(18) 0.9926(4) 0.64154(16) 0.0578(9) Uani 1 d . . . N2 N 0.2509(6) 0.5558(16) 0.7009(6) 0.090(4) Uani 1 d . . B H1L H 0.2893 0.6231 0.7051 0.134 Uiso 1 calc R . . H1N H 0.2494 0.5174 0.7374 0.134 Uiso 1 calc R . . H1M H 0.2057 0.6011 0.685 0.134 Uiso 1 calc R . . N3 N 0.6279(7) 0.9815(14) 0.5665(6) 0.086(4) Uani 1 d . . . H01H H 0.6438 0.9623 0.6064 0.129 Uiso 1 calc R . . H01I H 0.5917 0.9144 0.5497 0.129 Uiso 1 calc R . . H01J H 0.6079 1.0743 0.5614 0.129 Uiso 1 calc R . . N4 N 0.9258(5) 1.0232(12) 0.7867(5) 0.061(3) Uani 1 d . . . H01A H 0.9557 0.9451 0.8022 0.092 Uiso 1 calc R . . H01B H 0.9228 1.0877 0.8167 0.092 Uiso 1 calc R . . H01C H 0.9464 1.0697 0.7588 0.092 Uiso 1 calc R . . C8 C 0.8469(7) 0.9681(16) 0.7578(6) 0.062(4) Uani 1 d . . . H01D H 0.8117 1.0539 0.7496 0.075 Uiso 1 calc R . . H01E H 0.8288 0.9021 0.7863 0.075 Uiso 1 calc R . . C6 C 0.7403(7) 1.1072(14) 0.5439(6) 0.060(4) Uani 1 d . . . H01F H 0.7069 1.1913 0.5271 0.072 Uiso 1 calc R . . H01G H 0.7779 1.0946 0.5184 0.072 Uiso 1 calc R . . C4 C 0.2637(11) 0.4387(18) 0.6617(7) 0.093(6) Uani 1 d . . . H1J H 0.222 0.3653 0.6582 0.111 Uiso 1 calc R . B H1K H 0.312 0.388 0.6803 0.111 Uiso 1 calc R . . C5 C 0.6924(7) 0.9711(13) 0.5379(6) 0.050(3) Uani 1 d . . . H02A H 0.6731 0.9495 0.4947 0.06 Uiso 1 calc R . . H02B H 0.7249 0.8866 0.5557 0.06 Uiso 1 calc R . . C7 C 0.8438(7) 0.8847(13) 0.6996(6) 0.047(3) Uani 1 d . . . H02C H 0.7906 0.8521 0.6834 0.056 Uiso 1 calc R . . H02D H 0.8758 0.7947 0.7085 0.056 Uiso 1 calc R . . C2 C 0.1120(9) 0.3761(18) 0.4640(7) 0.088(5) Uiso 1 d . . . H2F H 0.1638 0.3468 0.4604 0.106 Uiso 0.5 calc PR 2 A H2G H 0.0759 0.2961 0.4469 0.106 Uiso 0.5 calc PR 2 A H1F H 0.1544 0.3037 0.4733 0.106 Uiso 0.5 d PR 1 A H1G H 0.065 0.3172 0.4495 0.106 Uiso 0.5 d PR 1 A N1A N 0.0563(12) 0.567(2) 0.3894(11) 0.070(5) Uiso 0.600(17) d P 1 B H1C H 0.0642 0.6228 0.3583 0.105 Uiso 0.5 calc PR 1 B H1B H 0.052 0.6266 0.4204 0.105 Uiso 0.5 calc PR 1 B H1A H 0.0127 0.5133 0.3774 0.105 Uiso 0.5 calc PR 1 B N1B N 0.0967(18) 0.513(3) 0.3696(15) 0.070(5) Uiso 0.400(17) d P 2 B H2A H 0.1358 0.5721 0.365 0.105 Uiso 0.5 calc PR 2 B H2C H 0.0526 0.5447 0.3451 0.105 Uiso 0.5 calc PR 2 B H2B H 0.1062 0.4181 0.36 0.105 Uiso 0.5 calc PR 2 B C1A C 0.1222(14) 0.463(3) 0.4092(13) 0.061(6) Uiso 0.600(17) d P 1 B H1D H 0.1704 0.5207 0.4193 0.074 Uiso 0.5 calc PR 1 B H1E H 0.1254 0.3941 0.3762 0.074 Uiso 0.5 calc PR 1 B C1B C 0.089(2) 0.519(4) 0.4317(18) 0.061(6) Uiso 0.400(17) d P 2 B H2E H 0.0356 0.5413 0.4326 0.074 Uiso 0.5 calc PR 2 B H2D H 0.1216 0.5997 0.4527 0.074 Uiso 0.5 calc PR 2 B S1B S 0.1101(14) 0.407(2) 0.5418(10) 0.070(6) Uani 0.400(17) d P 2 B C3 C 0.2679(7) 0.4876(19) 0.6001(7) 0.083(5) Uani 1 d . . B H1H H 0.2722 0.3983 0.5759 0.1 Uiso 1 calc R . . H1I H 0.3154 0.5458 0.6032 0.1 Uiso 1 calc R . . S1A S 0.0997(9) 0.4854(19) 0.5340(8) 0.086(4) Uani 0.600(17) d P 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 Pb1 0.0504(4) 0.0232(3) 0.0281(4) -0.0012(3) 0.0113(3) 0.0004(3) Pb2 0.0335(2) 0.0300(3) 0.0314(3) -0.0015(2) 0.00682(19) -0.0002(2) I1 0.0849(6) 0.0437(5) 0.0491(6) 0.0168(4) 0.0134(5) -0.0159(5) I2 0.0715(6) 0.0685(6) 0.0591(7) 0.0015(5) 0.0190(5) 0.0016(5) I3 0.0545(5) 0.0475(5) 0.0481(6) -0.0226(4) 0.0060(4) 0.0117(4) I4 0.0315(4) 0.0672(6) 0.0685(7) -0.0050(5) -0.0006(4) 0.0013(4) I5 0.0526(5) 0.0586(6) 0.0599(6) -0.0304(5) 0.0084(5) 0.0029(5) I6 0.0628(6) 0.0590(6) 0.0617(7) 0.0291(5) 0.0149(5) 0.0004(5) I7 0.0328(4) 0.0674(6) 0.0533(6) -0.0076(5) -0.0002(4) 0.0049(4) I8 0.0922(7) 0.0788(7) 0.0673(7) -0.0239(6) 0.0175(6) -0.0085(6) S2 0.145(4) 0.062(3) 0.087(4) 0.012(2) -0.042(3) -0.006(3) S3 0.070(2) 0.047(2) 0.056(2) 0.0063(18) -0.0134(19) -0.0151(19) S4 0.0419(18) 0.085(3) 0.046(2) 0.004(2) 0.0102(16) -0.0054(19) N2 0.057(8) 0.149(13) 0.063(9) -0.006(9) 0.014(7) 0.005(8) N3 0.065(8) 0.099(10) 0.097(11) 0.026(8) 0.024(8) -0.020(7) N4 0.048(6) 0.076(8) 0.053(7) 0.013(6) -0.004(5) -0.006(6) C8 0.056(9) 0.084(11) 0.048(9) -0.007(8) 0.015(7) -0.010(8) C6 0.056(8) 0.062(9) 0.050(9) 0.012(7) -0.015(7) -0.008(8) C4 0.134(16) 0.075(11) 0.060(13) -0.005(10) 0.001(11) 0.026(11) C5 0.059(8) 0.045(8) 0.038(8) -0.009(6) -0.007(7) -0.011(7) C7 0.046(7) 0.036(7) 0.054(9) 0.003(7) 0.002(7) 0.011(6) S1B 0.058(11) 0.104(15) 0.052(9) -0.009(10) 0.022(8) -0.023(11) C3 0.048(8) 0.137(15) 0.065(11) -0.004(11) 0.011(8) 0.004(9) S1A 0.042(4) 0.131(12) 0.082(7) 0.000(9) 0.007(4) 0.001(8) #------------------ 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 Pb1 I3 3.1636(8) 3_666 ? Pb1 I3 3.1636(8) . ? Pb1 I1 3.1784(8) 3_666 ? Pb1 I1 3.1784(8) . ? Pb1 I2 3.2051(11) 3_666 ? Pb1 I2 3.2051(11) . ? Pb2 I6 3.0867(10) . ? Pb2 I5 3.1147(10) . ? Pb2 I7 3.2129(9) . ? Pb2 I4 3.2246(9) . ? Pb2 I3 3.2938(9) . ? Pb2 I1 3.3024(9) 3_676 ? I1 Pb2 3.3024(9) 3_676 ? I8 I8 2.782(2) 3_667 ? S2 C3 1.777(15) . ? S2 S1A 1.837(18) . ? S2 S1B 2.16(2) . ? S3 C6 1.796(12) . ? S3 S4 2.060(5) . ? S4 C7 1.802(12) . ? N2 C4 1.407(18) . ? N3 C5 1.425(15) . ? N4 C8 1.478(15) . ? C8 C7 1.486(16) . ? C6 C5 1.458(15) . ? C4 C3 1.46(2) . ? C2 C1B 1.46(4) . ? C2 C1A 1.49(3) . ? C2 S1B 1.77(3) . ? C2 S1A 1.89(2) . ? N1A C1A 1.47(4) . ? N1B C1B 1.42(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Pb1 I3 180.00(3) 3_666 . ? I3 Pb1 I1 88.75(3) 3_666 3_666 ? I3 Pb1 I1 91.25(3) . 3_666 ? I3 Pb1 I1 91.25(3) 3_666 . ? I3 Pb1 I1 88.75(3) . . ? I1 Pb1 I1 180 3_666 . ? I3 Pb1 I2 86.80(2) 3_666 3_666 ? I3 Pb1 I2 93.20(2) . 3_666 ? I1 Pb1 I2 91.15(3) 3_666 3_666 ? I1 Pb1 I2 88.85(3) . 3_666 ? I3 Pb1 I2 93.20(2) 3_666 . ? I3 Pb1 I2 86.80(2) . . ? I1 Pb1 I2 88.85(3) 3_666 . ? I1 Pb1 I2 91.15(3) . . ? I2 Pb1 I2 180 3_666 . ? I6 Pb2 I5 91.26(3) . . ? I6 Pb2 I7 89.56(3) . . ? I5 Pb2 I7 95.27(3) . . ? I6 Pb2 I4 87.55(3) . . ? I5 Pb2 I4 93.98(3) . . ? I7 Pb2 I4 170.36(3) . . ? I6 Pb2 I3 95.35(3) . . ? I5 Pb2 I3 173.33(3) . . ? I7 Pb2 I3 85.69(2) . . ? I4 Pb2 I3 85.43(3) . . ? I6 Pb2 I1 175.31(3) . 3_676 ? I5 Pb2 I1 90.33(3) . 3_676 ? I7 Pb2 I1 94.68(3) . 3_676 ? I4 Pb2 I1 87.95(3) . 3_676 ? I3 Pb2 I1 83.01(3) . 3_676 ? Pb1 I1 Pb2 177.30(3) . 3_676 ? Pb1 I3 Pb2 160.58(3) . . ? C3 S2 S1A 112.4(8) . . ? C3 S2 S1B 93.7(8) . . ? S1A S2 S1B 18.8(7) . . ? C6 S3 S4 103.5(5) . . ? C7 S4 S3 103.3(4) . . ? N4 C8 C7 113.3(11) . . ? C5 C6 S3 117.5(9) . . ? N2 C4 C3 114.8(14) . . ? N3 C5 C6 114.1(11) . . ? C8 C7 S4 114.4(9) . . ? C1B C2 C1A 38.7(14) . . ? C1B C2 S1B 106.9(18) . . ? C1A C2 S1B 139.5(16) . . ? C1B C2 S1A 84.3(17) . . ? C1A C2 S1A 118.2(14) . . ? S1B C2 S1A 22.6(7) . . ? N1A C1A C2 110(2) . . ? N1B C1B C2 112(3) . . ? C2 S1B S2 98.8(10) . . ? C4 C3 S2 116.3(11) . . ? S2 S1A C2 106.9(10) . . ? 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 N4 H01A I1 4_676 0.89 2.86 3.671(10) 151.5 N4 H01C S4 . 0.89 2.73 3.183(11) 113.1 N4 H01C I6 2_656 0.89 3.01 3.824(10) 153.3 N3 H01H I4 . 0.89 2.9 3.726(13) 155.1 N3 H01I I3 . 0.89 3.04 3.757(11) 139 N2 H1L I6 . 0.89 2.8 3.570(12) 145.3 N2 H1N I7 2_546 0.89 2.74 3.598(12) 163.4 N2 H1M I5 2_546 0.89 2.94 3.722(11) 147.3 N1A H1C I6 4_575 0.89 2.94 3.42(2) 115.7 N1A H1A I5 4_575 0.89 2.99 3.75(2) 143.4 N1B H2A S3 3_676 0.89 2.67 3.47(3) 149.6 N1B H2C I6 4_575 0.89 3.07 3.91(3) 158.6 data_2 _database_code_depnum_ccdc_archive 'CCDC 625235' _audit_creation_date 2007-01-16T10:44:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C24 H92 I22 N12 O4 Pb5 S12' _chemical_formula_sum 'C24 H92 I22 N12 O4 Pb5 S12' _chemical_formula_weight 4825.5 #------------------ UNIT CELL INFORMATION -----------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' 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 23.232(1) _cell_length_b 8.7714(3) _cell_length_c 25.812(1) _cell_angle_alpha 90 _cell_angle_beta 100.98(1) _cell_angle_gamma 90 _cell_volume 5163.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 14.975 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.0307 _exptl_absorpt_correction_T_max 0.5534 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 83432 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 15029 _reflns_number_gt 6869 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _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 0.000014(5) _refine_ls_number_reflns 15029 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.0933 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.01 _refine_diff_density_max 1.825 _refine_diff_density_min -2.135 #------------------ 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' O O 0.0106 0.006 '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 Pb1 Pb 0 0 0 0.02876(12) Uani 1 d S . . Pb2 Pb -0.161283(15) 0.50471(3) -0.144989(12) 0.03077(9) Uani 1 d . . . Pb3 Pb -0.330447(15) -0.00751(4) -0.272079(13) 0.03375(10) Uani 1 d . . . I1 I -0.08282(3) -0.24518(7) -0.06720(2) 0.0584(2) Uani 1 d . . . I2 I 0.09052(3) -0.07847(7) -0.07551(2) 0.04577(18) Uani 1 d . . . I3 I -0.06135(3) 0.26423(6) -0.07757(2) 0.04094(17) Uani 1 d . . . I4 I -0.10452(3) 0.56343(8) -0.24938(2) 0.05111(19) Uani 1 d . . . I5 I -0.24481(3) 0.76728(7) -0.18834(3) 0.0568(2) Uani 1 d . . . I6 I -0.22879(3) 0.44239(8) -0.05101(2) 0.05050(18) Uani 1 d . . . I7 I -0.24510(3) 0.26942(7) -0.21076(3) 0.0559(2) Uani 1 d . . . I8 I -0.25221(3) -0.06161(7) -0.35622(2) 0.04838(18) Uani 1 d . . . I9 I -0.40525(3) 0.23583(7) -0.34417(2) 0.05058(19) Uani 1 d . . . I10 I -0.40876(3) 0.01406(8) -0.18081(3) 0.0663(2) Uani 1 d . . . I11 I -0.40718(3) -0.26933(7) -0.32470(2) 0.05013(19) Uani 1 d . . . S1 S 0.08100(11) 0.6235(3) 0.80451(9) 0.0477(7) Uani 1 d . . . S2 S 0.03584(10) 0.4585(3) 0.83587(9) 0.0423(6) Uani 1 d . . . S3 S 0.32180(13) 0.4956(3) 0.44402(11) 0.0685(9) Uani 1 d . . . S4 S 0.27914(16) 0.3350(3) 0.47883(11) 0.0853(11) Uani 1 d . . C S5 S 0.45479(12) 0.9544(3) 0.56732(10) 0.0574(8) Uani 1 d . . . S6 S 0.40861(12) 1.1125(3) 0.59974(9) 0.0543(7) Uani 1 d . . . O1 O -0.5117(4) 0.4872(8) -0.4248(3) 0.100(3) Uiso 1 d . . . O2 O 0.4618(4) 0.2984(10) 0.4964(3) 0.129(3) Uiso 1 d . . . C2 C 0.1093(4) 0.5302(11) 0.7524(3) 0.054(3) Uani 1 d . . . H2A H 0.1433 0.5863 0.7462 0.065 Uiso 1 calc R . . H2B H 0.1224 0.4289 0.7643 0.065 Uiso 1 calc R . . N1 N 0.0207(4) 0.4085(9) 0.7016(3) 0.067(3) Uani 1 d . . . H1C H 0.0354 0.3146 0.7054 0.1 Uiso 1 calc R . . H1D H -0.0046 0.4153 0.6711 0.1 Uiso 1 calc R . . H1E H 0.0023 0.429 0.7281 0.1 Uiso 1 calc R . . C1 C 0.0675(6) 0.5164(12) 0.7022(4) 0.079(4) Uani 1 d . . . H1A H 0.0504 0.6159 0.6929 0.095 Uiso 1 calc R . . H1B H 0.0891 0.4875 0.675 0.095 Uiso 1 calc R . . N5 N 0.3930(3) 1.0439(8) 0.4473(3) 0.059(2) Uani 1 d . . . H5C H 0.4167 1.1104 0.4669 0.089 Uiso 1 calc R . . H5D H 0.3679 1.0937 0.4227 0.089 Uiso 1 calc R . . H5E H 0.4141 0.9795 0.432 0.089 Uiso 1 calc R . . N6 N 0.4713(3) 1.1053(9) 0.7178(3) 0.059(2) Uani 1 d . . . H6C H 0.4834 1.153 0.6914 0.089 Uiso 1 calc R . . H6D H 0.5022 1.0751 0.7415 0.089 Uiso 1 calc R . . H6E H 0.4496 1.1687 0.733 0.089 Uiso 1 calc R . . C11 C 0.3862(4) 1.0141(10) 0.6541(4) 0.058(3) Uani 1 d . . . H11A H 0.3592 1.0785 0.6686 0.069 Uiso 1 calc R . . H11B H 0.3654 0.9219 0.6409 0.069 Uiso 1 calc R . . C9 C 0.3603(4) 0.9586(10) 0.4811(4) 0.052(3) Uani 1 d . . . H9A H 0.3309 0.8962 0.4592 0.063 Uiso 1 calc R . . H9B H 0.3402 1.0299 0.5002 0.063 Uiso 1 calc R . . C10 C 0.3991(5) 0.8590(11) 0.5196(4) 0.072(3) Uani 1 d . . . H10A H 0.4184 0.7873 0.5 0.086 Uiso 1 calc R . . H10B H 0.3745 0.8004 0.5388 0.086 Uiso 1 calc R . . C12 C 0.4361(5) 0.9726(10) 0.6973(4) 0.058(3) Uani 1 d . . . H12A H 0.4209 0.9248 0.7258 0.069 Uiso 1 calc R . . H12B H 0.461 0.8991 0.6841 0.069 Uiso 1 calc R . . N2 N 0.0821(3) 0.5163(7) 0.9573(3) 0.051(2) Uani 1 d . . . H2C H 0.0461 0.5168 0.9378 0.077 Uiso 1 calc R . . H2D H 0.0925 0.6112 0.9672 0.077 Uiso 1 calc R . . H2E H 0.0826 0.4588 0.9858 0.077 Uiso 1 calc R . . C3 C 0.0933(4) 0.3615(9) 0.8811(3) 0.037(2) Uani 1 d . . . H3A H 0.0763 0.2736 0.8953 0.044 Uiso 1 calc R . . H3B H 0.1218 0.324 0.8612 0.044 Uiso 1 calc R . . N3 N 0.2621(3) 0.4675(8) 0.3229(3) 0.056(2) Uani 1 d . . . H3C H 0.2682 0.5393 0.3002 0.084 Uiso 1 calc R . . H3D H 0.2416 0.3915 0.3055 0.084 Uiso 1 calc R . . H3E H 0.2965 0.4322 0.34 0.084 Uiso 1 calc R . . C4 C 0.1244(4) 0.4526(10) 0.9255(3) 0.042(2) Uani 1 d . . . H4A H 0.145 0.5356 0.9122 0.051 Uiso 1 calc R . . H4B H 0.1531 0.3894 0.9479 0.051 Uiso 1 calc R . . C6 C 0.2655(4) 0.6062(10) 0.4061(4) 0.061(3) Uani 1 d . . . H6A H 0.24 0.6417 0.4292 0.073 Uiso 1 calc R . . H6B H 0.2834 0.6955 0.3935 0.073 Uiso 1 calc R . . C5 C 0.2295(5) 0.5326(12) 0.3609(4) 0.073(3) Uani 1 d . . . H5A H 0.2017 0.6066 0.3428 0.087 Uiso 1 calc R . . H5B H 0.2071 0.4518 0.3735 0.087 Uiso 1 calc R . . C7 C 0.2819(6) 0.4065(15) 0.5462(4) 0.105(5) Uani 1 d . . . H7A1 H 0.2855 0.3241 0.5717 0.126 Uiso 0.5 calc PR 1 A H7B1 H 0.3137 0.4784 0.5566 0.126 Uiso 0.5 calc PR 1 A H7A2 H 0.2592 0.3346 0.5626 0.126 Uiso 0.5 d PR 2 A H7B2 H 0.3224 0.3927 0.5635 0.126 Uiso 0.5 d PR 2 A N4 N 0.2100(7) 0.5475(11) 0.5780(6) 0.180(7) Uani 1 d . . . H4C1 H 0.2432 0.5759 0.5989 0.27 Uiso 0.5 calc PR 1 B H4D1 H 0.1908 0.4829 0.5952 0.27 Uiso 0.5 calc PR 1 B H4E1 H 0.1878 0.6293 0.5684 0.27 Uiso 0.5 calc PR 1 B H4C2 H 0.182 0.5104 0.5526 0.27 Uiso 0.5 d PR 2 B H4D2 H 0.2026 0.6452 0.5834 0.27 Uiso 0.5 d PR 2 B H4E2 H 0.2106 0.4951 0.6076 0.27 Uiso 0.5 d PR 2 B C8A C 0.2208(11) 0.486(3) 0.5394(8) 0.061(6) Uiso 0.5 d P 1 C H8A1 H 0.2183 0.5618 0.5116 0.073 Uiso 0.5 calc PR 1 C H8B1 H 0.1907 0.4104 0.5276 0.073 Uiso 0.5 calc PR 1 C C8B C 0.2686(12) 0.534(3) 0.5618(10) 0.080(8) Uiso 0.5 d P 2 C H8A2 H 0.2698 0.6077 0.5339 0.096 Uiso 0.5 calc PR 2 C H8B2 H 0.2985 0.5638 0.5917 0.096 Uiso 0.5 calc PR 2 C 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 0.0326(3) 0.0237(2) 0.0280(3) -0.0013(2) 0.0010(2) -0.0009(2) Pb2 0.0312(2) 0.02624(18) 0.03163(19) -0.00173(16) -0.00236(15) -0.00044(17) Pb3 0.0315(2) 0.0320(2) 0.0362(2) -0.00109(16) 0.00258(15) -0.00048(17) I1 0.0706(5) 0.0410(4) 0.0534(4) -0.0075(3) -0.0138(4) -0.0235(4) I2 0.0506(5) 0.0457(4) 0.0453(4) 0.0030(3) 0.0199(3) 0.0039(3) I3 0.0462(4) 0.0389(4) 0.0376(4) 0.0104(3) 0.0079(3) 0.0148(3) I4 0.0400(4) 0.0686(5) 0.0453(4) -0.0018(3) 0.0097(3) 0.0000(4) I5 0.0632(5) 0.0493(4) 0.0541(4) 0.0103(3) 0.0014(4) 0.0278(4) I6 0.0411(4) 0.0674(5) 0.0449(4) -0.0050(3) 0.0130(3) 0.0028(4) I7 0.0651(5) 0.0429(4) 0.0540(4) -0.0121(3) -0.0027(4) -0.0229(4) I8 0.0362(4) 0.0634(4) 0.0474(4) -0.0004(3) 0.0125(3) 0.0010(4) I9 0.0480(4) 0.0473(4) 0.0552(4) 0.0110(3) 0.0069(3) 0.0116(3) I10 0.0614(5) 0.0799(6) 0.0600(5) 0.0130(4) 0.0172(4) 0.0133(4) I11 0.0496(5) 0.0480(4) 0.0520(4) -0.0095(3) 0.0075(3) -0.0205(3) S1 0.064(2) 0.0406(15) 0.0373(14) 0.0038(11) 0.0080(13) -0.0051(13) S2 0.0406(16) 0.0555(16) 0.0304(13) 0.0040(11) 0.0056(11) -0.0010(13) S3 0.056(2) 0.094(2) 0.0544(18) -0.0060(16) 0.0086(15) 0.0103(18) S4 0.145(3) 0.0541(19) 0.063(2) 0.0011(15) 0.034(2) 0.024(2) S5 0.0393(17) 0.076(2) 0.0517(17) -0.0114(14) -0.0028(13) 0.0129(15) S6 0.0531(19) 0.0585(18) 0.0460(16) -0.0041(13) -0.0034(13) 0.0091(14) C2 0.059(8) 0.070(7) 0.037(6) -0.001(5) 0.023(5) -0.022(6) N1 0.078(7) 0.076(7) 0.042(5) -0.012(5) 0.002(5) -0.007(6) C1 0.107(11) 0.079(9) 0.055(8) 0.005(6) 0.027(8) -0.015(8) N5 0.065(6) 0.074(6) 0.039(5) -0.015(4) 0.010(4) -0.027(5) N6 0.047(6) 0.077(7) 0.050(5) 0.005(5) 0.000(4) 0.000(5) C11 0.049(7) 0.066(7) 0.060(7) -0.014(6) 0.014(6) -0.009(6) C9 0.046(7) 0.050(7) 0.056(7) -0.012(5) -0.001(6) -0.007(6) C10 0.084(9) 0.055(7) 0.072(8) -0.018(6) 0.002(7) 0.005(7) C12 0.075(8) 0.055(7) 0.044(6) 0.005(5) 0.016(6) -0.008(6) N2 0.061(6) 0.055(5) 0.039(5) 0.002(4) 0.009(4) -0.001(4) C3 0.031(6) 0.034(5) 0.049(6) 0.008(4) 0.018(5) 0.006(4) N3 0.062(6) 0.064(6) 0.043(5) 0.005(4) 0.012(4) 0.007(5) C4 0.041(6) 0.057(6) 0.030(5) 0.001(5) 0.009(5) 0.015(5) C6 0.072(9) 0.038(6) 0.076(8) 0.000(6) 0.027(7) 0.000(6) C5 0.062(9) 0.086(9) 0.070(8) -0.020(7) 0.011(7) 0.014(7) C7 0.152(15) 0.103(11) 0.070(9) -0.006(8) 0.046(9) 0.004(10) N4 0.232(18) 0.062(8) 0.287(19) 0.032(10) 0.154(15) 0.038(9) #------------------ 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 Pb1 I1 3.1725(6) 3 ? Pb1 I1 3.1725(6) . ? Pb1 I2 3.2028(6) 3 ? Pb1 I2 3.2028(6) . ? Pb1 I3 3.2132(5) 3 ? Pb1 I3 3.2132(5) . ? Pb2 I5 3.0813(7) . ? Pb2 I7 3.1102(7) . ? Pb2 I6 3.1769(7) . ? Pb2 I4 3.2585(7) . ? Pb2 I1 3.2820(7) 1_565 ? Pb2 I3 3.3657(6) . ? Pb3 I11 3.0618(7) . ? Pb3 I8 3.1225(7) . ? Pb3 I9 3.1316(7) . ? Pb3 I10 3.2449(7) . ? Pb3 I5 3.3006(7) 1_545 ? Pb3 I7 3.3379(7) . ? I1 Pb2 3.2821(7) 1_545 ? I5 Pb3 3.3006(7) 1_565 ? S1 C2 1.802(8) . ? S1 S2 2.044(3) . ? S2 C3 1.809(8) . ? S3 C6 1.767(10) . ? S3 S4 2.028(4) . ? S4 C7 1.838(10) . ? S5 C10 1.812(10) . ? S5 S6 2.029(3) . ? S6 C11 1.807(9) . ? C2 C1 1.470(13) . ? N1 C1 1.440(11) . ? N5 C9 1.465(10) . ? N6 C12 1.461(10) . ? C11 C12 1.492(14) . ? C9 C10 1.490(12) . ? N2 C4 1.503(9) . ? C3 C4 1.469(10) . ? N3 C5 1.465(10) . ? C6 C5 1.451(12) . ? C7 C8B 1.25(2) . ? C7 C8A 1.56(2) . ? N4 C8A 1.20(2) . ? N4 C8B 1.50(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 Pb1 I1 180.00(2) 3 . ? I1 Pb1 I2 85.512(18) 3 3 ? I1 Pb1 I2 94.488(18) . 3 ? I1 Pb1 I2 94.488(18) 3 . ? I1 Pb1 I2 85.512(18) . . ? I2 Pb1 I2 180.000(17) 3 . ? I1 Pb1 I3 89.851(16) 3 3 ? I1 Pb1 I3 90.149(16) . 3 ? I2 Pb1 I3 92.324(15) 3 3 ? I2 Pb1 I3 87.676(15) . 3 ? I1 Pb1 I3 90.149(16) 3 . ? I1 Pb1 I3 89.851(16) . . ? I2 Pb1 I3 87.676(15) 3 . ? I2 Pb1 I3 92.323(15) . . ? I3 Pb1 I3 180.00(3) 3 . ? I5 Pb2 I7 90.70(2) . . ? I5 Pb2 I6 92.150(19) . . ? I7 Pb2 I6 87.349(19) . . ? I5 Pb2 I4 84.703(18) . . ? I7 Pb2 I4 87.907(18) . . ? I6 Pb2 I4 174.27(2) . . ? I5 Pb2 I1 87.735(19) . 1_565 ? I7 Pb2 I1 173.95(2) . 1_565 ? I6 Pb2 I1 86.867(18) . 1_565 ? I4 Pb2 I1 97.765(19) . 1_565 ? I5 Pb2 I3 168.76(2) . . ? I7 Pb2 I3 99.484(18) . . ? I6 Pb2 I3 83.664(17) . . ? I4 Pb2 I3 100.290(17) . . ? I1 Pb2 I3 81.642(18) 1_565 . ? I11 Pb3 I8 86.812(18) . . ? I11 Pb3 I9 92.14(2) . . ? I8 Pb3 I9 91.202(18) . . ? I11 Pb3 I10 90.353(19) . . ? I8 Pb3 I10 174.29(2) . . ? I9 Pb3 I10 93.854(19) . . ? I11 Pb3 I5 93.955(19) . 1_545 ? I8 Pb3 I5 90.366(19) . 1_545 ? I9 Pb3 I5 173.78(2) . 1_545 ? I10 Pb3 I5 84.887(18) . 1_545 ? I11 Pb3 I7 177.83(2) . . ? I8 Pb3 I7 93.926(19) . . ? I9 Pb3 I7 89.889(19) . . ? I10 Pb3 I7 88.733(19) . . ? I5 Pb3 I7 84.002(19) 1_545 . ? Pb1 I1 Pb2 174.81(3) . 1_545 ? Pb1 I3 Pb2 162.67(2) . . ? Pb2 I5 Pb3 160.82(2) . 1_565 ? Pb2 I7 Pb3 174.44(3) . . ? C2 S1 S2 105.2(3) . . ? C3 S2 S1 102.5(3) . . ? C6 S3 S4 104.7(4) . . ? C7 S4 S3 104.5(4) . . ? C10 S5 S6 103.3(4) . . ? C11 S6 S5 104.3(3) . . ? C1 C2 S1 115.0(8) . . ? N1 C1 C2 115.7(8) . . ? C12 C11 S6 113.5(7) . . ? N5 C9 C10 112.4(8) . . ? C9 C10 S5 116.4(7) . . ? N6 C12 C11 112.2(8) . . ? C4 C3 S2 116.1(6) . . ? C3 C4 N2 110.7(7) . . ? C5 C6 S3 117.0(7) . . ? C6 C5 N3 114.7(9) . . ? C8B C7 C8A 50.2(14) . . ? C8B C7 S4 130.2(15) . . ? C8A C7 S4 100.4(11) . . ? C8A N4 C8B 52.5(13) . . ? N4 C8A C7 116.0(19) . . ? C7 C8B N4 117(2) . . ? 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 H1C I4 2_545 0.89 2.83 3.682(8) 160.1 N1 H1D I2 2 0.89 2.86 3.752(8) 176.1 N1 H1E S2 . 0.89 2.76 3.443(7) 135.1 N1 H1E I4 1_556 0.89 2.9 3.648(8) 142.1 N5 H5C O2 1_565 0.89 2.02 2.893(11) 165.5 N5 H5D I8 3_565 0.89 2.91 3.650(8) 141 N5 H5E I9 3_565 0.89 2.93 3.672(7) 142.4 N6 H6C S6 . 0.89 2.68 3.118(7) 111.6 N6 H6C I9 1_666 0.89 2.99 3.721(7) 140.1 N6 H6D I10 1_666 0.89 2.65 3.532(7) 172.8 N6 H6E I11 2_565 0.89 2.78 3.550(7) 145 N2 H2C S2 . 0.89 2.65 3.155(7) 117.3 N2 H2D I2 1_566 0.89 2.93 3.668(7) 140.8 N2 H2E I1 3_556 0.89 2.81 3.699(7) 172.8 N3 H3C I7 3_565 0.89 2.82 3.664(7) 158.6 N3 H3D I8 3 0.89 3.17 3.680(7) 118.9 N3 H3E S3 . 0.89 2.7 3.179(8) 115.3 N3 H3E I11 3 0.89 3.03 3.784(7) 143.3 N4 H4E2 I5 2_545 0.89 2.89 3.733(13) 159.3 N4 H4D2 I6 2 0.89 2.84 3.576(10) 141.1 N4 H4D2 I6 2 0.89 2.84 3.576(10) 141.1 N4 H4E2 I5 2_545 0.89 2.89 3.733(13) 159.3 # Attachment 'revised(3)_Mercier.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 625236' _audit_creation_date 2006-06-22T11:36:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C24 H88 I22 N12 O2 Pb5 S12' _chemical_formula_sum 'C24 H88 I22 N12 O2 Pb5 S12' _chemical_formula_weight 4789.58 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 23.25610(10) _cell_length_b 8.77790(10) _cell_length_c 25.57040(10) _cell_angle_alpha 90 _cell_angle_beta 100.3660(10) _cell_angle_gamma 90 _cell_volume 5134.74(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.275 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.045 _exptl_crystal_density_diffrn 3.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 15.057 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.1784 _exptl_absorpt_correction_T_max 0.513 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 353(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 101625 _diffrn_reflns_av_R_equivalents 0.0888 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measured_fraction_theta_full 0.983 _reflns_number_total 14785 _reflns_number_gt 7310 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ 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^)+(0.0241P)^2^+36.4307P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _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 0.000017(5) _refine_ls_number_reflns 14785 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1029 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.5 _refine_diff_density_min -1.28 #------------------ 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' O O 0.0106 0.006 '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 Pb1 Pb 1 0 1 0.03522(12) Uani 1 d S . . Pb2 Pb 0.836922(16) 0.50588(4) 0.856299(13) 0.03826(10) Uani 1 d . . . Pb3 Pb 0.665008(17) -0.00273(4) 0.731196(15) 0.04450(11) Uani 1 d . . . I1 I 1.09110(3) -0.07554(8) 0.92392(3) 0.05410(19) Uani 1 d . . . I2 I 0.93785(3) 0.26415(8) 0.92239(3) 0.05185(19) Uani 1 d . . . I3 I 0.91703(4) 0.75445(8) 0.93327(3) 0.0681(2) Uani 1 d . . . I4 I 0.89436(3) 0.56408(10) 0.75223(3) 0.0645(2) Uani 1 d . . . I5 I 0.75094(4) 0.76302(9) 0.81345(3) 0.0728(3) Uani 1 d . . . I6 I 0.77023(4) 0.44058(10) 0.95221(3) 0.0654(2) Uani 1 d . . . I7 I 0.75463(4) 0.26746(9) 0.79154(3) 0.0708(2) Uani 1 d . . . I8 I 0.74858(3) -0.05916(10) 0.64777(3) 0.0640(2) Uani 1 d . . . I9 I 0.59502(4) 0.24315(9) 0.65736(3) 0.0662(2) Uani 1 d . . . I10 I 0.58604(4) 0.02237(11) 0.82140(3) 0.0800(3) Uani 1 d . . . I11 I 0.58979(4) -0.26305(9) 0.67575(3) 0.0659(2) Uani 1 d . . . N1 N 0.0210(5) 0.4115(14) 0.7009(4) 0.102(4) Uani 1 d . . . H1A H 0.0379 0.3229 0.7113 0.153 Uiso 1 calc R . . H1B H -0.0007 0.4011 0.6687 0.153 Uiso 1 calc R . . H1C H -0.0015 0.4405 0.7238 0.153 Uiso 1 calc R . . C1 C 0.0633(9) 0.5196(18) 0.6992(5) 0.129(7) Uani 1 d . . . H1D H 0.0444 0.6172 0.6907 0.155 Uiso 1 calc R . . H1E H 0.0841 0.494 0.6707 0.155 Uiso 1 calc R . . C2 C 0.1061(5) 0.5355(13) 0.7489(4) 0.072(4) Uani 1 d . . . H2D H 0.1392 0.5932 0.7412 0.087 Uiso 1 calc R . . H2E H 0.1202 0.4348 0.7603 0.087 Uiso 1 calc R . . S1 S 0.07995(14) 0.6269(3) 0.80333(11) 0.0604(8) Uani 1 d . . . S2 S 0.03554(12) 0.4614(3) 0.83539(10) 0.0527(7) Uani 1 d . . . C3 C 0.0925(4) 0.3630(12) 0.8803(4) 0.053(3) Uani 1 d . . . H3A H 0.0752 0.276 0.895 0.063 Uiso 1 calc R . . H3B H 0.1207 0.3243 0.8599 0.063 Uiso 1 calc R . . C4 C 0.1237(5) 0.4547(12) 0.9245(4) 0.059(3) Uani 1 d . . . H4A H 0.1443 0.5369 0.9105 0.071 Uiso 1 calc R . . H4B H 0.1525 0.3915 0.9468 0.071 Uiso 1 calc R . . N2 N 0.0831(4) 0.5193(10) 0.9570(3) 0.067(3) Uani 1 d . . . H2A H 0.0611 0.5908 0.9385 0.101 Uiso 1 calc R . . H2B H 0.1034 0.5602 0.9865 0.101 Uiso 1 calc R . . H2C H 0.0602 0.4457 0.9657 0.101 Uiso 1 calc R . . N3 N 0.7357(4) 0.5353(11) 0.6800(3) 0.077(3) Uani 1 d . . . H3C H 0.7054 0.5873 0.6626 0.115 Uiso 1 calc R . . H3D H 0.7585 0.5973 0.7022 0.115 Uiso 1 calc R . . H3E H 0.7229 0.4603 0.6983 0.115 Uiso 1 calc R . . C5 C 0.7689(6) 0.4716(17) 0.6424(5) 0.094(5) Uani 1 d . . . H5A H 0.7914 0.553 0.6302 0.113 Uiso 1 calc R . . H5B H 0.7964 0.3984 0.661 0.113 Uiso 1 calc R . . C6 C 0.7360(6) 0.3984(15) 0.5970(5) 0.082(4) Uani 1 d . . A H6A H 0.7196 0.3059 0.6089 0.098 Uiso 1 calc R . . H6B H 0.763 0.3681 0.574 0.098 Uiso 1 calc R . . S3 S 0.67948(16) 0.5001(5) 0.55873(13) 0.0878(11) Uani 1 d . . . S4A S 0.7130(13) 0.646(3) 0.5237(9) 0.181(12) Uani 0.5 d P 1 A S4B S 0.7231(8) 0.674(2) 0.5215(5) 0.075(3) Uani 0.5 d P 2 A C7 C 0.7167(8) 0.583(2) 0.4557(5) 0.128(6) Uani 1 d . . . H7A1 H 0.6772 0.6008 0.4369 0.153 Uiso 1 calc R 1 A H7B1 H 0.7401 0.6616 0.4432 0.153 Uiso 1 calc R 1 A H7A2 H 0.6885 0.502 0.4494 0.153 Uiso 1 d R 2 A H7B2 H 0.7085 0.6607 0.428 0.153 Uiso 1 d R 2 A C8A C 0.7328(18) 0.455(3) 0.431(3) 0.23(4) Uani 0.55(4) d P 1 A H8A1 H 0.7265 0.3658 0.4522 0.275 Uiso 0.55(4) calc PR 1 A H8B1 H 0.7085 0.4445 0.3966 0.275 Uiso 0.55(4) calc PR 1 A C8B C 0.7753(14) 0.543(4) 0.4650(11) 0.068(12) Uani 0.45(4) d P 2 A H8A2 H 0.7987 0.6356 0.469 0.081 Uiso 0.45(4) calc PR 2 A H8B2 H 0.7842 0.487 0.4981 0.081 Uiso 0.45(4) calc PR 2 A N4 N 0.7895(8) 0.4602(15) 0.4262(9) 0.204(10) Uani 1 d . . . H4C1 H 0.8 0.3707 0.4145 0.306 Uiso 1 calc R 1 A H4D1 H 0.8116 0.4806 0.4576 0.306 Uiso 1 calc R 1 A H4E1 H 0.7943 0.5328 0.4031 0.306 Uiso 1 calc R 1 A H4C2 H 0.8265 0.4288 0.4325 0.306 Uiso 1 d R 2 A H4D2 H 0.7835 0.5194 0.3975 0.306 Uiso 1 d R 2 A H4E2 H 0.7659 0.3798 0.4208 0.306 Uiso 1 d R 2 A N5 N 0.6135(5) 0.5485(12) 1.0587(4) 0.084(3) Uani 1 d . . . H5C H 0.5813 0.5935 1.0414 0.126 Uiso 1 calc R . . H5D H 0.6387 0.6191 1.0735 0.126 Uiso 1 calc R . . H5E H 0.6042 0.488 1.0838 0.126 Uiso 1 calc R . . C9 C 0.6396(6) 0.4593(16) 1.0219(5) 0.082(4) Uani 1 d . . . H9A H 0.6675 0.3888 1.0418 0.099 Uiso 1 calc R . . H9B H 0.6608 0.5264 1.002 0.099 Uiso 1 calc R . . C10 C 0.5966(7) 0.3739(15) 0.9850(6) 0.106(5) Uani 1 d . . . H10A H 0.5761 0.3069 1.0055 0.127 Uiso 1 calc R . . H10B H 0.6175 0.3099 0.9637 0.127 Uiso 1 calc R . . S5 S 0.54345(16) 0.4809(6) 0.94075(15) 0.1230(18) Uani 1 d . . . S6 S 0.58998(18) 0.6248(5) 0.90497(13) 0.0897(11) Uani 1 d . . . C11 C 0.6083(7) 0.5117(16) 0.8488(6) 0.104(5) Uiso 1 d . . . H11A H 0.6374 0.5697 0.8344 0.125 Uiso 1 calc R . . H11B H 0.6276 0.42 0.8641 0.125 Uiso 1 calc R . . C12 C 0.5628(8) 0.461(2) 0.8014(7) 0.135(6) Uiso 1 d . . . H12A H 0.5813 0.4226 0.773 0.162 Uiso 1 calc R . . H12B H 0.5375 0.3829 0.8116 0.162 Uiso 1 calc R . . N6 N 0.5322(6) 0.5928(17) 0.7865(5) 0.146(5) Uiso 1 d . . . H6C H 0.5216 0.6355 0.8149 0.219 Uiso 1 calc R . . H6D H 0.5005 0.571 0.7626 0.219 Uiso 1 calc R . . H6E H 0.5548 0.6572 0.7724 0.219 Uiso 1 calc R . . O1 O 0.5278(11) 0.874(3) 1.0020(10) 0.362(13) Uiso 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 Pb1 0.0401(3) 0.0290(3) 0.0345(2) -0.0029(2) 0.0013(2) -0.0007(2) Pb2 0.0395(2) 0.03250(19) 0.03918(19) -0.00269(17) -0.00251(16) 0.00012(18) Pb3 0.0409(2) 0.0399(2) 0.0511(2) -0.00068(19) 0.00398(17) -0.0007(2) I1 0.0578(5) 0.0546(4) 0.0545(4) 0.0036(3) 0.0225(4) 0.0051(4) I2 0.0586(5) 0.0486(4) 0.0490(4) 0.0138(3) 0.0115(3) 0.0186(3) I3 0.0835(6) 0.0480(5) 0.0629(5) -0.0095(4) -0.0135(4) -0.0277(4) I4 0.0530(5) 0.0850(6) 0.0560(4) -0.0016(4) 0.0112(4) 0.0008(4) I5 0.0918(7) 0.0621(5) 0.0591(5) 0.0070(4) -0.0007(4) 0.0400(5) I6 0.0576(5) 0.0834(6) 0.0577(4) -0.0076(4) 0.0172(4) 0.0033(4) I7 0.0835(6) 0.0540(5) 0.0683(5) -0.0146(4) -0.0044(4) -0.0297(4) I8 0.0476(5) 0.0842(6) 0.0621(5) -0.0029(4) 0.0151(4) 0.0010(4) I9 0.0648(5) 0.0566(5) 0.0749(5) 0.0144(4) 0.0068(4) 0.0142(4) I10 0.0726(6) 0.1045(7) 0.0672(5) 0.0063(5) 0.0240(4) 0.0173(5) I11 0.0639(5) 0.0576(5) 0.0754(5) -0.0119(4) 0.0102(4) -0.0223(4) N1 0.124(11) 0.116(10) 0.059(7) -0.018(7) -0.004(7) 0.012(9) C1 0.22(2) 0.120(14) 0.052(8) -0.020(8) 0.035(11) -0.090(14) C2 0.088(10) 0.076(9) 0.064(8) -0.003(6) 0.043(7) -0.033(7) S1 0.081(2) 0.0506(17) 0.0497(16) 0.0045(13) 0.0116(15) -0.0055(15) S2 0.0522(17) 0.0657(19) 0.0403(14) 0.0072(12) 0.0083(12) -0.0012(14) C3 0.052(7) 0.060(7) 0.049(6) 0.001(5) 0.016(5) 0.001(6) C4 0.069(8) 0.064(7) 0.044(6) 0.001(5) 0.012(6) 0.005(6) N2 0.100(8) 0.068(6) 0.037(5) 0.004(4) 0.020(5) -0.003(6) N3 0.090(8) 0.090(8) 0.051(6) 0.005(5) 0.016(5) 0.023(6) C5 0.072(10) 0.116(12) 0.088(10) -0.029(9) -0.004(8) 0.022(9) C6 0.094(11) 0.076(9) 0.079(9) 0.006(7) 0.025(8) 0.004(8) S3 0.069(2) 0.127(3) 0.065(2) -0.004(2) 0.0074(17) 0.012(2) S4A 0.37(3) 0.064(10) 0.146(13) 0.024(8) 0.149(15) 0.075(14) S4B 0.128(9) 0.053(7) 0.045(5) 0.003(4) 0.018(5) 0.007(6) C7 0.127(17) 0.19(2) 0.074(10) 0.034(11) 0.026(10) 0.009(14) C8A 0.10(3) 0.052(19) 0.59(10) 0.02(4) 0.20(5) 0.03(2) C8B 0.035(19) 0.09(3) 0.08(2) -0.022(16) 0.009(14) 0.009(17) N4 0.19(2) 0.071(10) 0.39(3) 0.066(15) 0.15(2) 0.033(11) N5 0.080(8) 0.104(8) 0.064(6) 0.000(6) 0.002(6) 0.006(7) C9 0.074(10) 0.105(11) 0.066(8) 0.007(8) 0.006(7) 0.030(8) C10 0.157(16) 0.069(10) 0.094(11) 0.005(8) 0.027(11) -0.029(10) S5 0.055(2) 0.229(5) 0.079(2) 0.046(3) -0.0063(19) -0.031(3) S6 0.094(3) 0.104(3) 0.067(2) 0.006(2) 0.002(2) -0.012(2) #------------------ 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 Pb1 I3 3.1775(7) 1_545 ? Pb1 I3 3.1775(7) 3_767 ? Pb1 I1 3.1931(7) 3_757 ? Pb1 I1 3.1931(7) . ? Pb1 I2 3.2205(6) . ? Pb1 I2 3.2205(6) 3_757 ? Pb2 I5 3.0831(8) . ? Pb2 I7 3.1055(8) . ? Pb2 I6 3.1808(8) . ? Pb2 I4 3.2258(8) . ? Pb2 I3 3.2841(8) . ? Pb2 I2 3.3824(7) . ? Pb3 I11 3.0658(8) . ? Pb3 I9 3.1251(8) . ? Pb3 I8 3.1726(8) . ? Pb3 I10 3.2041(9) . ? Pb3 I5 3.3366(8) 1_545 ? Pb3 I7 3.3455(8) . ? I3 Pb1 3.1775(7) 1_565 ? I5 Pb3 3.3366(8) 1_565 ? N1 C1 1.373(16) . ? C1 C2 1.471(18) . ? C2 S1 1.805(11) . ? S1 S2 2.038(4) . ? S2 C3 1.808(10) . ? C3 C4 1.470(13) . ? C4 N2 1.480(12) . ? N3 C5 1.449(14) . ? C5 C6 1.423(16) . ? C6 S3 1.737(13) . ? S3 S4A 1.82(3) . ? S3 S4B 2.15(2) . ? S4A C7 1.84(2) . ? S4B C7 1.85(2) . ? C7 C8A 1.37(4) . ? C7 C8B 1.38(3) . ? C8A N4 1.35(3) . ? C8B N4 1.32(3) . ? N5 C9 1.438(14) . ? C9 C10 1.454(17) . ? C10 S5 1.785(15) . ? S5 S6 1.990(5) . ? S6 C11 1.857(14) . ? C11 C12 1.52(2) . ? C12 N6 1.375(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Pb1 I3 180 1_545 3_767 ? I3 Pb1 I1 93.59(2) 1_545 3_757 ? I3 Pb1 I1 86.41(2) 3_767 3_757 ? I3 Pb1 I1 86.41(2) 1_545 . ? I3 Pb1 I1 93.59(2) 3_767 . ? I1 Pb1 I1 180.0000(10) 3_757 . ? I3 Pb1 I2 89.748(19) 1_545 . ? I3 Pb1 I2 90.252(19) 3_767 . ? I1 Pb1 I2 87.280(17) 3_757 . ? I1 Pb1 I2 92.720(17) . . ? I3 Pb1 I2 90.252(19) 1_545 3_757 ? I3 Pb1 I2 89.748(19) 3_767 3_757 ? I1 Pb1 I2 92.720(17) 3_757 3_757 ? I1 Pb1 I2 87.280(17) . 3_757 ? I2 Pb1 I2 180 . 3_757 ? I5 Pb2 I7 90.33(3) . . ? I5 Pb2 I6 91.77(2) . . ? I7 Pb2 I6 87.16(2) . . ? I5 Pb2 I4 85.94(2) . . ? I7 Pb2 I4 88.50(2) . . ? I6 Pb2 I4 175.08(2) . . ? I5 Pb2 I3 89.33(2) . . ? I7 Pb2 I3 174.87(2) . . ? I6 Pb2 I3 87.73(2) . . ? I4 Pb2 I3 96.59(2) . . ? I5 Pb2 I2 169.82(2) . . ? I7 Pb2 I2 98.59(2) . . ? I6 Pb2 I2 83.83(2) . . ? I4 Pb2 I2 99.11(2) . . ? I3 Pb2 I2 81.35(2) . . ? I11 Pb3 I9 92.50(2) . . ? I11 Pb3 I8 86.58(2) . . ? I9 Pb3 I8 90.98(2) . . ? I11 Pb3 I10 91.77(2) . . ? I9 Pb3 I10 94.80(2) . . ? I8 Pb3 I10 174.05(3) . . ? I11 Pb3 I5 93.40(2) . 1_545 ? I9 Pb3 I5 173.83(3) . 1_545 ? I8 Pb3 I5 87.58(2) . 1_545 ? I10 Pb3 I5 86.82(2) . 1_545 ? I11 Pb3 I7 176.33(3) . . ? I9 Pb3 I7 90.15(2) . . ? I8 Pb3 I7 90.84(2) . . ? I10 Pb3 I7 90.54(2) . . ? I5 Pb3 I7 83.88(2) 1_545 . ? Pb1 I2 Pb2 162.50(3) . . ? Pb1 I3 Pb2 175.35(3) 1_565 . ? Pb2 I5 Pb3 162.14(3) . 1_565 ? Pb2 I7 Pb3 175.34(3) . . ? N1 C1 C2 114.6(12) . . ? C1 C2 S1 116.0(11) . . ? C2 S1 S2 105.0(4) . . ? C3 S2 S1 103.3(4) . . ? C4 C3 S2 115.6(8) . . ? C3 C4 N2 111.3(9) . . ? C6 C5 N3 116.4(12) . . ? C5 C6 S3 117.9(10) . . ? C6 S3 S4A 107.0(10) . . ? C6 S3 S4B 104.2(7) . . ? S4A S3 S4B 3.4(11) . . ? S3 S4A C7 110.4(14) . . ? C7 S4B S3 97.4(9) . . ? C8A C7 C8B 62(2) . . ? C8A C7 S4A 138(3) . . ? C8B C7 S4A 97.2(17) . . ? C8A C7 S4B 142(3) . . ? C8B C7 S4B 92.1(16) . . ? S4A C7 S4B 10.9(14) . . ? N4 C8A C7 112(4) . . ? N4 C8B C7 112(2) . . ? C8B N4 C8A 64(3) . . ? N5 C9 C10 112.5(12) . . ? C9 C10 S5 117.2(10) . . ? C10 S5 S6 104.7(5) . . ? C11 S6 S5 103.6(5) . . ? C12 C11 S6 123.2(12) . . ? N6 C12 C11 103.0(15) . . ? 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 I4 2_646 0.89 2.83 3.709(12) 172.3 N1 H1B I1 2_656 0.89 2.88 3.743(10) 164.5 N1 H1C S2 . 0.89 2.83 3.422(10) 124.9 N1 H1C I4 1_455 0.89 2.86 3.686(12) 154.2 N2 H2A I1 1_465 0.89 3.05 3.668(9) 128.4 N2 H2B I6 3_667 0.89 3.07 3.782(10) 138.2 N2 H2B I2 3_667 0.89 3.09 3.728(8) 130.5 N2 H2C I3 3_667 0.89 3.09 3.694(8) 126.9 N3 H3C S3 . 0.89 2.72 3.156(10) 111.1 N3 H3C I11 1_565 0.89 3.06 3.812(10) 142.8 N3 H3E I7 . 0.89 2.91 3.661(9) 143.3 N4 H4E2 I6 4_565 0.89 2.92 3.623(13) 136.9 N4 H4D2 I5 4_575 0.89 2.87 3.754(17) 170.6 N4 H4D2 I5 4_575 0.89 2.87 3.754(17) 170.6 N4 H4E2 I6 4_565 0.89 2.92 3.623(13) 136.9 N5 H5C S5 . 0.89 2.75 3.214(10) 113.9 N5 H5D I8 4_566 0.89 2.94 3.535(10) 125.4 N5 H5E I9 4_566 0.89 2.8 3.674(10) 167.2 N6 H6C S6 . 0.89 2.55 3.097(14) 120 N6 H6C I9 2_656 0.89 3.07 3.754(14) 134.7 N6 H6D I10 2_656 0.89 2.7 3.582(14) 171 N6 H6E I11 1_565 0.89 2.83 3.575(14) 142.6 data_4 _database_code_depnum_ccdc_archive 'CCDC 628793' _audit_creation_date 2007-01-15T19:07:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C4 H14 Br4 N2 Pb1 S2' _chemical_formula_sum 'C4 H14 Br4 N2 Pb S2' _chemical_formula_weight 681.12 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 11.4941(5) _cell_length_b 11.6541(5) _cell_length_c 23.092(1) _cell_angle_alpha 90 _cell_angle_beta 91.45(1) _cell_angle_gamma 90 _cell_volume 3092.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.181 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 2.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 21.488 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(Coppens et al. 1970)' _exptl_absorpt_correction_T_min 0.0369 _exptl_absorpt_correction_T_max 0.4679 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type area_detector _diffrn_measurement_method CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 23307 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 4503 _reflns_number_gt 3122 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _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^)+(0.0135P)^2^+23.5112P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _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 0.00028(2) _refine_ls_number_reflns 4503 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.0792 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.653 _refine_diff_density_min -1.798 #------------------ 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' Br Br -0.2901 2.4595 '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 0.24307(2) 0.09421(2) 0.253810(12) 0.02452(10) Uani 1 d . . . Br1 Br 0.5 0.14880(9) 0.25 0.0348(3) Uani 1 d S . . Br2 Br 0.24928(6) 0.07012(7) 0.38759(4) 0.0389(2) Uani 1 d . . . Br3 Br 0 0.01530(10) 0.25 0.0405(3) Uani 1 d S . . Br4 Br 0.25347(7) 0.08876(7) 0.12692(3) 0.0396(2) Uani 1 d . . . Br5 Br 0.31620(7) -0.15180(6) 0.25395(4) 0.0365(2) Uani 1 d . . . S1 S 0.5867(2) 0.3101(2) 0.49273(10) 0.0516(6) Uani 1 d . . . S2 S 0.5228(2) 0.14787(18) 0.49488(9) 0.0461(5) Uani 1 d . . . N1 N 0.5887(5) 0.3335(5) 0.3577(3) 0.0386(16) Uani 1 d . . . H1A H 0.6269 0.3982 0.3656 0.058 Uiso 1 calc R . . H1B H 0.5782 0.3267 0.3195 0.058 Uiso 1 calc R . . H1C H 0.6297 0.274 0.3711 0.058 Uiso 1 calc R . . N2 N 0.4979(6) 0.0751(6) 0.6323(3) 0.0456(17) Uani 1 d . . . H2C H 0.4447 0.0198 0.6336 0.068 Uiso 1 calc R . . H2D H 0.5244 0.0905 0.6681 0.068 Uiso 1 calc R . . H2E H 0.5566 0.0522 0.6108 0.068 Uiso 1 calc R . . C1 C 0.4747(6) 0.3359(7) 0.3854(4) 0.040(2) Uani 1 d . . . H1D H 0.4434 0.2587 0.3865 0.048 Uiso 1 calc R . . H1E H 0.4214 0.3828 0.3623 0.048 Uiso 1 calc R . . C2 C 0.4830(7) 0.3826(7) 0.4452(4) 0.051(2) Uani 1 d . . . H2A H 0.4068 0.3781 0.4621 0.061 Uiso 1 calc R . . H2B H 0.5042 0.463 0.4431 0.061 Uiso 1 calc R . . C3 C 0.4049(7) 0.1608(7) 0.5447(4) 0.046(2) Uani 1 d . . . H3A H 0.355 0.2237 0.5322 0.055 Uiso 1 calc R . . H3B H 0.359 0.0911 0.5431 0.055 Uiso 1 calc R . . C4 C 0.4439(8) 0.1815(7) 0.6062(4) 0.048(2) Uani 1 d . . . H4A H 0.3777 0.2045 0.6287 0.058 Uiso 1 calc R . . H4B H 0.5002 0.2436 0.6075 0.058 Uiso 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 Pb 0.02267(13) 0.02163(14) 0.02924(16) 0.00078(12) 0.00037(10) -0.00049(11) Br1 0.0225(4) 0.0372(6) 0.0444(7) 0 -0.0055(4) 0 Br2 0.0410(4) 0.0363(5) 0.0393(5) -0.0049(4) -0.0005(4) 0.0012(3) Br3 0.0203(4) 0.0504(7) 0.0507(7) 0 -0.0018(5) 0 Br4 0.0443(4) 0.0431(5) 0.0311(4) 0.0002(4) -0.0036(3) -0.0071(4) Br5 0.0451(4) 0.0208(4) 0.0439(5) -0.0011(3) 0.0068(4) -0.0013(3) S1 0.0576(13) 0.0634(15) 0.0338(12) -0.0035(11) -0.0025(10) -0.0154(12) S2 0.0633(14) 0.0413(12) 0.0343(12) 0.0038(10) 0.0100(10) 0.0082(11) N1 0.046(4) 0.035(4) 0.036(4) -0.001(3) 0.003(3) 0.001(3) N2 0.049(4) 0.052(5) 0.036(4) 0.005(3) -0.001(3) 0.005(3) C1 0.030(4) 0.046(5) 0.046(5) 0.014(4) -0.002(4) 0.000(4) C2 0.065(5) 0.042(5) 0.046(5) 0.013(4) 0.021(5) 0.016(4) C3 0.051(5) 0.049(5) 0.038(5) 0.013(4) 0.000(4) 0.008(4) C4 0.062(6) 0.042(5) 0.041(5) 0.002(4) 0.015(4) 0.013(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 Pb Br4 2.9363(8) . ? Pb Br3 2.9405(4) . ? Pb Br5 2.9877(7) . ? Pb Br1 3.0244(3) . ? Pb Br5 3.0417(7) 4 ? Pb Br2 3.1010(9) . ? Br1 Pb 3.0244(3) 2_655 ? Br3 Pb 2.9405(4) 2 ? Br5 Pb 3.0417(7) 4_545 ? S1 C2 1.809(9) . ? S1 S2 2.029(3) . ? S2 C3 1.806(8) . ? N1 C1 1.472(9) . ? N2 C4 1.507(10) . ? C1 C2 1.485(11) . ? C3 C4 1.497(11) . ? 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 Br4 Pb Br3 91.493(16) . . ? Br4 Pb Br5 87.81(2) . . ? Br3 Pb Br5 88.11(3) . . ? Br4 Pb Br1 84.897(16) . . ? Br3 Pb Br1 173.04(3) . . ? Br5 Pb Br1 85.81(2) . . ? Br4 Pb Br5 88.68(2) . 4 ? Br3 Pb Br5 95.24(3) . 4 ? Br5 Pb Br5 175.209(10) . 4 ? Br1 Pb Br5 90.63(3) . 4 ? Br4 Pb Br2 172.60(2) . . ? Br3 Pb Br2 89.964(15) . . ? Br5 Pb Br2 84.99(2) . . ? Br1 Pb Br2 92.875(15) . . ? Br5 Pb Br2 98.41(2) 4 . ? Pb Br1 Pb 155.71(4) . 2_655 ? Pb Br3 Pb 143.55(4) . 2 ? Pb Br5 Pb 150.60(3) . 4_545 ? C2 S1 S2 102.5(3) . . ? C3 S2 S1 102.4(3) . . ? N1 C1 C2 112.0(6) . . ? C1 C2 S1 114.8(6) . . ? C4 C3 S2 114.0(6) . . ? C3 C4 N2 110.9(7) . . ? 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 Br2 3 0.89 2.49 3.381(6) 175.2 N1 H1B Br1 . 0.89 2.76 3.424(6) 132.6 N1 H1B Br3 3 0.89 2.85 3.403(6) 121.4 N1 H1C Br4 2_655 0.89 2.54 3.394(6) 160.5 N2 H2C Br4 6_556 0.89 2.54 3.397(7) 162.6 N2 H2D Br5 5_656 0.89 2.64 3.460(7) 154.6 N2 H2E Br2 5_656 0.89 2.65 3.404(6) 143.5