# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chen-Wei Liu' _publ_contact_author_email chenwei@mail.ndhu.edu.tw loop_ _publ_author_name 'Chen-Wei Liu' 'Wen-Shiang Chang' 'Yu-Min Chang' 'Yi-Feng Lin' B.Sarkar data_1a _database_code_depnum_ccdc_archive 'CCDC 735326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 O4 P2 Pb Se4' _chemical_formula_weight 821.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 P2(1)/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 24.6360(11) _cell_length_b 11.1560(5) _cell_length_c 8.6199(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.0290(10) _cell_angle_gamma 90.00 _cell_volume 2365.78(19) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8467 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.27 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 13.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0521 _exptl_absorpt_correction_T_max 0.2610 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34412 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5881 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0363P)^2^+0.9055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5881 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.225345(6) 0.215347(12) 0.101496(17) 0.03771(6) Uani 1 1 d . . . Se1 Se 0.201954(16) 0.46322(3) 0.16422(5) 0.03995(9) Uani 1 1 d . . . Se2 Se 0.130910(17) 0.28104(3) -0.12342(5) 0.04072(10) Uani 1 1 d . . . Se3 Se 0.309993(16) 0.23510(3) 0.38839(4) 0.03723(9) Uani 1 1 d . . . Se4 Se 0.297847(18) 0.53221(4) 0.55196(5) 0.04650(10) Uani 1 1 d . . . P1 P 0.13264(4) 0.44740(8) 0.00158(11) 0.03315(19) Uani 1 1 d . . . P2 P 0.34128(4) 0.41881(9) 0.40668(11) 0.03430(19) Uani 1 1 d . . . O1 O 0.13062(11) 0.5597(2) -0.1111(3) 0.0429(6) Uani 1 1 d . . . O2 O 0.07667(11) 0.4599(2) 0.0814(3) 0.0425(6) Uani 1 1 d . . . O3 O 0.40396(11) 0.4081(3) 0.4588(3) 0.0455(7) Uani 1 1 d . . . O4 O 0.34502(12) 0.4632(2) 0.2344(3) 0.0416(6) Uani 1 1 d . . . C1 C 0.17210(16) 0.5780(3) -0.2259(5) 0.0416(9) Uani 1 1 d . . . H1A H 0.2005 0.5170 -0.2108 0.050 Uiso 1 1 calc R . . C3 C 0.1443(2) 0.5629(5) -0.3844(5) 0.0611(13) Uani 1 1 d . . . H3A H 0.1302 0.4830 -0.3948 0.092 Uiso 1 1 calc R . . H3B H 0.1700 0.5769 -0.4624 0.092 Uiso 1 1 calc R . . H3C H 0.1150 0.6194 -0.3971 0.092 Uiso 1 1 calc R . . C2 C 0.1963(2) 0.6999(4) -0.1958(7) 0.0645(14) Uani 1 1 d . . . H2A H 0.2133 0.7023 -0.0930 0.097 Uiso 1 1 calc R . . H2B H 0.1682 0.7594 -0.2048 0.097 Uiso 1 1 calc R . . H2C H 0.2230 0.7160 -0.2704 0.097 Uiso 1 1 calc R . . C4 C 0.06495(18) 0.5514(5) 0.1971(5) 0.0554(12) Uani 1 1 d . . . H4A H 0.0982 0.5716 0.2588 0.067 Uiso 1 1 calc R . . C5 C 0.0427(2) 0.6612(5) 0.1160(8) 0.0759(16) Uani 1 1 d . . . H5A H 0.0698 0.6943 0.0525 0.114 Uiso 1 1 calc R . . H5B H 0.0330 0.7194 0.1918 0.114 Uiso 1 1 calc R . . H5C H 0.0111 0.6401 0.0519 0.114 Uiso 1 1 calc R . . C6 C 0.0246(3) 0.4959(6) 0.2989(7) 0.0858(19) Uani 1 1 d . . . H6A H 0.0405 0.4267 0.3496 0.129 Uiso 1 1 calc R . . H6B H -0.0071 0.4724 0.2369 0.129 Uiso 1 1 calc R . . H6C H 0.0146 0.5530 0.3757 0.129 Uiso 1 1 calc R . . C7 C 0.42139(17) 0.3707(5) 0.6158(5) 0.0532(11) Uani 1 1 d . . . H7A H 0.3894 0.3505 0.6734 0.064 Uiso 1 1 calc R . . C9 C 0.4509(2) 0.4732(6) 0.6942(7) 0.0803(17) Uani 1 1 d . . . H9A H 0.4267 0.5402 0.7011 0.120 Uiso 1 1 calc R . . H9B H 0.4813 0.4957 0.6350 0.120 Uiso 1 1 calc R . . H9C H 0.4638 0.4494 0.7967 0.120 Uiso 1 1 calc R . . C8 C 0.4562(3) 0.2611(6) 0.6018(8) 0.0805(17) Uani 1 1 d . . . H8A H 0.4353 0.1985 0.5512 0.121 Uiso 1 1 calc R . . H8B H 0.4689 0.2350 0.7035 0.121 Uiso 1 1 calc R . . H8C H 0.4869 0.2800 0.5418 0.121 Uiso 1 1 calc R . . C10 C 0.34590(19) 0.5901(4) 0.1863(5) 0.0507(10) Uani 1 1 d . . . H10A H 0.3161 0.6324 0.2335 0.061 Uiso 1 1 calc R . . C12 C 0.3357(2) 0.5903(5) 0.0139(6) 0.0692(14) Uani 1 1 d . . . H12A H 0.3015 0.5525 -0.0124 0.104 Uiso 1 1 calc R . . H12B H 0.3642 0.5471 -0.0333 0.104 Uiso 1 1 calc R . . H12C H 0.3350 0.6714 -0.0233 0.104 Uiso 1 1 calc R . . C11 C 0.3981(3) 0.6479(6) 0.2381(8) 0.094(2) Uani 1 1 d . . . H11A H 0.4023 0.6450 0.3494 0.141 Uiso 1 1 calc R . . H11B H 0.3979 0.7299 0.2043 0.141 Uiso 1 1 calc R . . H11C H 0.4276 0.6061 0.1942 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.04198(9) 0.03329(8) 0.03866(9) 0.00316(5) 0.00971(6) 0.00314(5) Se1 0.0390(2) 0.03379(18) 0.0464(2) -0.00342(15) -0.00314(16) -0.00068(15) Se2 0.0427(2) 0.0404(2) 0.0392(2) -0.00784(15) 0.00341(16) -0.00241(15) Se3 0.0418(2) 0.03260(18) 0.03804(19) -0.00068(14) 0.00866(16) 0.00132(15) Se4 0.0500(2) 0.0387(2) 0.0521(2) -0.00884(17) 0.01580(19) -0.00260(17) P1 0.0321(4) 0.0340(4) 0.0339(5) -0.0009(4) 0.0068(4) 0.0021(4) P2 0.0331(5) 0.0364(5) 0.0338(5) 0.0011(4) 0.0052(4) -0.0017(4) O1 0.0443(15) 0.0439(15) 0.0414(14) 0.0097(12) 0.0124(12) 0.0127(12) O2 0.0341(14) 0.0493(15) 0.0448(15) -0.0100(12) 0.0103(11) -0.0007(12) O3 0.0320(14) 0.0638(18) 0.0409(14) 0.0085(13) 0.0043(11) -0.0031(12) O4 0.0503(16) 0.0396(14) 0.0355(13) 0.0052(11) 0.0065(12) -0.0029(12) C1 0.045(2) 0.0372(19) 0.044(2) 0.0070(16) 0.0158(17) 0.0090(16) C3 0.066(3) 0.074(3) 0.043(2) 0.007(2) 0.006(2) 0.022(3) C2 0.078(4) 0.041(2) 0.077(4) 0.005(2) 0.025(3) -0.001(2) C4 0.039(2) 0.077(3) 0.051(3) -0.027(2) 0.0076(19) 0.004(2) C5 0.072(4) 0.054(3) 0.104(5) -0.019(3) 0.025(3) 0.003(3) C6 0.090(4) 0.104(5) 0.067(4) 0.009(3) 0.044(3) 0.024(4) C7 0.038(2) 0.078(3) 0.044(2) 0.014(2) 0.0029(18) -0.005(2) C9 0.072(4) 0.105(5) 0.062(3) -0.014(3) -0.011(3) 0.006(3) C8 0.071(4) 0.082(4) 0.087(4) 0.014(3) -0.014(3) 0.012(3) C10 0.058(3) 0.040(2) 0.056(3) 0.0088(19) 0.011(2) -0.0048(19) C12 0.092(4) 0.061(3) 0.055(3) 0.018(2) 0.009(3) -0.012(3) C11 0.090(4) 0.081(4) 0.108(5) 0.029(4) -0.018(4) -0.040(4) _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 Se1 2.8817(4) . ? Pb1 Se3 2.9040(4) 4_565 ? Pb1 Se2 3.0384(5) . ? Pb1 Se3 3.1572(4) . ? Se1 P1 2.1585(10) . ? Se2 P1 2.1454(10) . ? Se3 P2 2.1924(10) . ? Se3 Pb1 2.9041(4) 4_566 ? Se4 P2 2.1107(10) . ? P1 O2 1.580(3) . ? P1 O1 1.584(3) . ? P2 O4 1.573(3) . ? P2 O3 1.590(3) . ? O1 C1 1.474(5) . ? O2 C4 1.466(5) . ? O3 C7 1.458(5) . ? O4 C10 1.475(5) . ? C1 C2 1.503(6) . ? C1 C3 1.505(6) . ? C4 C6 1.494(7) . ? C4 C5 1.498(8) . ? C7 C9 1.497(8) . ? C7 C8 1.502(8) . ? C10 C11 1.485(7) . ? C10 C12 1.494(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 Se1 Pb1 Se3 95.360(12) . 4_565 ? Se1 Pb1 Se2 74.591(11) . . ? Se3 Pb1 Se2 95.835(12) 4_565 . ? Se1 Pb1 Se3 85.204(11) . . ? Se3 Pb1 Se3 90.889(12) 4_565 . ? Se2 Pb1 Se3 159.189(11) . . ? P1 Se1 Pb1 87.64(3) . . ? P1 Se2 Pb1 83.91(3) . . ? P2 Se3 Pb1 92.18(3) . 4_566 ? P2 Se3 Pb1 109.68(3) . . ? Pb1 Se3 Pb1 92.410(12) 4_566 . ? O2 P1 O1 101.38(15) . . ? O2 P1 Se2 107.49(11) . . ? O1 P1 Se2 112.14(12) . . ? O2 P1 Se1 112.87(11) . . ? O1 P1 Se1 109.38(12) . . ? Se2 P1 Se1 113.02(4) . . ? O4 P2 O3 100.73(15) . . ? O4 P2 Se4 115.35(11) . . ? O3 P2 Se4 113.10(12) . . ? O4 P2 Se3 105.33(11) . . ? O3 P2 Se3 106.43(12) . . ? Se4 P2 Se3 114.56(4) . . ? C1 O1 P1 121.4(2) . . ? C4 O2 P1 124.4(3) . . ? C7 O3 P2 121.2(2) . . ? C10 O4 P2 124.7(3) . . ? O1 C1 C2 107.0(3) . . ? O1 C1 C3 107.2(3) . . ? C2 C1 C3 114.5(4) . . ? O2 C4 C6 105.8(4) . . ? O2 C4 C5 109.4(4) . . ? C6 C4 C5 112.0(4) . . ? O3 C7 C9 108.2(4) . . ? O3 C7 C8 107.5(4) . . ? C9 C7 C8 113.0(4) . . ? O4 C10 C11 110.9(4) . . ? O4 C10 C12 106.1(4) . . ? C11 C10 C12 113.3(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.095 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.132 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 735327' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H70 O8 P4 Pb2 Se8' _chemical_formula_weight 1728.80 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5929(4) _cell_length_b 10.7784(5) _cell_length_c 13.7982(6) _cell_angle_alpha 81.0330(10) _cell_angle_beta 83.8620(10) _cell_angle_gamma 82.9420(10) _cell_volume 1392.95(11) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4620 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.29 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 11.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3767 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10769 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6715 _reflns_number_gt 5624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0341P)^2^+0.0444P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6715 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.247393(14) 1.032384(13) -0.013421(11) 0.03191(5) Uani 1 1 d . . . Se1 Se 0.09452(4) 1.27769(4) -0.00436(3) 0.03943(10) Uani 1 1 d . . . Se2 Se 0.37283(5) 1.19353(4) -0.17881(3) 0.04205(11) Uani 1 1 d . . . Se3 Se 0.02502(4) 0.99441(3) -0.15343(3) 0.03271(9) Uani 1 1 d . . . Se4 Se 0.45727(4) 1.12088(4) 0.11257(3) 0.03503(9) Uani 1 1 d . . . P1 P 0.04386(10) 0.79310(9) -0.12060(7) 0.0295(2) Uani 1 1 d . . . P2 P 0.47398(10) 0.95683(10) 0.22134(7) 0.0312(2) Uani 1 1 d . . . O1 O 0.0255(3) 0.7291(3) -0.2142(2) 0.0382(6) Uani 1 1 d . . . O2 O 0.2026(3) 0.7460(2) -0.1043(2) 0.0373(6) Uani 1 1 d . . . O3 O 0.3230(3) 0.9108(3) 0.2466(2) 0.0399(6) Uani 1 1 d . . . O4 O 0.5041(3) 0.9906(3) 0.32498(19) 0.0378(6) Uani 1 1 d . . . C1 C -0.1087(5) 0.7450(5) -0.2584(4) 0.0515(12) Uani 1 1 d . . . H1A H -0.1764 0.8055 -0.2253 0.062 Uiso 1 1 calc R . . C2 C -0.0804(8) 0.7978(7) -0.3647(5) 0.091(2) Uani 1 1 d . . . H2A H -0.1676 0.8101 -0.3964 0.136 Uiso 1 1 calc R . . H2B H -0.0127 0.7394 -0.3970 0.136 Uiso 1 1 calc R . . H2C H -0.0425 0.8782 -0.3697 0.136 Uiso 1 1 calc R . . C3 C -0.1650(8) 0.6218(7) -0.2450(5) 0.106(3) Uani 1 1 d . . . H3A H -0.2540 0.6313 -0.2743 0.159 Uiso 1 1 calc R . . H3B H -0.1798 0.5907 -0.1753 0.159 Uiso 1 1 calc R . . H3C H -0.0984 0.5621 -0.2768 0.159 Uiso 1 1 calc R . . C4 C 0.2484(4) 0.6098(4) -0.0778(4) 0.0458(11) Uani 1 1 d . . . H4A H 0.1652 0.5618 -0.0687 0.055 Uiso 1 1 calc R . . C5 C 0.3465(6) 0.5692(5) -0.1614(4) 0.0681(16) Uani 1 1 d . . . H5A H 0.2964 0.5798 -0.2200 0.102 Uiso 1 1 calc R . . H5B H 0.3822 0.4810 -0.1449 0.102 Uiso 1 1 calc R . . H5C H 0.4247 0.6204 -0.1735 0.102 Uiso 1 1 calc R . . C6 C 0.3131(6) 0.5953(6) 0.0168(4) 0.0715(16) Uani 1 1 d . . . H6A H 0.2430 0.6225 0.0675 0.107 Uiso 1 1 calc R . . H6B H 0.3909 0.6466 0.0092 0.107 Uiso 1 1 calc R . . H6C H 0.3477 0.5073 0.0357 0.107 Uiso 1 1 calc R . . C7 C 0.2984(5) 0.7987(4) 0.3197(4) 0.0467(11) Uani 1 1 d . . . H7A H 0.3861 0.7655 0.3512 0.056 Uiso 1 1 calc R . . C8 C 0.1854(6) 0.8404(6) 0.3955(4) 0.0683(15) Uani 1 1 d . . . H8A H 0.2190 0.9022 0.4289 0.103 Uiso 1 1 calc R . . H8B H 0.1623 0.7680 0.4430 0.103 Uiso 1 1 calc R . . H8C H 0.1020 0.8779 0.3634 0.103 Uiso 1 1 calc R . . C9 C 0.2546(7) 0.7016(6) 0.2656(5) 0.0830(19) Uani 1 1 d . . . H9A H 0.3311 0.6771 0.2181 0.125 Uiso 1 1 calc R . . H9B H 0.1721 0.7368 0.2315 0.125 Uiso 1 1 calc R . . H9C H 0.2322 0.6280 0.3122 0.125 Uiso 1 1 calc R . . C10 C 0.6343(4) 1.0443(4) 0.3349(3) 0.0415(10) Uani 1 1 d . . . H10A H 0.6854 1.0621 0.2689 0.050 Uiso 1 1 calc R . . C11 C 0.5915(6) 1.1667(5) 0.3748(4) 0.0656(15) Uani 1 1 d . . . H11A H 0.5336 1.2232 0.3297 0.098 Uiso 1 1 calc R . . H11B H 0.6752 1.2054 0.3822 0.098 Uiso 1 1 calc R . . H11C H 0.5382 1.1505 0.4385 0.098 Uiso 1 1 calc R . . C12 C 0.7252(6) 0.9496(5) 0.3990(4) 0.0645(15) Uani 1 1 d . . . H12A H 0.7468 0.8726 0.3695 0.097 Uiso 1 1 calc R . . H12B H 0.6755 0.9309 0.4637 0.097 Uiso 1 1 calc R . . H12C H 0.8121 0.9839 0.4052 0.097 Uiso 1 1 calc R . . C21 C 0.5835(11) 0.4976(9) 0.4634(8) 0.169(6) Uani 1 1 d . . . H21A H 0.6334 0.4130 0.4792 0.203 Uiso 1 1 calc R . . H21B H 0.5647 0.5079 0.3941 0.203 Uiso 1 1 calc R . . C22 C 0.6735(14) 0.5841(10) 0.4727(9) 0.177(5) Uani 1 1 d . . . H22A H 0.6812 0.5835 0.5430 0.212 Uiso 1 1 calc R . . H22B H 0.6306 0.6682 0.4465 0.212 Uiso 1 1 calc R . . C23 C 0.8293(13) 0.5637(11) 0.4194(9) 0.205(7) Uani 1 1 d . . . H23A H 0.8837 0.6289 0.4315 0.307 Uiso 1 1 calc R . . H23B H 0.8242 0.5683 0.3491 0.307 Uiso 1 1 calc R . . H23C H 0.8744 0.4814 0.4453 0.307 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02653(8) 0.03645(8) 0.03349(8) -0.00705(6) -0.00252(6) -0.00396(5) Se1 0.0396(2) 0.0342(2) 0.0422(2) -0.00505(17) 0.00717(19) -0.00507(17) Se2 0.0441(2) 0.0386(2) 0.0396(2) -0.00301(17) 0.00496(19) 0.00015(18) Se3 0.03073(19) 0.03285(18) 0.0355(2) -0.00457(15) -0.00583(16) -0.00498(15) Se4 0.0322(2) 0.0385(2) 0.0356(2) -0.00508(16) -0.00723(17) -0.00496(16) P1 0.0256(5) 0.0319(5) 0.0330(5) -0.0093(4) -0.0026(4) -0.0048(4) P2 0.0268(5) 0.0407(5) 0.0276(5) -0.0063(4) -0.0029(4) -0.0070(4) O1 0.0298(14) 0.0459(16) 0.0437(17) -0.0201(13) -0.0046(12) -0.0042(12) O2 0.0253(13) 0.0352(14) 0.0525(18) -0.0074(12) -0.0074(13) -0.0027(11) O3 0.0298(14) 0.0504(17) 0.0410(16) -0.0039(13) -0.0051(12) -0.0119(12) O4 0.0339(14) 0.0571(17) 0.0254(14) -0.0098(12) -0.0021(12) -0.0126(13) C1 0.033(2) 0.076(3) 0.056(3) -0.039(3) -0.012(2) -0.005(2) C2 0.120(6) 0.093(5) 0.069(4) 0.001(3) -0.048(4) -0.030(4) C3 0.129(6) 0.121(6) 0.087(5) -0.013(4) -0.014(5) -0.089(5) C4 0.034(2) 0.035(2) 0.066(3) 0.001(2) -0.006(2) -0.0022(17) C5 0.073(4) 0.048(3) 0.080(4) -0.020(3) 0.001(3) 0.012(3) C6 0.060(3) 0.079(4) 0.065(4) 0.015(3) -0.012(3) 0.006(3) C7 0.039(2) 0.050(2) 0.053(3) -0.003(2) -0.002(2) -0.018(2) C8 0.063(3) 0.091(4) 0.050(3) -0.006(3) 0.007(3) -0.017(3) C9 0.099(5) 0.065(4) 0.095(5) -0.025(3) -0.001(4) -0.039(3) C10 0.033(2) 0.061(3) 0.034(2) -0.0094(19) -0.0012(18) -0.0162(19) C11 0.076(4) 0.068(3) 0.062(3) -0.021(3) -0.016(3) -0.020(3) C12 0.053(3) 0.082(4) 0.063(3) -0.013(3) -0.026(3) -0.006(3) C21 0.257(15) 0.082(6) 0.182(12) -0.060(7) -0.121(11) 0.065(8) C22 0.262(15) 0.084(7) 0.191(13) -0.012(7) -0.060(12) -0.023(9) C23 0.272(17) 0.112(8) 0.191(13) -0.016(8) 0.052(12) 0.061(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Se1 2.8754(4) . ? Pb1 Se2 2.8920(5) . ? Pb1 Se4 3.1182(4) . ? Pb1 Se3 3.1293(4) . ? Se1 P1 2.1602(11) 2_575 ? Se2 P2 2.1581(11) 2_675 ? Se3 P1 2.1356(10) . ? Se4 P2 2.1353(11) . ? P1 O2 1.573(3) . ? P1 O1 1.590(3) . ? P1 Se1 2.1602(11) 2_575 ? P2 O3 1.574(3) . ? P2 O4 1.593(3) . ? P2 Se2 2.1581(10) 2_675 ? O1 C1 1.464(5) . ? O2 C4 1.480(5) . ? O3 C7 1.474(5) . ? O4 C10 1.466(5) . ? C1 C3 1.473(8) . ? C1 C2 1.498(8) . ? C4 C6 1.483(7) . ? C4 C5 1.494(7) . ? C7 C9 1.500(7) . ? C7 C8 1.501(7) . ? C10 C12 1.500(7) . ? C10 C11 1.503(7) . ? C21 C22 1.374(15) . ? C21 C21 1.80(2) 2_666 ? C22 C23 1.599(16) . ? 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 Se1 Pb1 Se2 75.461(12) . . ? Se1 Pb1 Se4 85.148(12) . . ? Se2 Pb1 Se4 86.524(13) . . ? Se1 Pb1 Se3 85.821(12) . . ? Se2 Pb1 Se3 86.772(13) . . ? Se4 Pb1 Se3 169.868(11) . . ? P1 Se1 Pb1 92.39(3) 2_575 . ? P2 Se2 Pb1 93.21(3) 2_675 . ? P1 Se3 Pb1 95.76(3) . . ? P2 Se4 Pb1 97.97(3) . . ? O2 P1 O1 100.64(15) . . ? O2 P1 Se3 107.82(11) . . ? O1 P1 Se3 111.88(12) . . ? O2 P1 Se1 111.06(12) . 2_575 ? O1 P1 Se1 110.77(12) . 2_575 ? Se3 P1 Se1 113.85(4) . 2_575 ? O3 P2 O4 101.12(15) . . ? O3 P2 Se4 107.93(12) . . ? O4 P2 Se4 111.65(12) . . ? O3 P2 Se2 111.19(12) . 2_675 ? O4 P2 Se2 110.15(11) . 2_675 ? Se4 P2 Se2 114.05(5) . 2_675 ? C1 O1 P1 121.7(2) . . ? C4 O2 P1 120.6(2) . . ? C7 O3 P2 121.5(3) . . ? C10 O4 P2 120.2(2) . . ? O1 C1 C3 108.9(5) . . ? O1 C1 C2 107.2(4) . . ? C3 C1 C2 112.5(5) . . ? O2 C4 C6 106.9(4) . . ? O2 C4 C5 107.4(4) . . ? C6 C4 C5 114.3(4) . . ? O3 C7 C9 107.2(4) . . ? O3 C7 C8 107.0(4) . . ? C9 C7 C8 112.5(4) . . ? O4 C10 C12 108.9(4) . . ? O4 C10 C11 107.0(4) . . ? C12 C10 C11 114.0(4) . . ? C22 C21 C21 118.1(10) . 2_666 ? C21 C22 C23 116.5(11) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.541 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.120