# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Jiang-Gao Mao' 'A. Clearfield' 'Zhong-Ming Sun' 'Yan-Qiong Sun' 'Hui-Yi Zeng' _publ_contact_author_name 'Prof Jiang-Gao Mao' _publ_contact_author_address ; Prof Jiang-Gao Mao State Key Laboratory of Structure Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Science Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email MJG@MS.FJIRSM.AC.CN _publ_section_title ; Hydrothermal synthesis, characterization and crystal structures of two new layered lead(II) materials ; #For complex 1 data_1 _database_code_CSD 214482 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H54 N4 O26 P8 Pb5' _chemical_formula_weight 2242.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M Pbca #(No. 61) 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 13.0056(2) _cell_length_b 13.75480(10) _cell_length_c 30.0991(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5384.41(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 15.909 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method 'narrow frame method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 17434 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.11 _reflns_number_total 4790 _reflns_number_gt 3646 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+69.5536P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4790 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 0.22013(3) -0.04358(3) 0.468839(18) 0.02031(17) Uani 1 1 d . . . Pb2 Pb 0.5000 0.0000 0.5000 0.01994(19) Uani 1 2 d S . . Pb3 Pb -0.05141(4) -0.20685(3) 0.500126(18) 0.02085(17) Uani 1 1 d . . . P1 P 0.0403(2) -0.0106(2) 0.56082(12) 0.0166(7) Uani 1 1 d . . . P2 P 0.3605(2) -0.1294(2) 0.59141(13) 0.0212(8) Uani 1 1 d . . . P3 P 0.1940(2) -0.2925(2) 0.46357(12) 0.0170(7) Uani 1 1 d . . . P4 P 0.4315(2) -0.1333(3) 0.39964(12) 0.0207(8) Uani 1 1 d . . . N1 N 0.2056(8) -0.0030(7) 0.6185(4) 0.021(2) Uani 1 1 d . . . H11A H 0.2330 0.0267 0.5943 0.025 Uiso 1 1 calc R . . N2 N 0.2277(7) -0.1778(8) 0.3907(4) 0.019(2) Uani 1 1 d . . . C1 C 0.2237(10) 0.0009(10) 0.7037(5) 0.023(3) Uani 1 1 d . . . C2 C 0.2954(12) -0.0504(10) 0.7269(6) 0.037(4) Uani 1 1 d . . . H2A H 0.3588 -0.0628 0.7137 0.044 Uiso 1 1 calc R . . C3 C 0.2772(14) -0.0847(11) 0.7693(6) 0.044(4) Uani 1 1 d . . . H3A H 0.3273 -0.1202 0.7842 0.052 Uiso 1 1 calc R . . C4 C 0.1859(15) -0.0662(11) 0.7888(5) 0.044(4) Uani 1 1 d . . . H4A H 0.1730 -0.0900 0.8172 0.052 Uiso 1 1 calc R . . C5 C 0.1119(13) -0.0129(12) 0.7674(5) 0.040(4) Uani 1 1 d . . . H5A H 0.0508 0.0023 0.7818 0.048 Uiso 1 1 calc R . . C6 C 0.1282(12) 0.0180(11) 0.7247(5) 0.037(4) Uani 1 1 d . . . H6A H 0.0763 0.0504 0.7095 0.045 Uiso 1 1 calc R . . C7 C 0.2498(9) 0.0459(10) 0.6588(5) 0.023(3) Uani 1 1 d . . . H7A H 0.2265 0.1129 0.6590 0.027 Uiso 1 1 calc R . . H7B H 0.3240 0.0470 0.6558 0.027 Uiso 1 1 calc R . . C8 C 0.0920(9) 0.0124(10) 0.6169(5) 0.025(3) Uani 1 1 d . . . H8A H 0.0765 0.0788 0.6255 0.030 Uiso 1 1 calc R . . H8B H 0.0589 -0.0308 0.6379 0.030 Uiso 1 1 calc R . . C9 C 0.2333(9) -0.1082(9) 0.6159(5) 0.020(3) Uani 1 1 d . . . H9A H 0.1820 -0.1418 0.5983 0.024 Uiso 1 1 calc R . . H9B H 0.2319 -0.1356 0.6456 0.024 Uiso 1 1 calc R . . C11 C 0.1364(11) -0.1722(9) 0.3153(5) 0.026(3) Uani 1 1 d . . . C12 C 0.0377(10) -0.2129(10) 0.3163(5) 0.028(3) Uani 1 1 d . . . H12A H 0.0013 -0.2147 0.3428 0.034 Uiso 1 1 calc R . . C13 C -0.0055(14) -0.2498(12) 0.2786(7) 0.049(5) Uani 1 1 d . . . H13A H -0.0713 -0.2762 0.2797 0.058 Uiso 1 1 calc R . . C14 C 0.0471(17) -0.2483(12) 0.2394(6) 0.056(5) Uani 1 1 d . . . H14A H 0.0158 -0.2724 0.2139 0.067 Uiso 1 1 calc R . . C15 C 0.1442(18) -0.2123(11) 0.2368(6) 0.062(6) Uani 1 1 d . . . H15A H 0.1803 -0.2133 0.2102 0.074 Uiso 1 1 calc R . . C16 C 0.1885(13) -0.1734(11) 0.2757(5) 0.038(4) Uani 1 1 d . . . H16A H 0.2547 -0.1480 0.2744 0.046 Uiso 1 1 calc R . . C17 C 0.1780(10) -0.1197(9) 0.3564(5) 0.026(3) Uani 1 1 d . . . H17A H 0.2270 -0.0713 0.3465 0.031 Uiso 1 1 calc R . . H17B H 0.1213 -0.0852 0.3701 0.031 Uiso 1 1 calc R . . C18 C 0.1619(8) -0.2570(8) 0.4066(4) 0.017(3) Uani 1 1 d . . . H18A H 0.1696 -0.3127 0.3872 0.020 Uiso 1 1 calc R . . H18B H 0.0906 -0.2364 0.4054 0.020 Uiso 1 1 calc R . . C19 C 0.3313(10) -0.2119(10) 0.3767(5) 0.025(3) Uani 1 1 d . . . H19A H 0.3356 -0.2117 0.3445 0.030 Uiso 1 1 calc R . . H19B H 0.3418 -0.2781 0.3869 0.030 Uiso 1 1 calc R . . O11 O -0.0529(6) 0.0561(7) 0.5576(3) 0.028(2) Uani 1 1 d . . . O12 O 0.0166(7) -0.1178(6) 0.5577(3) 0.024(2) Uani 1 1 d . . . O13 O 0.1253(6) 0.0249(6) 0.5307(3) 0.0205(19) Uani 1 1 d . . . O21 O 0.3654(6) -0.0690(7) 0.5500(3) 0.028(2) Uani 1 1 d . . . O22 O 0.3659(7) -0.2377(7) 0.5868(4) 0.036(3) Uani 1 1 d . . . O23 O 0.4381(7) -0.0933(7) 0.6272(3) 0.032(2) Uani 1 1 d . . . H23A H 0.4786 -0.0550 0.6159 0.048 Uiso 1 1 calc R . . O31 O 0.1904(8) -0.2005(7) 0.4925(3) 0.032(2) Uani 1 1 d . . . O32 O 0.3000(6) -0.3392(6) 0.4629(3) 0.027(2) Uani 1 1 d . . . O33 O 0.1138(7) -0.3639(6) 0.4799(4) 0.032(2) Uani 1 1 d . . . O41 O 0.4378(7) -0.1468(7) 0.4505(3) 0.026(2) Uani 1 1 d . . . O42 O 0.4161(7) -0.0282(7) 0.3873(4) 0.035(3) Uani 1 1 d . . . O43 O 0.5297(6) -0.1781(8) 0.3771(3) 0.031(2) Uani 1 1 d . . . H43A H 0.5800 -0.1683 0.3929 0.047 Uiso 1 1 calc R . . O1W O 0.1983(6) -0.3491(8) 0.5742(3) 0.031(2) Uani 1 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 0.0169(2) 0.0187(3) 0.0253(3) -0.0004(2) 0.0009(2) -0.00073(19) Pb2 0.0167(3) 0.0196(3) 0.0235(4) 0.0027(3) 0.0009(3) 0.0012(3) Pb3 0.0234(3) 0.0207(3) 0.0184(3) -0.0011(2) -0.0005(2) -0.00132(19) P1 0.0155(14) 0.0215(16) 0.0128(17) 0.0026(14) -0.0014(13) -0.0026(12) P2 0.0154(15) 0.0242(17) 0.024(2) -0.0037(16) 0.0023(14) 0.0009(13) P3 0.0129(15) 0.0175(15) 0.021(2) 0.0042(15) 0.0016(13) -0.0005(12) P4 0.0159(15) 0.0264(18) 0.020(2) 0.0016(16) 0.0004(14) -0.0053(13) N1 0.025(5) 0.021(5) 0.015(6) 0.009(5) -0.002(5) -0.005(4) N2 0.015(5) 0.028(6) 0.016(6) 0.005(5) 0.002(4) -0.001(4) C1 0.027(7) 0.027(7) 0.015(7) 0.000(6) 0.005(6) 0.001(6) C2 0.043(9) 0.030(8) 0.038(10) -0.006(8) -0.013(7) 0.008(7) C3 0.069(12) 0.031(8) 0.031(10) 0.015(8) -0.011(9) 0.004(8) C4 0.080(13) 0.038(9) 0.012(9) 0.007(7) -0.003(8) -0.021(9) C5 0.052(10) 0.056(10) 0.013(8) 0.002(8) 0.003(7) -0.023(8) C6 0.036(8) 0.043(9) 0.032(10) -0.016(8) -0.003(7) -0.007(7) C7 0.020(6) 0.025(7) 0.024(8) -0.005(6) -0.008(6) 0.000(5) C8 0.013(6) 0.032(7) 0.031(9) 0.002(7) -0.002(6) 0.000(5) C9 0.020(6) 0.024(7) 0.016(7) 0.000(6) 0.007(5) 0.001(5) C11 0.040(8) 0.017(6) 0.020(8) 0.005(6) -0.007(6) 0.012(6) C12 0.029(7) 0.029(8) 0.026(9) 0.003(7) -0.006(6) 0.013(6) C13 0.050(10) 0.032(8) 0.063(14) -0.003(9) -0.027(10) -0.002(8) C14 0.097(16) 0.036(10) 0.034(12) 0.007(9) -0.025(10) -0.018(10) C15 0.126(19) 0.030(9) 0.031(11) -0.001(8) -0.003(12) -0.025(11) C16 0.065(11) 0.034(8) 0.016(9) 0.008(7) 0.004(7) -0.017(8) C17 0.026(7) 0.018(6) 0.034(9) -0.002(6) 0.000(6) -0.005(6) C18 0.012(5) 0.014(6) 0.023(8) 0.004(6) 0.002(5) -0.004(5) C19 0.032(7) 0.025(7) 0.019(8) -0.006(6) 0.004(6) -0.001(6) O11 0.015(4) 0.034(5) 0.034(6) -0.006(5) -0.005(4) -0.001(4) O12 0.029(5) 0.020(5) 0.023(6) 0.004(4) -0.005(4) -0.002(4) O13 0.024(4) 0.028(5) 0.010(5) -0.009(4) 0.004(4) -0.008(4) O21 0.023(5) 0.047(6) 0.014(5) 0.010(5) 0.000(4) 0.003(4) O22 0.026(5) 0.026(5) 0.056(8) -0.003(5) -0.001(5) -0.001(4) O23 0.024(5) 0.038(6) 0.033(6) 0.001(5) 0.001(4) -0.008(4) O31 0.044(6) 0.023(5) 0.030(7) 0.005(5) 0.002(5) -0.004(4) O32 0.019(5) 0.020(4) 0.042(7) 0.007(5) -0.008(4) 0.007(4) O33 0.028(5) 0.022(5) 0.047(7) 0.011(5) 0.008(5) -0.007(4) O41 0.031(5) 0.036(6) 0.012(5) 0.000(4) -0.003(4) -0.009(4) O42 0.031(5) 0.030(5) 0.045(7) 0.009(5) -0.009(5) -0.010(4) O43 0.015(4) 0.055(6) 0.023(6) -0.011(5) 0.005(4) 0.002(4) O1W 0.017(5) 0.060(7) 0.016(6) 0.022(5) -0.001(4) -0.006(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 O31 2.305(9) . ? Pb1 O11 2.322(8) 5_556 ? Pb1 O13 2.423(8) . ? Pb2 O33 2.462(9) 8_665 ? Pb2 O33 2.462(9) 4_546 ? Pb2 O21 2.495(9) 5_656 ? Pb2 O21 2.495(9) . ? Pb2 O41 2.636(9) 5_656 ? Pb2 O41 2.636(9) . ? Pb3 O12 2.300(9) . ? Pb3 O32 2.319(9) 4_446 ? Pb3 O41 2.507(9) 4_446 ? P1 O12 1.509(9) . ? P1 O13 1.512(9) . ? P1 O11 1.523(9) . ? P1 C8 1.844(15) . ? P2 O22 1.497(10) . ? P2 O21 1.501(10) . ? P2 O23 1.557(10) . ? P2 C9 1.835(12) . ? P3 O33 1.514(9) . ? P3 O32 1.521(8) . ? P3 O31 1.537(10) . ? P3 C18 1.831(13) . ? P4 O42 1.505(10) . ? P4 O41 1.544(10) . ? P4 O43 1.573(9) . ? P4 C19 1.829(13) . ? N1 C8 1.493(15) . ? N1 C9 1.493(16) . ? N1 C7 1.501(17) . ? N2 C17 1.456(17) . ? N2 C18 1.465(15) . ? N2 C19 1.487(16) . ? C1 C2 1.36(2) . ? C1 C6 1.414(19) . ? C1 C7 1.523(19) . ? C2 C3 1.38(2) . ? C3 C4 1.35(2) . ? C4 C5 1.37(2) . ? C5 C6 1.37(2) . ? C11 C16 1.37(2) . ? C11 C12 1.400(19) . ? C11 C17 1.533(19) . ? C12 C13 1.36(2) . ? C13 C14 1.37(3) . ? C14 C15 1.36(3) . ? C15 C16 1.41(2) . ? O11 Pb1 2.322(8) 5_556 ? O32 Pb3 2.319(9) 4_546 ? O33 Pb2 2.462(9) 4_446 ? O41 Pb3 2.507(9) 4_546 ? 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 O31 Pb1 O11 83.1(4) . 5_556 ? O31 Pb1 O13 92.4(3) . . ? O11 Pb1 O13 79.3(3) 5_556 . ? O33 Pb2 O33 180.0(5) 8_665 4_546 ? O33 Pb2 O21 89.1(3) 8_665 5_656 ? O33 Pb2 O21 90.9(3) 4_546 5_656 ? O33 Pb2 O21 90.9(3) 8_665 . ? O33 Pb2 O21 89.1(3) 4_546 . ? O21 Pb2 O21 180.000(1) 5_656 . ? O33 Pb2 O41 75.0(3) 8_665 5_656 ? O33 Pb2 O41 105.0(3) 4_546 5_656 ? O21 Pb2 O41 80.4(3) 5_656 5_656 ? O21 Pb2 O41 99.6(3) . 5_656 ? O33 Pb2 O41 105.0(3) 8_665 . ? O33 Pb2 O41 75.0(3) 4_546 . ? O21 Pb2 O41 99.6(3) 5_656 . ? O21 Pb2 O41 80.4(3) . . ? O41 Pb2 O41 180.000(1) 5_656 . ? O12 Pb3 O32 79.2(3) . 4_446 ? O12 Pb3 O41 90.2(3) . 4_446 ? O32 Pb3 O41 83.6(3) 4_446 4_446 ? O12 P1 O13 115.3(5) . . ? O12 P1 O11 115.0(5) . . ? O13 P1 O11 110.4(5) . . ? O12 P1 C8 107.4(6) . . ? O13 P1 C8 103.1(5) . . ? O11 P1 C8 104.3(6) . . ? O22 P2 O21 118.2(6) . . ? O22 P2 O23 110.5(6) . . ? O21 P2 O23 111.8(6) . . ? O22 P2 C9 103.7(6) . . ? O21 P2 C9 106.5(6) . . ? O23 P2 C9 104.8(6) . . ? O33 P3 O32 110.8(5) . . ? O33 P3 O31 109.3(6) . . ? O32 P3 O31 112.5(6) . . ? O33 P3 C18 108.6(6) . . ? O32 P3 C18 107.8(6) . . ? O31 P3 C18 107.7(6) . . ? O42 P4 O41 111.5(6) . . ? O42 P4 O43 112.2(6) . . ? O41 P4 O43 109.8(5) . . ? O42 P4 C19 112.3(6) . . ? O41 P4 C19 109.9(6) . . ? O43 P4 C19 100.6(6) . . ? C8 N1 C9 112.0(10) . . ? C8 N1 C7 110.0(10) . . ? C9 N1 C7 112.6(10) . . ? C17 N2 C18 112.3(9) . . ? C17 N2 C19 112.0(10) . . ? C18 N2 C19 112.8(10) . . ? C2 C1 C6 117.2(15) . . ? C2 C1 C7 120.9(13) . . ? C6 C1 C7 121.7(13) . . ? C1 C2 C3 122.2(16) . . ? C4 C3 C2 119.3(15) . . ? C3 C4 C5 120.9(15) . . ? C6 C5 C4 119.9(17) . . ? C5 C6 C1 120.3(16) . . ? N1 C7 C1 116.6(10) . . ? N1 C8 P1 111.6(9) . . ? N1 C9 P2 113.2(8) . . ? C16 C11 C12 117.9(14) . . ? C16 C11 C17 122.2(13) . . ? C12 C11 C17 119.7(13) . . ? C13 C12 C11 120.6(15) . . ? C12 C13 C14 120.4(17) . . ? C15 C14 C13 121.4(18) . . ? C14 C15 C16 118.2(19) . . ? C11 C16 C15 121.5(16) . . ? N2 C17 C11 118.1(11) . . ? N2 C18 P3 111.7(8) . . ? N2 C19 P4 110.6(9) . . ? P1 O11 Pb1 136.3(5) . 5_556 ? P1 O12 Pb3 130.2(5) . . ? P1 O13 Pb1 135.1(5) . . ? P2 O21 Pb2 137.8(5) . . ? P3 O31 Pb1 126.2(6) . . ? P3 O32 Pb3 129.3(6) . 4_546 ? P3 O33 Pb2 170.7(6) . 4_446 ? P4 O41 Pb3 133.4(5) . 4_546 ? P4 O41 Pb2 119.0(5) . . ? Pb3 O41 Pb2 105.2(3) 4_546 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.307 _refine_diff_density_min -3.585 _refine_diff_density_rms 0.338 data_2 _database_code_CSD 214483 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Cl2 N2 O17 P4 Pb3' _chemical_formula_weight 1368.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 I2/a #(No. 15) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 9.8986(2) _cell_length_b 31.4972(4) _cell_length_c 10.9253(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.2900(10) _cell_angle_gamma 90.00 _cell_volume 3391.76(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 15.274 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method 'Narrow frame method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 5499 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2967 _reflns_number_gt 2609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+15.0352P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2967 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 -0.11869(4) 0.212408(14) 0.86091(4) 0.0192(2) Uani 1 1 d . . . Pb2 Pb 0.2500 0.250823(19) 0.0000 0.0191(3) Uani 1 2 d S . . Cl1 Cl -0.2500 0.14161(16) 1.0000 0.0346(10) Uani 1 2 d S . . Cl2 Cl 0.2500 0.09798(16) 0.0000 0.0385(11) Uani 1 2 d S . . P1 P 0.0034(3) 0.21076(9) 0.2048(3) 0.0139(6) Uani 1 1 d . . . P2 P 0.0121(3) 0.15229(10) 0.5943(3) 0.0194(7) Uani 1 1 d . . . C1 C -0.1067(17) 0.0228(5) 0.1372(15) 0.047(4) Uani 1 1 d . . . H1A H -0.1163 0.0167 0.0536 0.056 Uiso 1 1 calc R . . C2 C -0.0108(15) 0.0517(4) 0.1838(13) 0.036(3) Uani 1 1 d . . . H2A H 0.0450 0.0648 0.1313 0.043 Uiso 1 1 calc R . . C3 C 0.0032(13) 0.0613(4) 0.3071(12) 0.029(3) Uani 1 1 d . . . C4 C -0.076(2) 0.0416(6) 0.3887(16) 0.056(5) Uani 1 1 d . . . H4A H -0.0660 0.0479 0.4723 0.067 Uiso 1 1 calc R . . C5 C -0.171(2) 0.0119(7) 0.3396(19) 0.084(8) Uani 1 1 d . . . H5A H -0.2250 -0.0024 0.3917 0.101 Uiso 1 1 calc R . . C6 C -0.187(2) 0.0034(7) 0.214(2) 0.076(7) Uani 1 1 d . . . H6A H -0.2530 -0.0157 0.1832 0.091 Uiso 1 1 calc R . . C7 C 0.1112(12) 0.0928(4) 0.3561(11) 0.023(3) Uani 1 1 d . . . H7A H 0.1403 0.0856 0.4408 0.028 Uiso 1 1 calc R . . H7B H 0.1892 0.0899 0.3091 0.028 Uiso 1 1 calc R . . C8 C -0.0435(11) 0.1489(4) 0.4316(10) 0.021(3) Uani 1 1 d . . . H8A H -0.1135 0.1274 0.4201 0.025 Uiso 1 1 calc R . . H8B H -0.0842 0.1758 0.4056 0.025 Uiso 1 1 calc R . . C9 C 0.0267(11) 0.1540(3) 0.2196(10) 0.013(2) Uani 1 1 d . . . H9A H -0.0566 0.1401 0.1878 0.016 Uiso 1 1 calc R . . H9B H 0.0974 0.1454 0.1690 0.016 Uiso 1 1 calc R . . N1 N 0.0644(8) 0.1387(3) 0.3505(8) 0.017(2) Uani 1 1 d . . . H11A H 0.1378 0.1544 0.3793 0.021 Uiso 1 1 calc R . . O11 O 0.0969(8) 0.2309(3) 0.3053(8) 0.027(2) Uani 1 1 d . . . O12 O -0.1432(8) 0.2209(3) 0.2280(8) 0.0240(19) Uani 1 1 d . . . O13 O 0.0318(9) 0.2207(3) 0.0739(8) 0.0258(19) Uani 1 1 d . . . O21 O 0.0188(11) 0.1052(3) 0.6387(9) 0.039(2) Uani 1 1 d . . . H21A H 0.0437 0.1045 0.7124 0.059 Uiso 1 1 calc R . . O22 O -0.0980(8) 0.1771(3) 0.6509(7) 0.0239(19) Uani 1 1 d . . . O23 O 0.1532(8) 0.1710(3) 0.6045(8) 0.030(2) Uani 1 1 d . . . O1W O -0.2500 0.2657(4) 1.0000 0.022(2) Uani 1 2 d S . . O2W O 0.3412(8) 0.1831(3) 0.1334(8) 0.027(2) Uani 1 1 d . . . O3W O -0.0452(13) 0.0847(4) 0.8541(11) 0.064(3) Uani 1 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 0.0170(3) 0.0233(4) 0.0175(3) 0.00085(17) 0.00253(19) 0.00073(15) Pb2 0.0151(4) 0.0211(4) 0.0207(4) 0.000 0.0001(2) 0.000 Cl1 0.037(2) 0.029(3) 0.035(3) 0.000 -0.0081(18) 0.000 Cl2 0.039(3) 0.031(3) 0.047(3) 0.000 0.012(2) 0.000 P1 0.0138(14) 0.0140(15) 0.0139(14) -0.0029(11) 0.0004(10) -0.0015(10) P2 0.0211(14) 0.0200(17) 0.0173(15) 0.0006(12) 0.0024(11) 0.0023(11) C1 0.064(10) 0.034(9) 0.041(9) -0.016(7) 0.002(7) -0.020(8) C2 0.048(8) 0.028(8) 0.033(8) 0.001(6) 0.016(6) -0.001(6) C3 0.031(7) 0.024(7) 0.033(7) -0.003(6) 0.005(5) -0.001(5) C4 0.078(12) 0.052(11) 0.041(9) -0.007(8) 0.020(8) -0.030(9) C5 0.114(18) 0.075(15) 0.069(13) -0.036(12) 0.038(12) -0.075(14) C6 0.084(15) 0.068(14) 0.077(13) -0.038(11) 0.017(11) -0.054(11) C7 0.030(6) 0.011(6) 0.030(7) -0.006(5) 0.005(5) 0.002(5) C8 0.013(5) 0.033(7) 0.019(6) 0.005(5) 0.008(4) 0.007(5) C9 0.020(5) 0.006(5) 0.015(5) 0.006(4) 0.004(4) 0.007(4) N1 0.012(4) 0.023(5) 0.018(5) -0.004(4) 0.002(3) -0.006(4) O11 0.028(5) 0.016(5) 0.036(5) -0.014(4) -0.005(4) -0.008(4) O12 0.015(4) 0.032(5) 0.026(5) 0.002(4) 0.005(3) 0.007(3) O13 0.024(4) 0.031(5) 0.025(5) 0.004(4) 0.011(3) 0.000(3) O21 0.069(7) 0.020(5) 0.032(5) 0.010(4) 0.015(5) 0.010(4) O22 0.022(4) 0.031(5) 0.019(4) -0.005(4) 0.002(3) 0.002(3) O23 0.013(4) 0.043(6) 0.033(5) -0.006(4) 0.000(3) 0.006(4) O1W 0.023(6) 0.023(7) 0.018(6) 0.000 -0.002(4) 0.000 O2W 0.026(5) 0.033(5) 0.023(5) -0.002(4) -0.002(3) -0.006(4) O3W 0.058(7) 0.082(10) 0.053(7) 0.025(6) 0.015(6) 0.002(6) _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 O12 2.480(8) 2_456 ? Pb1 O12 2.552(9) 8 ? Pb1 O22 2.574(8) . ? Pb1 O13 2.658(9) 1_556 ? Pb1 O1W 2.679(8) . ? Pb1 Cl1 3.055(4) . ? Pb2 O13 2.557(8) 2 ? Pb2 O13 2.557(8) . ? Pb2 O11 2.561(8) 7 ? Pb2 O11 2.561(8) 8_554 ? Pb2 O2W 2.692(9) 2 ? Pb2 O2W 2.692(9) . ? Cl1 Pb1 3.055(4) 2_457 ? P1 O11 1.510(8) . ? P1 O13 1.515(9) . ? P1 O12 1.530(8) . ? P1 C9 1.806(10) . ? P2 O23 1.511(9) . ? P2 O22 1.518(8) . ? P2 O21 1.559(9) . ? P2 C8 1.814(12) . ? C1 C6 1.36(3) . ? C1 C2 1.38(2) . ? C2 C3 1.375(19) . ? C3 C4 1.39(2) . ? C3 C7 1.519(17) . ? C4 C5 1.40(2) . ? C5 C6 1.39(3) . ? C7 N1 1.519(15) . ? C8 N1 1.485(13) . ? C9 N1 1.523(13) . ? O11 Pb2 2.561(8) 7 ? O12 Pb1 2.480(8) 2_456 ? O12 Pb1 2.552(9) 8_554 ? O13 Pb1 2.658(9) 1_554 ? O1W Pb1 2.679(8) 2_457 ? 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 O12 Pb1 O12 69.6(3) 2_456 8 ? O12 Pb1 O22 81.3(3) 2_456 . ? O12 Pb1 O22 81.9(3) 8 . ? O12 Pb1 O13 140.2(3) 2_456 1_556 ? O12 Pb1 O13 115.7(3) 8 1_556 ? O22 Pb1 O13 137.6(3) . 1_556 ? O12 Pb1 O1W 70.2(2) 2_456 . ? O12 Pb1 O1W 77.4(3) 8 . ? O22 Pb1 O1W 149.15(18) . . ? O13 Pb1 O1W 72.78(19) 1_556 . ? O12 Pb1 Cl1 80.9(2) 2_456 . ? O12 Pb1 Cl1 149.44(18) 8 . ? O22 Pb1 Cl1 101.6(2) . . ? O13 Pb1 Cl1 82.30(18) 1_556 . ? O1W Pb1 Cl1 85.6(2) . . ? O13 Pb2 O13 136.4(4) 2 . ? O13 Pb2 O11 83.9(3) 2 7 ? O13 Pb2 O11 105.9(3) . 7 ? O13 Pb2 O11 105.9(3) 2 8_554 ? O13 Pb2 O11 83.9(3) . 8_554 ? O11 Pb2 O11 154.1(4) 7 8_554 ? O13 Pb2 O2W 77.6(3) 2 2 ? O13 Pb2 O2W 68.0(3) . 2 ? O11 Pb2 O2W 140.4(3) 7 2 ? O11 Pb2 O2W 65.5(3) 8_554 2 ? O13 Pb2 O2W 68.0(3) 2 . ? O13 Pb2 O2W 77.6(3) . . ? O11 Pb2 O2W 65.5(3) 7 . ? O11 Pb2 O2W 140.4(3) 8_554 . ? O2W Pb2 O2W 75.2(4) 2 . ? Pb1 Cl1 Pb1 86.25(13) . 2_457 ? O11 P1 O13 116.4(5) . . ? O11 P1 O12 108.6(5) . . ? O13 P1 O12 112.0(5) . . ? O11 P1 C9 106.6(5) . . ? O13 P1 C9 104.8(5) . . ? O12 P1 C9 107.9(5) . . ? O23 P2 O22 117.5(5) . . ? O23 P2 O21 109.6(5) . . ? O22 P2 O21 112.0(5) . . ? O23 P2 C8 106.8(5) . . ? O22 P2 C8 105.4(5) . . ? O21 P2 C8 104.5(6) . . ? C6 C1 C2 119.4(15) . . ? C3 C2 C1 120.7(13) . . ? C2 C3 C4 121.4(13) . . ? C2 C3 C7 119.5(12) . . ? C4 C3 C7 119.1(13) . . ? C3 C4 C5 116.9(16) . . ? C6 C5 C4 121.1(17) . . ? C1 C6 C5 120.5(16) . . ? N1 C7 C3 113.9(10) . . ? N1 C8 P2 115.3(7) . . ? N1 C9 P1 114.6(7) . . ? C8 N1 C7 114.5(9) . . ? C8 N1 C9 111.4(8) . . ? C7 N1 C9 112.8(8) . . ? P1 O11 Pb2 167.1(6) . 7 ? P1 O12 Pb1 142.6(5) . 2_456 ? P1 O12 Pb1 103.0(4) . 8_554 ? Pb1 O12 Pb1 110.4(3) 2_456 8_554 ? P1 O13 Pb2 127.6(5) . . ? P1 O13 Pb1 131.9(5) . 1_554 ? Pb2 O13 Pb1 100.5(3) . 1_554 ? P2 O22 Pb1 134.8(4) . . ? Pb1 O1W Pb1 102.5(4) 2_457 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.450 _refine_diff_density_min -4.580 _refine_diff_density_rms 0.426