# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Ruibiao Fu' _publ_contact_author_email furb@fjirsm.ac.cn _publ_section_title ; Syntheses, crystal structures, thermal stabilities and luminescence of two metal phosphonates ; loop_ _publ_author_name 'Ruibiao Fu' 'Shengmin Hu' 'Xintao Xu' # Attachment '- 1.CIF' data_f1 _database_code_depnum_ccdc_archive 'CCDC 831048' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 O12 P2 Zn3' _chemical_formula_weight 746.46 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' Zn Zn 0.2839 1.4301 '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 16.566(15) _cell_length_b 8.573(8) _cell_length_c 18.719(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.70(2) _cell_angle_gamma 90.00 _cell_volume 2603(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5673 _cell_measurement_theta_min 2.6224 _cell_measurement_theta_max 27.5750 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 2.933 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8357 _exptl_absorpt_correction_T_max 1.0000 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19359 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5913 _reflns_number_gt 4458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0773P)^2^+39.4828P] 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 5913 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2038 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Zn1 Zn -0.24254(6) 0.19845(11) 0.26012(5) 0.0230(2) Uani 1 1 d . . . Zn2 Zn -0.06357(6) 0.77358(11) 0.27275(5) 0.0223(2) Uani 1 1 d . . . Zn3 Zn -0.54833(6) 0.26450(11) 0.29065(5) 0.0247(3) Uani 1 1 d . . . P1 P -0.08421(12) 0.4049(2) 0.28062(12) 0.0217(4) Uani 1 1 d . . . P2 P -0.39029(14) 0.4392(3) 0.25646(14) 0.0302(5) Uani 1 1 d . . . O1 O -0.1454(4) 0.3092(7) 0.3126(3) 0.0295(13) Uani 1 1 d . . . O2 O -0.1173(4) 0.5681(7) 0.2587(3) 0.0285(13) Uani 1 1 d . . . O3 O -0.0549(4) 0.3192(7) 0.2193(3) 0.0280(13) Uani 1 1 d . . . O4 O 0.2261(3) 0.5914(7) 0.3324(3) 0.0264(12) Uani 1 1 d . . . O5 O 0.1471(4) 0.4500(7) 0.2498(3) 0.0322(14) Uani 1 1 d . . . O6 O -0.3213(4) 0.3606(8) 0.2273(4) 0.0433(18) Uani 1 1 d . . . O7 O -0.4352(4) 0.3244(7) 0.2950(3) 0.0292(13) Uani 1 1 d . . . O8 O -0.4441(5) 0.5297(8) 0.1981(4) 0.0414(16) Uani 1 1 d . . . O9 O -0.2835(4) 1.0642(7) 0.3296(3) 0.0294(13) Uani 1 1 d . . . O10 O -0.3634(4) 0.9348(7) 0.2376(3) 0.0317(14) Uani 1 1 d . . . O11 O -0.1950(9) 0.4275(18) 0.4501(6) 0.082(4) Uani 0.75 1 d P . . O12 O -0.2624(9) 0.5522(18) 0.1282(9) 0.100(6) Uani 0.75 1 d P . . O13 O -0.2505(17) 0.301(3) 0.0425(13) 0.106(9) Uani 0.50 1 d P . . N1 N 0.0560(4) 0.2010(8) 0.6149(4) 0.0262(15) Uani 1 1 d . . . N2 N 0.0712(4) 0.3129(7) 0.3484(4) 0.0205(13) Uani 1 1 d . . . N3 N -0.4515(5) 0.7041(8) 0.5981(4) 0.0303(16) Uani 1 1 d . . . N4 N -0.4076(5) 0.7144(9) 0.3290(4) 0.0305(16) Uani 1 1 d . . . C1 C -0.0137(5) 0.2113(9) 0.5639(5) 0.0255(17) Uani 1 1 d . . . H1 H -0.0630 0.2258 0.5795 0.031 Uiso 1 1 calc R . . C2 C -0.0169(5) 0.2018(9) 0.4898(4) 0.0247(17) Uani 1 1 d . . . H2 H -0.0670 0.2105 0.4570 0.030 Uiso 1 1 calc R . . C3 C 0.0557(5) 0.1790(9) 0.4648(5) 0.0245(17) Uani 1 1 d . . . C4 C 0.1284(6) 0.1674(11) 0.5172(5) 0.034(2) Uani 1 1 d . . . H3 H 0.1784 0.1528 0.5029 0.040 Uiso 1 1 calc R . . C5 C 0.1264(6) 0.1774(13) 0.5897(5) 0.038(2) Uani 1 1 d . . . H4 H 0.1757 0.1676 0.6235 0.046 Uiso 1 1 calc R . . C6 C 0.0558(5) 0.1669(9) 0.3848(4) 0.0244(17) Uani 1 1 d . . . H5 H 0.0976 0.0917 0.3785 0.029 Uiso 1 1 calc R . . H6 H 0.0029 0.1258 0.3603 0.029 Uiso 1 1 calc R . . C7 C 0.1541(4) 0.3778(9) 0.3748(4) 0.0198(15) Uani 1 1 d . . . H7 H 0.1939 0.2939 0.3866 0.024 Uiso 1 1 calc R . . H8 H 0.1550 0.4390 0.4185 0.024 Uiso 1 1 calc R . . C8 C 0.1768(5) 0.4810(9) 0.3149(4) 0.0219(16) Uani 1 1 d . . . C9 C 0.0084(5) 0.4343(9) 0.3505(4) 0.0215(16) Uani 1 1 d . . . H9 H 0.0317 0.5357 0.3437 0.026 Uiso 1 1 calc R . . H10 H -0.0062 0.4335 0.3981 0.026 Uiso 1 1 calc R . . C10 C -0.5117(8) 0.7692(16) 0.5489(6) 0.061(4) Uani 1 1 d . . . H11 H -0.5522 0.8240 0.5663 0.073 Uiso 1 1 calc R . . C11 C -0.5184(7) 0.7616(16) 0.4755(6) 0.056(3) Uani 1 1 d . . . H12 H -0.5616 0.8121 0.4447 0.067 Uiso 1 1 calc R . . C12 C -0.4615(5) 0.6796(9) 0.4467(5) 0.0241(17) Uani 1 1 d . . . C13 C -0.3985(6) 0.6085(15) 0.4958(6) 0.051(3) Uani 1 1 d . . . H13 H -0.3586 0.5501 0.4793 0.061 Uiso 1 1 calc R . . C14 C -0.3956(6) 0.6253(14) 0.5699(5) 0.041(2) Uani 1 1 d . . . H14 H -0.3521 0.5790 0.6021 0.050 Uiso 1 1 calc R . . C15 C -0.4733(5) 0.6637(10) 0.3653(5) 0.0276(18) Uani 1 1 d . . . H15 H -0.4841 0.5545 0.3534 0.033 Uiso 1 1 calc R . . H16 H -0.5227 0.7210 0.3438 0.033 Uiso 1 1 calc R . . C16 C -0.3689(6) 0.8631(10) 0.3598(5) 0.0278(18) Uani 1 1 d . . . H17 H -0.3240 0.8393 0.4003 0.033 Uiso 1 1 calc R . . H18 H -0.4093 0.9239 0.3787 0.033 Uiso 1 1 calc R . . C17 C -0.3358(5) 0.9607(10) 0.3044(5) 0.0247(17) Uani 1 1 d . . . C18 C -0.3444(5) 0.5915(11) 0.3232(5) 0.0309(19) Uani 1 1 d . . . H19 H -0.3249 0.5441 0.3706 0.037 Uiso 1 1 calc R . . H20 H -0.2977 0.6390 0.3077 0.037 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 Zn1 0.0233(5) 0.0179(4) 0.0301(5) -0.0008(4) 0.0109(4) -0.0016(3) Zn2 0.0265(5) 0.0203(4) 0.0205(5) 0.0021(3) 0.0055(4) 0.0029(4) Zn3 0.0240(5) 0.0244(5) 0.0266(5) -0.0067(4) 0.0075(4) -0.0039(4) P1 0.0212(9) 0.0196(9) 0.0244(11) -0.0003(8) 0.0053(8) -0.0051(8) P2 0.0287(11) 0.0260(11) 0.0381(13) 0.0077(10) 0.0117(10) 0.0076(9) O1 0.033(3) 0.026(3) 0.033(3) -0.005(2) 0.014(3) -0.015(2) O2 0.029(3) 0.024(3) 0.030(3) 0.002(2) 0.001(3) 0.000(2) O3 0.032(3) 0.032(3) 0.019(3) -0.005(2) 0.006(2) -0.006(3) O4 0.025(3) 0.025(3) 0.028(3) -0.002(2) 0.002(2) -0.004(2) O5 0.043(4) 0.030(3) 0.024(3) 0.000(3) 0.008(3) -0.013(3) O6 0.039(4) 0.040(4) 0.060(5) 0.022(3) 0.033(4) 0.016(3) O7 0.026(3) 0.027(3) 0.034(3) -0.001(3) 0.005(3) -0.004(2) O8 0.060(4) 0.030(3) 0.030(4) 0.001(3) -0.001(3) 0.006(3) O9 0.028(3) 0.029(3) 0.031(3) 0.005(3) 0.007(3) 0.000(2) O10 0.034(3) 0.031(3) 0.030(3) 0.010(3) 0.008(3) -0.011(3) O11 0.111(11) 0.099(11) 0.037(7) -0.005(7) 0.017(7) 0.037(9) O12 0.088(10) 0.092(11) 0.137(14) 0.065(10) 0.060(10) 0.006(8) O13 0.16(2) 0.095(17) 0.076(15) 0.036(13) 0.059(16) 0.054(17) N1 0.027(3) 0.028(4) 0.022(4) 0.002(3) 0.002(3) 0.000(3) N2 0.025(3) 0.016(3) 0.021(3) 0.002(2) 0.006(3) -0.004(3) N3 0.033(4) 0.025(4) 0.031(4) -0.007(3) 0.002(3) 0.002(3) N4 0.032(4) 0.027(4) 0.033(4) 0.000(3) 0.006(3) -0.002(3) C1 0.026(4) 0.023(4) 0.029(5) -0.004(3) 0.010(3) 0.002(3) C2 0.029(4) 0.023(4) 0.020(4) 0.002(3) 0.000(3) -0.005(3) C3 0.031(4) 0.019(4) 0.025(4) 0.004(3) 0.010(3) -0.003(3) C4 0.033(5) 0.040(5) 0.027(5) -0.003(4) 0.004(4) 0.002(4) C5 0.036(5) 0.060(7) 0.019(4) 0.004(4) 0.007(4) 0.001(5) C6 0.036(4) 0.021(4) 0.018(4) 0.003(3) 0.009(3) -0.002(3) C7 0.019(3) 0.022(4) 0.018(4) 0.003(3) 0.003(3) -0.007(3) C8 0.022(4) 0.018(4) 0.023(4) -0.002(3) 0.000(3) -0.002(3) C9 0.025(4) 0.016(3) 0.025(4) -0.001(3) 0.008(3) -0.002(3) C10 0.062(7) 0.096(10) 0.027(5) -0.007(6) 0.013(5) 0.050(7) C11 0.044(6) 0.090(9) 0.031(6) -0.010(6) 0.001(5) 0.034(6) C12 0.023(4) 0.022(4) 0.027(4) -0.001(3) 0.004(3) -0.006(3) C13 0.043(6) 0.081(8) 0.033(6) 0.023(5) 0.021(5) 0.035(6) C14 0.030(5) 0.064(7) 0.031(5) 0.006(5) 0.007(4) 0.010(5) C15 0.036(4) 0.024(4) 0.026(4) 0.004(3) 0.013(4) 0.001(3) C16 0.038(5) 0.024(4) 0.023(4) 0.000(3) 0.008(4) -0.004(4) C17 0.019(4) 0.026(4) 0.030(5) 0.008(3) 0.006(3) 0.007(3) C18 0.032(4) 0.032(5) 0.026(5) 0.001(4) -0.001(4) 0.002(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 Zn1 O6 1.920(7) . ? Zn1 O1 1.953(6) . ? Zn1 O9 1.958(6) 1_545 ? Zn1 O4 2.026(6) 2_545 ? Zn2 O2 1.967(6) . ? Zn2 O3 1.978(6) 2 ? Zn2 O5 2.036(6) 2 ? Zn2 N1 2.093(7) 3_566 ? Zn2 N2 2.271(7) 2 ? Zn3 O7 1.930(6) . ? Zn3 O8 2.030(7) 2_445 ? Zn3 O10 2.058(6) 2_445 ? Zn3 N3 2.101(8) 3_466 ? Zn3 N4 2.251(8) 2_445 ? P1 O1 1.519(6) . ? P1 O3 1.523(6) . ? P1 O2 1.527(6) . ? P1 C9 1.821(8) . ? P2 O8 1.481(7) . ? P2 O7 1.504(6) . ? P2 O6 1.521(6) . ? P2 C18 1.859(9) . ? O3 Zn2 1.978(6) 2_545 ? O4 C8 1.250(9) . ? O4 Zn1 2.026(6) 2 ? O5 C8 1.247(10) . ? O5 Zn2 2.036(6) 2_545 ? O8 Zn3 2.030(7) 2_455 ? O9 C17 1.263(10) . ? O9 Zn1 1.958(6) 1_565 ? O10 C17 1.261(11) . ? O10 Zn3 2.058(6) 2_455 ? N1 C1 1.344(11) . ? N1 C5 1.358(11) . ? N1 Zn2 2.093(7) 3_566 ? N2 C7 1.472(9) . ? N2 C6 1.473(9) . ? N2 C9 1.476(10) . ? N2 Zn2 2.271(7) 2_545 ? N3 C10 1.334(13) . ? N3 C14 1.338(12) . ? N3 Zn3 2.101(8) 3_466 ? N4 C15 1.461(11) . ? N4 C16 1.490(11) . ? N4 C18 1.505(11) . ? N4 Zn3 2.251(8) 2_455 ? C1 C2 1.379(12) . ? C2 C3 1.390(12) . ? C3 C4 1.395(12) . ? C3 C6 1.500(11) . ? C4 C5 1.366(13) . ? C7 C8 1.533(11) . ? C10 C11 1.358(15) . ? C11 C12 1.371(13) . ? C12 C13 1.384(13) . ? C12 C15 1.503(12) . ? C13 C14 1.386(14) . ? C16 C17 1.518(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 O6 Zn1 O1 104.3(3) . . ? O6 Zn1 O9 109.5(3) . 1_545 ? O1 Zn1 O9 108.2(3) . 1_545 ? O6 Zn1 O4 104.7(3) . 2_545 ? O1 Zn1 O4 114.2(2) . 2_545 ? O9 Zn1 O4 115.2(3) 1_545 2_545 ? O2 Zn2 O3 127.0(2) . 2 ? O2 Zn2 O5 111.6(3) . 2 ? O3 Zn2 O5 119.5(3) 2 2 ? O2 Zn2 N1 99.2(3) . 3_566 ? O3 Zn2 N1 92.7(3) 2 3_566 ? O5 Zn2 N1 91.7(3) 2 3_566 ? O2 Zn2 N2 93.9(2) . 2 ? O3 Zn2 N2 84.2(2) 2 2 ? O5 Zn2 N2 77.6(2) 2 2 ? N1 Zn2 N2 165.5(3) 3_566 2 ? O7 Zn3 O8 109.8(3) . 2_445 ? O7 Zn3 O10 117.1(3) . 2_445 ? O8 Zn3 O10 132.4(3) 2_445 2_445 ? O7 Zn3 N3 96.9(3) . 3_466 ? O8 Zn3 N3 90.7(3) 2_445 3_466 ? O10 Zn3 N3 91.2(3) 2_445 3_466 ? O7 Zn3 N4 102.1(3) . 2_445 ? O8 Zn3 N4 84.2(3) 2_445 2_445 ? O10 Zn3 N4 79.0(3) 2_445 2_445 ? N3 Zn3 N4 161.0(3) 3_466 2_445 ? O1 P1 O3 112.1(3) . . ? O1 P1 O2 111.6(4) . . ? O3 P1 O2 113.0(4) . . ? O1 P1 C9 108.9(4) . . ? O3 P1 C9 104.9(3) . . ? O2 P1 C9 105.7(3) . . ? O8 P2 O7 114.5(4) . . ? O8 P2 O6 110.5(4) . . ? O7 P2 O6 111.3(4) . . ? O8 P2 C18 103.4(4) . . ? O7 P2 C18 108.1(4) . . ? O6 P2 C18 108.5(4) . . ? P1 O1 Zn1 127.8(4) . . ? P1 O2 Zn2 131.0(4) . . ? P1 O3 Zn2 120.1(3) . 2_545 ? C8 O4 Zn1 108.2(5) . 2 ? C8 O5 Zn2 118.5(5) . 2_545 ? P2 O6 Zn1 135.9(4) . . ? P2 O7 Zn3 136.4(4) . . ? P2 O8 Zn3 118.9(4) . 2_455 ? C17 O9 Zn1 118.0(6) . 1_565 ? C17 O10 Zn3 118.4(5) . 2_455 ? C1 N1 C5 115.9(7) . . ? C1 N1 Zn2 125.1(6) . 3_566 ? C5 N1 Zn2 119.0(6) . 3_566 ? C7 N2 C6 113.8(6) . . ? C7 N2 C9 109.8(6) . . ? C6 N2 C9 113.5(6) . . ? C7 N2 Zn2 104.5(4) . 2_545 ? C6 N2 Zn2 110.9(5) . 2_545 ? C9 N2 Zn2 103.6(5) . 2_545 ? C10 N3 C14 114.8(8) . . ? C10 N3 Zn3 118.6(6) . 3_466 ? C14 N3 Zn3 126.6(6) . 3_466 ? C15 N4 C16 112.2(7) . . ? C15 N4 C18 114.8(7) . . ? C16 N4 C18 112.0(7) . . ? C15 N4 Zn3 113.5(5) . 2_455 ? C16 N4 Zn3 104.4(5) . 2_455 ? C18 N4 Zn3 98.8(5) . 2_455 ? N1 C1 C2 124.2(8) . . ? C1 C2 C3 119.2(8) . . ? C2 C3 C4 117.0(8) . . ? C2 C3 C6 121.5(8) . . ? C4 C3 C6 121.5(8) . . ? C5 C4 C3 120.2(9) . . ? N1 C5 C4 123.4(9) . . ? N2 C6 C3 116.0(7) . . ? N2 C7 C8 108.8(6) . . ? O5 C8 O4 121.7(8) . . ? O5 C8 C7 119.0(7) . . ? O4 C8 C7 119.3(7) . . ? N2 C9 P1 112.2(5) . . ? N3 C10 C11 125.0(9) . . ? C10 C11 C12 120.1(10) . . ? C11 C12 C13 116.8(9) . . ? C11 C12 C15 119.1(8) . . ? C13 C12 C15 124.0(8) . . ? C12 C13 C14 119.1(9) . . ? N3 C14 C13 124.1(9) . . ? N4 C15 C12 119.3(7) . . ? N4 C16 C17 113.2(7) . . ? O10 C17 O9 125.2(8) . . ? O10 C17 C16 118.2(7) . . ? O9 C17 C16 116.6(8) . . ? N4 C18 P2 110.1(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.984 _refine_diff_density_min -1.616 _refine_diff_density_rms 0.201 # Attachment '- 2.CIF' data_f2 _database_code_depnum_ccdc_archive 'CCDC 831049' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 N4 O13 P2 Pb3' _chemical_formula_weight 1189.94 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9939(2) _cell_length_b 10.8591(5) _cell_length_c 14.3633(3) _cell_angle_alpha 88.893(6) _cell_angle_beta 74.348(5) _cell_angle_gamma 84.146(5) _cell_volume 1343.69(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3507 _cell_measurement_theta_min 2.3638 _cell_measurement_theta_max 27.5011 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 18.940 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5036 _exptl_absorpt_correction_T_max 1.0000 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16630 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6131 _reflns_number_gt 5464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6131 _refine_ls_number_parameters 385 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0484 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 -0.28419(2) 0.426682(17) 0.024468(14) 0.01799(5) Uani 1 1 d . . . Pb2 Pb 0.17816(2) 0.203194(16) -0.076425(14) 0.01816(5) Uani 1 1 d . . . Pb3 Pb 0.28022(2) -0.068010(16) 0.076155(14) 0.01904(6) Uani 1 1 d . . . P1 P -0.10759(13) 0.13231(11) 0.10102(9) 0.0135(3) Uani 1 1 d . . . P2 P 0.38349(13) 0.23295(11) 0.08383(9) 0.0148(3) Uani 1 1 d . . . O1 O -0.0945(4) 0.2221(3) 0.0152(2) 0.0197(8) Uani 1 1 d . . . O2 O -0.1956(4) 0.0246(3) 0.0900(2) 0.0187(7) Uani 1 1 d . . . O3 O 0.0534(4) 0.0971(3) 0.1141(3) 0.0234(8) Uani 1 1 d . . . O4 O -0.1217(4) 0.5636(3) 0.0994(3) 0.0318(10) Uani 1 1 d . . . O5 O 0.0610(4) 0.5697(3) 0.1760(3) 0.0290(9) Uani 1 1 d . . . O6 O 0.5414(4) 0.2729(3) 0.0816(3) 0.0271(9) Uani 1 1 d . . . O7 O 0.2754(4) 0.3315(3) 0.0524(2) 0.0209(8) Uani 1 1 d . . . O8 O 0.4037(4) 0.1142(3) 0.0223(3) 0.0217(8) Uani 1 1 d . . . O9 O 0.4252(5) -0.1946(3) 0.1886(3) 0.0368(10) Uani 1 1 d . . . O10 O 0.6020(5) -0.1751(4) 0.2667(4) 0.0520(13) Uani 1 1 d . . . O11 O -0.5265(4) 0.5640(3) 0.1165(3) 0.0253(8) Uani 1 1 d D . . H1 H -0.528(7) 0.647(2) 0.136(4) 0.07(2) Uiso 1 1 d D . . H2 H -0.593(5) 0.525(4) 0.167(3) 0.037(17) Uiso 1 1 d D . . O12 O 0.0067(5) 0.1837(4) -0.2004(3) 0.0311(9) Uani 1 1 d D . . H3 H -0.033(7) 0.268(3) -0.190(4) 0.07(2) Uiso 1 1 d D . . H4 H 0.063(6) 0.179(5) -0.2677(19) 0.07(2) Uiso 1 1 d D . . O13 O 0.7299(5) 0.5274(4) 0.7301(3) 0.0346(10) Uani 1 1 d D . . H5 H 0.739(6) 0.474(5) 0.677(3) 0.06(2) Uiso 1 1 d D . . H6 H 0.814(5) 0.502(5) 0.756(4) 0.06(2) Uiso 1 1 d D . . N1 N -0.2244(4) 0.3555(3) 0.1961(3) 0.0136(8) Uani 1 1 d . . . N2 N -0.2900(6) 0.4156(5) 0.5598(4) 0.0455(14) Uani 1 1 d . . . N3 N 0.3043(4) 0.0523(3) 0.2259(3) 0.0150(8) Uani 1 1 d . . . N4 N 0.1362(6) 0.1604(5) 0.5950(4) 0.0433(14) Uani 1 1 d . . . C1 C -0.2294(5) 0.2200(4) 0.2076(3) 0.0160(10) Uani 1 1 d . . . H7 H -0.3358 0.2008 0.2189 0.019 Uiso 1 1 calc R . . H8 H -0.1945 0.1939 0.2638 0.019 Uiso 1 1 calc R . . C2 C -0.0437(5) 0.5175(4) 0.1548(4) 0.0192(11) Uani 1 1 d . . . C3 C -0.0701(5) 0.3896(4) 0.1931(4) 0.0158(10) Uani 1 1 d . . . H9 H 0.0075 0.3305 0.1527 0.019 Uiso 1 1 calc R . . H10 H -0.0564 0.3847 0.2578 0.019 Uiso 1 1 calc R . . C4 C -0.3495(5) 0.4258(5) 0.2716(4) 0.0204(11) Uani 1 1 d . . . H11 H -0.4473 0.3939 0.2738 0.024 Uiso 1 1 calc R . . H12 H -0.3575 0.5117 0.2521 0.024 Uiso 1 1 calc R . . C5 C -0.3277(5) 0.4213(5) 0.3726(4) 0.0220(11) Uani 1 1 d . . . C6 C -0.2465(7) 0.5062(6) 0.4027(4) 0.0385(15) Uani 1 1 d . . . H13 H -0.2037 0.5677 0.3612 0.046 Uiso 1 1 calc R . . C7 C -0.2295(7) 0.4989(7) 0.4951(5) 0.0484(18) Uani 1 1 d . . . H14 H -0.1720 0.5558 0.5135 0.058 Uiso 1 1 calc R . . C8 C -0.3912(7) 0.3352(5) 0.4398(4) 0.0349(14) Uani 1 1 d . . . H15 H -0.4471 0.2757 0.4232 0.042 Uiso 1 1 calc R . . C9 C -0.3714(8) 0.3379(6) 0.5316(5) 0.0461(17) Uani 1 1 d . . . H16 H -0.4188 0.2810 0.5762 0.055 Uiso 1 1 calc R . . C10 C 0.2903(6) 0.1878(4) 0.2080(4) 0.0191(11) Uani 1 1 d . . . H17 H 0.3356 0.2286 0.2517 0.023 Uiso 1 1 calc R . . H18 H 0.1811 0.2178 0.2235 0.023 Uiso 1 1 calc R . . C11 C 0.4967(6) -0.1329(5) 0.2323(4) 0.0262(13) Uani 1 1 d . . . C12 C 0.4605(5) 0.0083(4) 0.2357(4) 0.0216(11) Uani 1 1 d . . . H19 H 0.4702 0.0388 0.2966 0.026 Uiso 1 1 calc R . . H20 H 0.5374 0.0437 0.1842 0.026 Uiso 1 1 calc R . . C13 C 0.1799(5) 0.0167(5) 0.3094(4) 0.0206(11) Uani 1 1 d . . . H21 H 0.1913 -0.0728 0.3141 0.025 Uiso 1 1 calc R . . H22 H 0.0813 0.0399 0.2952 0.025 Uiso 1 1 calc R . . C14 C 0.1708(6) 0.0697(5) 0.4067(4) 0.0225(11) Uani 1 1 d . . . C15 C 0.2647(6) 0.0220(5) 0.4643(4) 0.0351(15) Uani 1 1 d . . . H23 H 0.3417 -0.0423 0.4410 0.042 Uiso 1 1 calc R . . C16 C 0.2443(7) 0.0696(6) 0.5560(5) 0.0448(17) Uani 1 1 d . . . H24 H 0.3098 0.0361 0.5923 0.054 Uiso 1 1 calc R . . C17 C 0.0605(6) 0.1657(5) 0.4475(4) 0.0319(14) Uani 1 1 d . . . H25 H -0.0040 0.2034 0.4121 0.038 Uiso 1 1 calc R . . C18 C 0.0460(7) 0.2056(6) 0.5400(4) 0.0397(15) Uani 1 1 d . . . H26 H -0.0320 0.2682 0.5660 0.048 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 0.01728(10) 0.01771(10) 0.01894(11) -0.00257(8) -0.00421(8) -0.00289(7) Pb2 0.01744(10) 0.01342(10) 0.02243(11) -0.00024(8) -0.00345(8) -0.00121(7) Pb3 0.02643(11) 0.01301(10) 0.01892(11) -0.00080(8) -0.00788(8) -0.00279(7) P1 0.0153(6) 0.0104(6) 0.0137(7) -0.0027(5) -0.0020(5) -0.0012(5) P2 0.0136(6) 0.0122(6) 0.0183(7) -0.0010(5) -0.0038(5) -0.0014(5) O1 0.0223(18) 0.0210(19) 0.0138(19) 0.0013(15) -0.0006(15) -0.0036(14) O2 0.0221(18) 0.0113(17) 0.023(2) -0.0043(14) -0.0052(15) -0.0051(13) O3 0.0200(18) 0.0197(19) 0.032(2) -0.0099(16) -0.0103(16) 0.0040(14) O4 0.045(2) 0.0167(19) 0.043(3) 0.0089(18) -0.026(2) -0.0106(16) O5 0.029(2) 0.0173(19) 0.046(3) -0.0003(17) -0.0187(19) -0.0082(15) O6 0.0210(18) 0.025(2) 0.038(2) 0.0077(17) -0.0102(17) -0.0095(15) O7 0.0194(17) 0.0216(19) 0.020(2) 0.0007(15) -0.0047(15) 0.0046(14) O8 0.0238(18) 0.0135(18) 0.023(2) -0.0033(15) 0.0023(16) -0.0041(14) O9 0.058(3) 0.019(2) 0.038(3) -0.0060(18) -0.026(2) 0.0070(18) O10 0.049(3) 0.043(3) 0.071(4) 0.016(2) -0.033(3) 0.005(2) O11 0.031(2) 0.019(2) 0.023(2) -0.0023(16) -0.0012(17) -0.0042(16) O12 0.045(2) 0.024(2) 0.024(2) -0.0064(17) -0.0084(19) 0.0012(18) O13 0.040(2) 0.040(3) 0.026(2) -0.001(2) -0.015(2) 0.0010(19) N1 0.0130(19) 0.0104(19) 0.017(2) -0.0022(16) -0.0027(17) -0.0002(15) N2 0.053(3) 0.061(4) 0.023(3) -0.010(3) -0.015(3) 0.006(3) N3 0.016(2) 0.013(2) 0.015(2) -0.0016(16) -0.0033(17) -0.0013(15) N4 0.045(3) 0.061(4) 0.024(3) -0.012(3) -0.007(3) -0.005(3) C1 0.022(2) 0.010(2) 0.014(3) -0.0006(19) -0.002(2) -0.0030(18) C2 0.020(3) 0.017(3) 0.022(3) -0.006(2) -0.008(2) 0.000(2) C3 0.011(2) 0.015(2) 0.022(3) -0.004(2) -0.005(2) -0.0028(18) C4 0.018(2) 0.024(3) 0.017(3) -0.008(2) -0.003(2) 0.005(2) C5 0.020(3) 0.022(3) 0.021(3) -0.008(2) -0.003(2) 0.006(2) C6 0.045(4) 0.043(4) 0.026(4) -0.004(3) -0.005(3) -0.012(3) C7 0.048(4) 0.069(5) 0.032(4) -0.014(4) -0.014(3) -0.011(4) C8 0.041(3) 0.032(3) 0.028(4) -0.004(3) -0.004(3) -0.003(3) C9 0.066(5) 0.042(4) 0.024(4) 0.002(3) -0.004(3) 0.003(3) C10 0.026(3) 0.014(3) 0.016(3) 0.002(2) -0.004(2) -0.003(2) C11 0.020(3) 0.032(3) 0.019(3) 0.002(2) 0.004(2) 0.011(2) C12 0.019(3) 0.024(3) 0.021(3) 0.003(2) -0.004(2) -0.002(2) C13 0.021(3) 0.020(3) 0.018(3) -0.001(2) 0.001(2) -0.004(2) C14 0.025(3) 0.025(3) 0.015(3) 0.000(2) 0.002(2) -0.008(2) C15 0.035(3) 0.040(4) 0.026(3) 0.001(3) -0.005(3) 0.011(3) C16 0.044(4) 0.066(5) 0.026(4) 0.001(3) -0.016(3) 0.005(3) C17 0.031(3) 0.038(3) 0.025(3) 0.000(3) -0.005(3) 0.001(3) C18 0.038(4) 0.042(4) 0.030(4) -0.011(3) 0.004(3) 0.003(3) _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 O6 2.389(3) 1_455 ? Pb1 O11 2.565(3) . ? Pb1 O4 2.619(3) . ? Pb1 O1 2.642(3) . ? Pb1 N1 2.743(4) . ? Pb2 O1 2.440(3) . ? Pb2 O2 2.471(3) 2 ? Pb2 O4 2.565(3) 2_565 ? Pb2 O12 2.676(4) . ? Pb2 O7 2.711(3) . ? Pb3 O8 2.381(3) . ? Pb3 O3 2.523(3) . ? Pb3 N3 2.608(4) . ? Pb3 O9 2.624(4) . ? Pb3 O2 2.713(3) 2 ? P1 O2 1.511(3) . ? P1 O3 1.519(3) . ? P1 O1 1.543(3) . ? P1 C1 1.840(5) . ? P2 O7 1.517(3) . ? P2 O6 1.519(3) . ? P2 O8 1.545(4) . ? P2 C10 1.835(5) . ? O2 Pb2 2.471(3) 2 ? O2 Pb3 2.713(3) 2 ? O4 C2 1.261(6) . ? O4 Pb2 2.565(3) 2_565 ? O5 C2 1.253(6) . ? O6 Pb1 2.389(3) 1_655 ? O9 C11 1.256(7) . ? O10 C11 1.228(6) . ? N1 C3 1.463(5) . ? N1 C1 1.481(5) . ? N1 C4 1.491(6) . ? N2 C9 1.308(8) . ? N2 C7 1.332(9) . ? N3 C13 1.479(6) . ? N3 C12 1.479(5) . ? N3 C10 1.487(6) . ? N4 C16 1.328(8) . ? N4 C18 1.331(7) . ? C2 C3 1.501(6) . ? C4 C5 1.515(7) . ? C5 C6 1.376(8) . ? C5 C8 1.382(8) . ? C6 C7 1.376(8) . ? C8 C9 1.378(8) . ? C11 C12 1.534(7) . ? C13 C14 1.501(7) . ? C14 C17 1.383(7) . ? C14 C15 1.392(7) . ? C15 C16 1.382(8) . ? C17 C18 1.374(8) . ? 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 O6 Pb1 O11 79.83(12) 1_455 . ? O6 Pb1 O4 136.28(12) 1_455 . ? O11 Pb1 O4 87.42(12) . . ? O6 Pb1 O1 77.24(10) 1_455 . ? O11 Pb1 O1 149.32(11) . . ? O4 Pb1 O1 95.23(10) . . ? O6 Pb1 N1 76.88(11) 1_455 . ? O11 Pb1 N1 90.17(11) . . ? O4 Pb1 N1 61.40(11) . . ? O1 Pb1 N1 64.99(10) . . ? O1 Pb2 O2 93.87(11) . 2 ? O1 Pb2 O4 82.76(11) . 2_565 ? O2 Pb2 O4 164.04(11) 2 2_565 ? O1 Pb2 O12 71.85(12) . . ? O2 Pb2 O12 80.35(11) 2 . ? O4 Pb2 O12 83.79(11) 2_565 . ? O1 Pb2 O7 95.41(11) . . ? O2 Pb2 O7 125.92(10) 2 . ? O4 Pb2 O7 70.01(10) 2_565 . ? O12 Pb2 O7 152.31(10) . . ? O8 Pb3 O3 78.15(11) . . ? O8 Pb3 N3 71.06(12) . . ? O3 Pb3 N3 74.34(11) . . ? O8 Pb3 O9 109.85(12) . . ? O3 Pb3 O9 131.39(12) . . ? N3 Pb3 O9 64.57(11) . . ? O8 Pb3 O2 79.48(11) . 2 ? O3 Pb3 O2 73.15(10) . 2 ? N3 Pb3 O2 139.70(10) . 2 ? O9 Pb3 O2 154.38(11) . 2 ? O2 P1 O3 115.12(18) . . ? O2 P1 O1 111.34(19) . . ? O3 P1 O1 108.85(19) . . ? O2 P1 C1 105.7(2) . . ? O3 P1 C1 109.8(2) . . ? O1 P1 C1 105.63(19) . . ? O7 P2 O6 114.6(2) . . ? O7 P2 O8 110.1(2) . . ? O6 P2 O8 109.9(2) . . ? O7 P2 C10 108.5(2) . . ? O6 P2 C10 108.0(2) . . ? O8 P2 C10 105.2(2) . . ? P1 O1 Pb2 106.57(16) . . ? P1 O1 Pb1 122.32(18) . . ? Pb2 O1 Pb1 123.81(13) . . ? P1 O2 Pb2 144.20(18) . 2 ? P1 O2 Pb3 105.21(16) . 2 ? Pb2 O2 Pb3 94.86(11) 2 2 ? P1 O3 Pb3 143.5(2) . . ? C2 O4 Pb2 124.0(3) . 2_565 ? C2 O4 Pb1 121.0(3) . . ? Pb2 O4 Pb1 114.01(12) 2_565 . ? P2 O6 Pb1 144.5(2) . 1_655 ? P2 O7 Pb2 101.29(17) . . ? P2 O8 Pb3 124.65(19) . . ? C11 O9 Pb3 115.8(3) . . ? C3 N1 C1 110.5(3) . . ? C3 N1 C4 112.5(4) . . ? C1 N1 C4 111.8(4) . . ? C3 N1 Pb1 107.4(3) . . ? C1 N1 Pb1 109.6(3) . . ? C4 N1 Pb1 104.7(3) . . ? C9 N2 C7 116.1(6) . . ? C13 N3 C12 112.0(4) . . ? C13 N3 C10 112.1(4) . . ? C12 N3 C10 111.2(4) . . ? C13 N3 Pb3 106.7(3) . . ? C12 N3 Pb3 104.5(3) . . ? C10 N3 Pb3 110.0(3) . . ? C16 N4 C18 116.0(5) . . ? N1 C1 P1 112.6(3) . . ? O5 C2 O4 123.7(5) . . ? O5 C2 C3 117.7(4) . . ? O4 C2 C3 118.6(4) . . ? N1 C3 C2 113.1(4) . . ? N1 C4 C5 115.5(4) . . ? C6 C5 C8 116.6(5) . . ? C6 C5 C4 121.1(5) . . ? C8 C5 C4 122.3(5) . . ? C5 C6 C7 119.2(6) . . ? N2 C7 C6 124.2(6) . . ? C9 C8 C5 119.8(6) . . ? N2 C9 C8 124.0(6) . . ? N3 C10 P2 114.7(3) . . ? O10 C11 O9 125.4(5) . . ? O10 C11 C12 116.5(5) . . ? O9 C11 C12 117.9(4) . . ? N3 C12 C11 114.4(4) . . ? N3 C13 C14 117.8(4) . . ? C17 C14 C15 115.5(5) . . ? C17 C14 C13 121.4(5) . . ? C15 C14 C13 123.1(5) . . ? C16 C15 C14 120.5(5) . . ? N4 C16 C15 123.5(5) . . ? C18 C17 C14 120.2(5) . . ? N4 C18 C17 124.3(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H1 O9 0.942(19) 1.86(3) 2.786(5) 168(5) 1_465 O11 H2 O13 0.936(19) 1.77(2) 2.702(6) 172(5) 2_566 O12 H3 O5 0.946(19) 1.76(3) 2.693(5) 167(6) 2_565 O12 H4 N4 0.963(19) 1.91(2) 2.860(6) 168(6) 1_554 O13 H5 N2 0.948(19) 1.90(2) 2.808(7) 160(5) 1_655 O13 H6 O5 0.945(19) 1.79(2) 2.716(5) 165(6) 2_666 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.407 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.190