# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C63 H36 N9 O19 Zn4), O Zn4' _chemical_formula_sum 'C126 H72 N18 O39 Zn12' _chemical_formula_weight 3246.46 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 21.135(3) _cell_length_b 21.135(3) _cell_length_c 8.5104(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3292.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9034 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.36 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1626 _exptl_absorpt_coefficient_mu 2.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5090 _exptl_absorpt_correction_T_max 0.6055 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29909 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.39 _reflns_number_total 5533 _reflns_number_gt 4456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A ' _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 ; restraints used in refinements: simu 0.02 0.04 3.8 o3 o4 o3a o4a simu 0.02 0.04 3.8 o1 o2 o5 o6 o1b o2b o5b o6b sadi 0.01 c1 o1 c1 o1b sadi 0.01 c1 o2 c1 o2b sadi 0.01 c15 o5 c15 o5b sadi 0.01 c15 o6 c15 o6b eadp zn1 zn1b eadp zn2 zn2b 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^)+(0.0769P)^2^+4.7435P] 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 5533 _refine_ls_number_parameters 360 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.076 _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 Zn3 Zn 1.0000 1.0000 0.23483(14) 0.0237(3) Uani 0.50 3 d SP . . Zn4 Zn 0.90462(4) 0.92460(4) 0.06636(8) 0.02041(19) Uani 0.50 1 d P . . O3 O 0.9122(2) 0.8496(2) 0.1834(6) 0.0358(12) Uani 0.537(5) 1 d PU A 1 O4 O 1.0333(3) 0.8925(3) 0.1970(6) 0.0402(13) Uani 0.537(5) 1 d PU A 1 O3A O 0.9662(3) 0.8392(3) 0.1057(6) 0.0358(14) Uani 0.463(5) 1 d PU . 2 O4A O 0.9769(3) 0.9054(3) 0.3193(6) 0.0376(14) Uani 0.463(5) 1 d PU A 2 O7 O 1.0000 1.0000 0.0000 0.0204(10) Uani 1 6 d S . . O9 O 0.6667 0.3333 0.3469(4) 0.0200(7) Uani 1 3 d S . . N1 N 0.8160(2) 0.63660(17) 0.1604(4) 0.0501(10) Uani 1 1 d . B . N2 N 0.8665(2) 0.69685(16) 0.1722(4) 0.0458(9) Uani 1 1 d . . . N3 N 0.96934(15) 0.48019(18) 0.5287(3) 0.0354(7) Uani 1 1 d . . . C1 C 0.70887(18) 0.48763(16) 0.1082(4) 0.0258(6) Uani 1 1 d D . . C2 C 0.72473(18) 0.54636(17) -0.0105(4) 0.0261(6) Uani 1 1 d . B . C3 C 0.6852(2) 0.5265(2) -0.1484(4) 0.0354(8) Uani 1 1 d . . . H3 H 0.6487 0.4782 -0.1638 0.042 Uiso 1 1 calc R B . C4 C 0.6995(3) 0.5780(3) -0.2641(5) 0.0517(11) Uani 1 1 d . B . H4 H 0.6732 0.5642 -0.3576 0.062 Uiso 1 1 calc R . . C5 C 0.7527(3) 0.6499(3) -0.2407(5) 0.0638(15) Uani 1 1 d . . . H5 H 0.7618 0.6846 -0.3180 0.077 Uiso 1 1 calc R B . C6 C 0.7923(3) 0.6705(2) -0.1031(5) 0.0551(12) Uani 1 1 d . B . H6 H 0.8280 0.7190 -0.0875 0.066 Uiso 1 1 calc R . . C7 C 0.7789(2) 0.61896(18) 0.0122(4) 0.0340(8) Uani 1 1 d . . . C8 C 0.9045(2) 0.71419(18) 0.3194(4) 0.0323(7) Uani 1 1 d . . . C9 C 0.8955(3) 0.6609(2) 0.4270(5) 0.0531(12) Uani 1 1 d . . . H9 H 0.8630 0.6119 0.4056 0.064 Uiso 1 1 calc R . . C10 C 0.9345(3) 0.6805(3) 0.5655(5) 0.0633(14) Uani 1 1 d . . . H10 H 0.9287 0.6446 0.6367 0.076 Uiso 1 1 calc R . . C11 C 0.9821(3) 0.7532(2) 0.5991(5) 0.0524(11) Uani 1 1 d . . . H11 H 1.0079 0.7664 0.6933 0.063 Uiso 1 1 calc R . . C12 C 0.9912(2) 0.8061(2) 0.4927(4) 0.0387(8) Uani 1 1 d . . . H12 H 1.0232 0.8550 0.5157 0.046 Uiso 1 1 calc R . . C13 C 0.95330(18) 0.78752(17) 0.3513(4) 0.0264(6) Uani 1 1 d . A . C14 C 0.96631(18) 0.84774(17) 0.2410(4) 0.0272(7) Uani 1 1 d . . . C15 C 0.82092(16) 0.44578(17) 0.5921(4) 0.0240(6) Uani 1 1 d D . . C16 C 0.88302(16) 0.49150(17) 0.7000(3) 0.0250(6) Uani 1 1 d . B . C17 C 0.86787(19) 0.5154(2) 0.8392(4) 0.0344(8) Uani 1 1 d . . . H17 H 0.8197 0.5012 0.8643 0.041 Uiso 1 1 calc R B . C18 C 0.9231(2) 0.5599(3) 0.9406(5) 0.0522(11) Uani 1 1 d . B . H18 H 0.9122 0.5762 1.0328 0.063 Uiso 1 1 calc R . . C19 C 0.9942(2) 0.5803(3) 0.9057(5) 0.0676(16) Uani 1 1 d . . . H19 H 1.0314 0.6102 0.9746 0.081 Uiso 1 1 calc R B . C20 C 1.0110(2) 0.5564(3) 0.7680(5) 0.0560(13) Uani 1 1 d . B . H20 H 1.0593 0.5702 0.7453 0.067 Uiso 1 1 calc R . . C21 C 0.95536(17) 0.5115(2) 0.6640(4) 0.0326(8) Uani 1 1 d . . . Zn1 Zn 0.59554(2) 0.35928(2) 0.27491(4) 0.01971(12) Uani 0.930(2) 1 d P B 1 Zn2 Zn 0.6667 0.3333 0.57537(7) 0.01906(15) Uani 0.930(2) 3 d SP . 1 O1 O 0.76119(14) 0.48181(14) 0.1576(3) 0.0330(6) Uani 0.930(2) 1 d PDU . 1 O2 O 0.64193(14) 0.44673(14) 0.1456(3) 0.0360(6) Uani 0.930(2) 1 d PDU B 1 O5 O 0.83159(14) 0.45413(15) 0.4470(3) 0.0350(6) Uani 0.930(2) 1 d PDU . 1 O6 O 0.76139(13) 0.40349(14) 0.6588(3) 0.0341(6) Uani 0.930(2) 1 d PDU B 1 Zn1B Zn 0.7339(3) 0.3003(3) 0.3918(5) 0.01971(12) Uani 0.07 1 d P . 2 Zn2B Zn 0.6667 0.3333 0.0921(9) 0.01906(15) Uani 0.07 3 d SP . 2 O1B O 0.717(2) 0.5068(19) 0.2479(17) 0.042(6) Uani 0.070(2) 1 d PDU B 2 O2B O 0.695(2) 0.4323(13) 0.021(4) 0.039(6) Uani 0.070(2) 1 d PDU B 2 O5B O 0.809(2) 0.3859(12) 0.532(4) 0.043(7) Uani 0.070(2) 1 d PDU B 2 O6B O 0.7832(16) 0.4711(18) 0.535(4) 0.039(5) Uani 0.070(2) 1 d PDU B 2 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 Zn3 0.0206(4) 0.0206(4) 0.0299(6) 0.000 0.000 0.01029(19) Zn4 0.0174(3) 0.0174(3) 0.0257(3) -0.0003(2) 0.0006(2) 0.0082(3) O3 0.029(2) 0.028(2) 0.051(3) 0.011(2) -0.001(2) 0.0141(19) O4 0.029(2) 0.030(2) 0.061(3) 0.018(2) 0.006(2) 0.014(2) O3A 0.058(4) 0.021(2) 0.028(2) 0.0042(19) 0.000(2) 0.020(2) O4A 0.057(4) 0.022(3) 0.034(3) 0.003(2) 0.008(2) 0.020(2) O7 0.0164(14) 0.0164(14) 0.028(2) 0.000 0.000 0.0082(7) O9 0.0167(10) 0.0167(10) 0.0265(17) 0.000 0.000 0.0084(5) N1 0.064(2) 0.0189(15) 0.0458(18) 0.0027(13) -0.0228(17) 0.0042(15) N2 0.054(2) 0.0200(14) 0.0433(17) 0.0030(12) -0.0190(15) 0.0034(14) N3 0.0181(13) 0.0466(18) 0.0368(15) -0.0054(13) 0.0002(11) 0.0127(13) C1 0.0276(16) 0.0162(14) 0.0320(15) -0.0001(11) -0.0017(12) 0.0097(12) C2 0.0278(16) 0.0206(15) 0.0307(14) 0.0009(12) -0.0030(12) 0.0126(13) C3 0.0369(19) 0.0317(18) 0.0358(16) -0.0036(14) -0.0080(14) 0.0159(16) C4 0.063(3) 0.050(3) 0.0369(19) 0.0020(17) -0.0192(19) 0.025(2) C5 0.087(4) 0.043(2) 0.045(2) 0.0158(19) -0.018(2) 0.021(3) C6 0.070(3) 0.0235(19) 0.049(2) 0.0110(16) -0.014(2) 0.0062(19) C7 0.039(2) 0.0194(15) 0.0350(17) 0.0030(13) -0.0060(14) 0.0085(14) C8 0.0359(18) 0.0188(15) 0.0332(16) 0.0026(12) -0.0051(14) 0.0069(14) C9 0.067(3) 0.0209(18) 0.050(2) 0.0088(16) -0.015(2) 0.0053(18) C10 0.083(4) 0.042(2) 0.048(2) 0.0180(19) -0.016(2) 0.018(2) C11 0.064(3) 0.045(2) 0.0358(19) 0.0018(17) -0.0173(19) 0.018(2) C12 0.044(2) 0.0287(18) 0.0377(17) -0.0054(14) -0.0095(16) 0.0140(17) C13 0.0276(16) 0.0183(14) 0.0312(15) 0.0006(12) -0.0011(12) 0.0098(13) C14 0.0231(15) 0.0166(14) 0.0410(17) 0.0018(12) 0.0004(13) 0.0092(12) C15 0.0161(14) 0.0214(14) 0.0322(14) -0.0003(12) -0.0017(11) 0.0078(12) C16 0.0140(13) 0.0253(15) 0.0290(14) 0.0011(12) 0.0000(11) 0.0048(12) C17 0.0226(16) 0.039(2) 0.0332(16) -0.0054(14) 0.0030(13) 0.0095(15) C18 0.039(2) 0.064(3) 0.0374(19) -0.0197(19) 0.0001(17) 0.014(2) C19 0.031(2) 0.099(4) 0.043(2) -0.031(2) -0.0119(17) 0.010(2) C20 0.0180(17) 0.087(4) 0.045(2) -0.019(2) -0.0054(15) 0.012(2) C21 0.0169(15) 0.044(2) 0.0283(15) -0.0045(14) -0.0006(12) 0.0088(14) Zn1 0.01756(19) 0.0185(2) 0.02456(19) 0.00119(13) 0.00058(13) 0.01010(15) Zn2 0.0157(2) 0.0157(2) 0.0258(3) 0.000 0.000 0.00783(10) O1 0.0261(13) 0.0274(13) 0.0435(14) 0.0132(11) 0.0014(11) 0.0120(11) O2 0.0246(13) 0.0297(14) 0.0520(15) 0.0175(12) 0.0089(11) 0.0122(11) O5 0.0231(12) 0.0411(15) 0.0262(11) -0.0039(10) -0.0031(9) 0.0050(11) O6 0.0174(12) 0.0365(14) 0.0323(13) 0.0006(10) -0.0018(9) 0.0014(10) Zn1B 0.01756(19) 0.0185(2) 0.02456(19) 0.00119(13) 0.00058(13) 0.01010(15) Zn2B 0.0157(2) 0.0157(2) 0.0258(3) 0.000 0.000 0.00783(10) O1B 0.033(8) 0.033(8) 0.041(8) 0.013(8) -0.010(8) 0.002(8) O2B 0.037(10) 0.021(9) 0.055(11) 0.000(9) 0.004(10) 0.011(8) O5B 0.036(10) 0.038(10) 0.044(10) 0.007(9) -0.006(9) 0.010(9) O6B 0.028(8) 0.034(8) 0.046(9) 0.014(8) -0.011(8) 0.009(7) _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 Zn3 O4A 1.943(5) 2_765 ? Zn3 O4A 1.943(5) . ? Zn3 O4A 1.943(5) 3_675 ? Zn3 O7 1.9985(13) . ? Zn3 Zn4 3.1561(13) 6_655 ? Zn3 Zn4 3.1561(13) 5_565 ? Zn3 Zn4 3.1561(13) 4_775 ? Zn4 O7 1.9260(7) . ? Zn4 O3A 1.933(5) 5_565 ? Zn4 O3 1.945(4) . ? Zn4 O4 1.950(5) 3_675 ? Zn4 Zn3 3.1561(13) 4_775 ? O3 C14 1.263(5) . ? O4 C14 1.303(6) . ? O4 Zn4 1.950(5) 2_765 ? O3A C14 1.166(6) . ? O3A Zn4 1.933(5) 6_655 ? O4A C14 1.307(6) . ? O7 Zn4 1.9260(7) 6_655 ? O7 Zn4 1.9260(7) 2_765 ? O7 Zn4 1.9260(7) 4_775 ? O7 Zn4 1.9260(7) 3_675 ? O7 Zn4 1.9260(7) 5_565 ? O7 Zn3 1.9985(13) 4_775 ? O9 Zn1B 1.909(5) . ? O9 Zn1B 1.909(5) 3_665 ? O9 Zn1B 1.909(5) 2_655 ? O9 Zn1 1.9393(11) 2_655 ? O9 Zn1 1.9393(11) 3_665 ? O9 Zn1 1.9393(11) . ? O9 Zn2 1.944(3) . ? O9 Zn2B 2.168(9) . ? N1 N2 1.189(4) . ? N1 C7 1.432(5) . ? N2 C8 1.433(4) . ? N3 N3 1.239(6) 4_766 ? N3 C21 1.431(4) . ? C1 O1B 1.240(11) . ? C1 O1 1.245(4) . ? C1 O2 1.276(4) . ? C1 O2B 1.288(11) . ? C1 C2 1.503(4) . ? C2 C3 1.379(5) . ? C2 C7 1.395(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(7) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 C7 1.386(5) . ? C6 H6 0.9300 . ? C8 C9 1.389(5) . ? C8 C13 1.393(4) . ? C9 C10 1.378(6) . ? C9 H9 0.9300 . ? C10 C11 1.383(6) . ? C10 H10 0.9300 . ? C11 C12 1.375(5) . ? C11 H11 0.9300 . ? C12 C13 1.389(5) . ? C12 H12 0.9300 . ? C13 C14 1.492(4) . ? C15 O5 1.252(4) . ? C15 O6B 1.257(10) . ? C15 O6 1.257(4) . ? C15 O5B 1.267(11) . ? C15 C16 1.494(4) . ? C16 C17 1.387(4) . ? C16 C21 1.401(4) . ? C17 C18 1.376(5) . ? C17 H17 0.9300 . ? C18 C19 1.373(6) . ? C18 H18 0.9300 . ? C19 C20 1.391(6) . ? C19 H19 0.9300 . ? C20 C21 1.396(5) . ? C20 H20 0.9300 . ? Zn1 O1 1.939(2) 2_655 ? Zn1 O2 1.943(2) . ? Zn1 O5 1.949(2) 2_655 ? Zn1 Zn2 3.1502(7) . ? Zn2 O6 1.934(2) 3_665 ? Zn2 O6 1.934(2) . ? Zn2 O6 1.934(2) 2_655 ? Zn2 Zn1 3.1502(7) 2_655 ? Zn2 Zn1 3.1502(7) 3_665 ? O1 Zn1 1.939(2) 3_665 ? O5 Zn1 1.949(2) 3_665 ? Zn1B O1B 1.86(3) 3_665 ? Zn1B O6B 1.96(3) 3_665 ? Zn1B O5B 2.08(3) . ? Zn2B O2B 1.96(3) 3_665 ? Zn2B O2B 1.96(3) 2_655 ? Zn2B O2B 1.96(3) . ? O1B Zn1B 1.86(3) 2_655 ? O6B Zn1B 1.96(3) 2_655 ? 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 O4A Zn3 O4A 107.12(18) 2_765 . ? O4A Zn3 O4A 107.12(18) 2_765 3_675 ? O4A Zn3 O4A 107.12(18) . 3_675 ? O4A Zn3 O7 111.73(16) 2_765 . ? O4A Zn3 O7 111.73(16) . . ? O4A Zn3 O7 111.73(16) 3_675 . ? O4A Zn3 Zn4 163.72(17) 2_765 . ? O4A Zn3 Zn4 80.68(18) . . ? O4A Zn3 Zn4 83.36(17) 3_675 . ? O7 Zn3 Zn4 52.09(3) . . ? O4A Zn3 Zn4 80.68(18) 2_765 2_765 ? O4A Zn3 Zn4 83.36(17) . 2_765 ? O4A Zn3 Zn4 163.72(17) 3_675 2_765 ? O7 Zn3 Zn4 52.09(3) . 2_765 ? Zn4 Zn3 Zn4 86.21(4) . 2_765 ? O4A Zn3 Zn4 83.36(16) 2_765 3_675 ? O4A Zn3 Zn4 163.72(17) . 3_675 ? O4A Zn3 Zn4 80.68(18) 3_675 3_675 ? O7 Zn3 Zn4 52.09(3) . 3_675 ? Zn4 Zn3 Zn4 86.21(4) . 3_675 ? Zn4 Zn3 Zn4 86.21(4) 2_765 3_675 ? O4A Zn3 Zn4 123.67(18) 2_765 6_655 ? O4A Zn3 Zn4 76.06(16) . 6_655 ? O4A Zn3 Zn4 126.06(16) 3_675 6_655 ? O7 Zn3 Zn4 35.693(19) . 6_655 ? Zn4 Zn3 Zn4 43.19(2) . 6_655 ? Zn4 Zn3 Zn4 43.19(2) 2_765 6_655 ? Zn4 Zn3 Zn4 87.79(4) 3_675 6_655 ? O4A Zn3 Zn4 126.06(16) 2_765 5_565 ? O4A Zn3 Zn4 123.67(18) . 5_565 ? O4A Zn3 Zn4 76.06(16) 3_675 5_565 ? O7 Zn3 Zn4 35.693(19) . 5_565 ? Zn4 Zn3 Zn4 43.19(2) . 5_565 ? Zn4 Zn3 Zn4 87.79(4) 2_765 5_565 ? Zn4 Zn3 Zn4 43.19(2) 3_675 5_565 ? Zn4 Zn3 Zn4 60.70(3) 6_655 5_565 ? O4A Zn3 Zn4 76.06(16) 2_765 4_775 ? O4A Zn3 Zn4 126.06(16) . 4_775 ? O4A Zn3 Zn4 123.67(18) 3_675 4_775 ? O7 Zn3 Zn4 35.693(19) . 4_775 ? Zn4 Zn3 Zn4 87.79(4) . 4_775 ? Zn4 Zn3 Zn4 43.19(2) 2_765 4_775 ? Zn4 Zn3 Zn4 43.19(2) 3_675 4_775 ? Zn4 Zn3 Zn4 60.70(3) 6_655 4_775 ? Zn4 Zn3 Zn4 60.70(3) 5_565 4_775 ? O7 Zn4 O3A 113.70(15) . 5_565 ? O7 Zn4 O3 110.22(14) . . ? O3A Zn4 O3 104.8(2) 5_565 . ? O7 Zn4 O4 109.84(15) . 3_675 ? O3A Zn4 O4 108.3(2) 5_565 3_675 ? O3 Zn4 O4 109.9(2) . 3_675 ? O7 Zn4 Zn4 55.890(9) . 6_655 ? O3A Zn4 Zn4 83.27(17) 5_565 6_655 ? O3 Zn4 Zn4 74.87(15) . 6_655 ? O4 Zn4 Zn4 165.15(15) 3_675 6_655 ? O7 Zn4 Zn4 55.890(9) . 5_565 ? O3A Zn4 Zn4 83.19(18) 5_565 5_565 ? O3 Zn4 Zn4 166.10(14) . 5_565 ? O4 Zn4 Zn4 77.48(16) 3_675 5_565 ? Zn4 Zn4 Zn4 95.16(4) 6_655 5_565 ? O7 Zn4 Zn3 54.96(3) . . ? O3A Zn4 Zn3 168.66(16) 5_565 . ? O3 Zn4 Zn3 81.19(15) . . ? O4 Zn4 Zn3 77.98(16) 3_675 . ? Zn4 Zn4 Zn3 89.14(3) 6_655 . ? Zn4 Zn4 Zn3 89.14(3) 5_565 . ? O7 Zn4 Zn3 37.257(19) . 4_775 ? O3A Zn4 Zn3 76.45(15) 5_565 4_775 ? O3 Zn4 Zn3 122.35(15) . 4_775 ? O4 Zn4 Zn3 124.63(15) 3_675 4_775 ? Zn4 Zn4 Zn3 47.68(2) 6_655 4_775 ? Zn4 Zn4 Zn3 47.68(2) 5_565 4_775 ? Zn3 Zn4 Zn3 92.21(5) . 4_775 ? C14 O3 Zn4 132.0(3) . . ? C14 O4 Zn4 131.9(3) . 2_765 ? C14 O3A Zn4 130.6(4) . 6_655 ? C14 O4A Zn3 127.5(4) . . ? Zn4 O7 Zn4 68.220(19) 6_655 2_765 ? Zn4 O7 Zn4 111.780(19) 6_655 4_775 ? Zn4 O7 Zn4 68.220(19) 2_765 4_775 ? Zn4 O7 Zn4 68.220(19) 6_655 . ? Zn4 O7 Zn4 111.780(19) 2_765 . ? Zn4 O7 Zn4 180.0 4_775 . ? Zn4 O7 Zn4 180.0 6_655 3_675 ? Zn4 O7 Zn4 111.780(19) 2_765 3_675 ? Zn4 O7 Zn4 68.220(19) 4_775 3_675 ? Zn4 O7 Zn4 111.780(19) . 3_675 ? Zn4 O7 Zn4 111.780(19) 6_655 5_565 ? Zn4 O7 Zn4 180.0 2_765 5_565 ? Zn4 O7 Zn4 111.780(19) 4_775 5_565 ? Zn4 O7 Zn4 68.220(19) . 5_565 ? Zn4 O7 Zn4 68.220(19) 3_675 5_565 ? Zn4 O7 Zn3 107.05(2) 6_655 . ? Zn4 O7 Zn3 72.95(2) 2_765 . ? Zn4 O7 Zn3 107.05(2) 4_775 . ? Zn4 O7 Zn3 72.95(2) . . ? Zn4 O7 Zn3 72.95(2) 3_675 . ? Zn4 O7 Zn3 107.05(2) 5_565 . ? Zn4 O7 Zn3 72.95(2) 6_655 4_775 ? Zn4 O7 Zn3 107.05(2) 2_765 4_775 ? Zn4 O7 Zn3 72.95(2) 4_775 4_775 ? Zn4 O7 Zn3 107.05(2) . 4_775 ? Zn4 O7 Zn3 107.05(2) 3_675 4_775 ? Zn4 O7 Zn3 72.95(2) 5_565 4_775 ? Zn3 O7 Zn3 180.0 . 4_775 ? Zn1B O9 Zn1B 116.10(11) . 3_665 ? Zn1B O9 Zn1B 116.10(11) . 2_655 ? Zn1B O9 Zn1B 116.10(11) 3_665 2_655 ? Zn1B O9 Zn1 62.94(15) . 2_655 ? Zn1B O9 Zn1 69.75(14) 3_665 2_655 ? Zn1B O9 Zn1 172.2(2) 2_655 2_655 ? Zn1B O9 Zn1 69.75(14) . 3_665 ? Zn1B O9 Zn1 172.2(2) 3_665 3_665 ? Zn1B O9 Zn1 62.94(15) 2_655 3_665 ? Zn1 O9 Zn1 110.49(9) 2_655 3_665 ? Zn1B O9 Zn1 172.2(2) . . ? Zn1B O9 Zn1 62.94(15) 3_665 . ? Zn1B O9 Zn1 69.75(14) 2_655 . ? Zn1 O9 Zn1 110.49(9) 2_655 . ? Zn1 O9 Zn1 110.49(9) 3_665 . ? Zn1B O9 Zn2 78.46(17) . . ? Zn1B O9 Zn2 78.46(17) 3_665 . ? Zn1B O9 Zn2 78.46(17) 2_655 . ? Zn1 O9 Zn2 108.43(9) 2_655 . ? Zn1 O9 Zn2 108.43(9) 3_665 . ? Zn1 O9 Zn2 108.43(9) . . ? Zn1B O9 Zn2B 101.54(17) . . ? Zn1B O9 Zn2B 101.54(17) 3_665 . ? Zn1B O9 Zn2B 101.54(17) 2_655 . ? Zn1 O9 Zn2B 71.57(9) 2_655 . ? Zn1 O9 Zn2B 71.57(9) 3_665 . ? Zn1 O9 Zn2B 71.57(9) . . ? Zn2 O9 Zn2B 179.93(1) . . ? N2 N1 C7 115.8(3) . . ? N1 N2 C8 115.9(3) . . ? N3 N3 C21 113.1(4) 4_766 . ? O1B C1 O1 74.0(19) . . ? O1B C1 O2 84.6(17) . . ? O1 C1 O2 126.0(3) . . ? O1B C1 O2B 141(2) . . ? O1 C1 O2B 85.2(18) . . ? O2 C1 O2B 81.7(17) . . ? O1B C1 C2 115.9(17) . . ? O1 C1 C2 117.8(3) . . ? O2 C1 C2 116.2(3) . . ? O2B C1 C2 102.6(17) . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 118.0(3) . . ? C7 C2 C1 122.5(3) . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 119.9(3) . . ? C6 C7 N1 123.3(3) . . ? C2 C7 N1 116.7(3) . . ? C9 C8 C13 119.9(3) . . ? C9 C8 N2 122.5(3) . . ? C13 C8 N2 117.6(3) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 119.0(3) . . ? C12 C13 C14 118.0(3) . . ? C8 C13 C14 123.0(3) . . ? O3A C14 O3 71.9(4) . . ? O3A C14 O4 75.3(4) . . ? O3 C14 O4 122.5(4) . . ? O3A C14 O4A 129.4(4) . . ? O3 C14 O4A 84.5(4) . . ? O4 C14 O4A 81.5(4) . . ? O3A C14 C13 120.3(4) . . ? O3 C14 C13 119.2(3) . . ? O4 C14 C13 118.1(3) . . ? O4A C14 C13 110.3(4) . . ? O5 C15 O6B 70.7(18) . . ? O5 C15 O6 126.3(3) . . ? O6B C15 O6 81.6(17) . . ? O5 C15 O5B 71.0(17) . . ? O6B C15 O5B 115(3) . . ? O6 C15 O5B 80.9(18) . . ? O5 C15 C16 118.5(3) . . ? O6B C15 C16 119.9(17) . . ? O6 C15 C16 115.2(3) . . ? O5B C15 C16 124.5(17) . . ? C17 C16 C21 119.5(3) . . ? C17 C16 C15 118.2(3) . . ? C21 C16 C15 122.3(3) . . ? C18 C17 C16 120.9(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 119.9(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 119.2(3) . . ? C20 C21 N3 121.7(3) . . ? C16 C21 N3 118.8(3) . . ? O1 Zn1 O9 110.58(9) 2_655 . ? O1 Zn1 O2 109.96(12) 2_655 . ? O9 Zn1 O2 110.74(9) . . ? O1 Zn1 O5 104.84(12) 2_655 2_655 ? O9 Zn1 O5 112.85(12) . 2_655 ? O2 Zn1 O5 107.67(12) . 2_655 ? O1 Zn1 Zn2 122.29(8) 2_655 . ? O9 Zn1 Zn2 35.83(9) . . ? O2 Zn1 Zn2 124.58(8) . . ? O5 Zn1 Zn2 77.02(8) 2_655 . ? O6 Zn2 O6 107.34(8) 3_665 . ? O6 Zn2 O6 107.34(8) 3_665 2_655 ? O6 Zn2 O6 107.34(8) . 2_655 ? O6 Zn2 O9 111.53(8) 3_665 . ? O6 Zn2 O9 111.53(8) . . ? O6 Zn2 O9 111.53(8) 2_655 . ? O6 Zn2 Zn1 75.79(8) 3_665 2_655 ? O6 Zn2 Zn1 125.00(8) . 2_655 ? O6 Zn2 Zn1 124.44(8) 2_655 2_655 ? O9 Zn2 Zn1 35.752(11) . 2_655 ? O6 Zn2 Zn1 124.44(8) 3_665 3_665 ? O6 Zn2 Zn1 75.79(8) . 3_665 ? O6 Zn2 Zn1 125.00(8) 2_655 3_665 ? O9 Zn2 Zn1 35.737(11) . 3_665 ? Zn1 Zn2 Zn1 60.771(18) 2_655 3_665 ? O6 Zn2 Zn1 125.00(8) 3_665 . ? O6 Zn2 Zn1 124.44(8) . . ? O6 Zn2 Zn1 75.79(8) 2_655 . ? O9 Zn2 Zn1 35.722(11) . . ? Zn1 Zn2 Zn1 60.771(18) 2_655 . ? Zn1 Zn2 Zn1 60.771(18) 3_665 . ? C1 O1 Zn1 131.1(2) . 3_665 ? C1 O2 Zn1 130.3(2) . . ? C15 O5 Zn1 129.3(2) . 3_665 ? C15 O6 Zn2 131.6(2) . . ? O1B Zn1B O9 127.0(6) 3_665 . ? O1B Zn1B O6B 108.2(13) 3_665 3_665 ? O9 Zn1B O6B 109.2(8) . 3_665 ? O1B Zn1B O5B 105.3(15) 3_665 . ? O9 Zn1B O5B 100.3(9) . . ? O6B Zn1B O5B 104.2(15) 3_665 . ? O2B Zn2B O2B 110.9(7) 3_665 2_655 ? O2B Zn2B O2B 110.9(7) 3_665 . ? O2B Zn2B O2B 110.9(7) 2_655 . ? O2B Zn2B O9 108.0(8) 3_665 . ? O2B Zn2B O9 108.0(8) 2_655 . ? O2B Zn2B O9 108.0(8) . . ? C1 O1B Zn1B 115(2) . 2_655 ? C1 O2B Zn2B 127(2) . . ? C15 O5B Zn1B 142(3) . . ? C15 O6B Zn1B 135(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.250 _refine_diff_density_min -2.250 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 934517' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H10 Cd N2 O5' _chemical_formula_sum 'C14 H10 Cd N2 O5' _chemical_formula_weight 398.64 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 26.784(4) _cell_length_b 26.784(4) _cell_length_c 11.102(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6897.2(19) _cell_formula_units_Z 18 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9834 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7135 _exptl_absorpt_correction_T_max 0.7704 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2706 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0100 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2706 _reflns_number_gt 2571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A ' _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^)+(0.0221P)^2^+9.8176P] 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 2706 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0162 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0440 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Cd1 Cd 0.340129(6) 0.048549(5) 0.519617(11) 0.03177(6) Uani 1 1 d . . . C1 C 0.40592(8) 0.14783(8) 0.63549(15) 0.0328(4) Uani 1 1 d . . . C2 C 0.44346(8) 0.20692(8) 0.68640(16) 0.0338(4) Uani 1 1 d . . . C3 C 0.49317(9) 0.24471(9) 0.6242(2) 0.0477(5) Uani 1 1 d . . . H3 H 0.5020 0.2329 0.5526 0.057 Uiso 1 1 calc R . . C4 C 0.52975(11) 0.29961(10) 0.6670(2) 0.0609(6) Uani 1 1 d . . . H4 H 0.5630 0.3243 0.6246 0.073 Uiso 1 1 calc R . . C5 C 0.51688(11) 0.31774(10) 0.7726(2) 0.0585(6) Uani 1 1 d . . . H5 H 0.5418 0.3545 0.8020 0.070 Uiso 1 1 calc R . . C6 C 0.46709(9) 0.28153(9) 0.8351(2) 0.0450(5) Uani 1 1 d . . . H6 H 0.4583 0.2941 0.9057 0.054 Uiso 1 1 calc R . . C7 C 0.43023(8) 0.22635(8) 0.79218(16) 0.0331(4) Uani 1 1 d . . . C8 C 0.30589(8) 0.16926(8) 0.97950(16) 0.0337(4) Uani 1 1 d . . . C9 C 0.27719(9) 0.11021(9) 0.9606(2) 0.0446(5) Uani 1 1 d . . . H9 H 0.2872 0.0948 0.8960 0.054 Uiso 1 1 calc R . . C10 C 0.23355(11) 0.07428(9) 1.0386(2) 0.0569(6) Uani 1 1 d . . . H10 H 0.2142 0.0346 1.0265 0.068 Uiso 1 1 calc R . . C11 C 0.21873(11) 0.09708(11) 1.1341(2) 0.0627(7) Uani 1 1 d . . . H11 H 0.1897 0.0727 1.1868 0.075 Uiso 1 1 calc R . . C12 C 0.24690(10) 0.15596(10) 1.15184(19) 0.0511(5) Uani 1 1 d . . . H12 H 0.2367 0.1709 1.2168 0.061 Uiso 1 1 calc R . . C13 C 0.29030(8) 0.19318(8) 1.07401(16) 0.0353(4) Uani 1 1 d . . . C14 C 0.31931(8) 0.25674(8) 1.09753(15) 0.0338(4) Uani 1 1 d . . . N1 N 0.38269(7) 0.18753(6) 0.86610(13) 0.0332(3) Uani 1 1 d . . . N2 N 0.35134(7) 0.20716(6) 0.89890(13) 0.0326(3) Uani 1 1 d . . . O1 O 0.42364(6) 0.13439(6) 0.54269(12) 0.0407(3) Uani 1 1 d . . . O2 O 0.35836(6) 0.11386(6) 0.68437(11) 0.0382(3) Uani 1 1 d . . . O3 O 0.34232(6) 0.29274(5) 1.01303(11) 0.0389(3) Uani 1 1 d . . . O4 O 0.32098(7) 0.27457(6) 1.20190(13) 0.0524(4) Uani 1 1 d . . . O1W O 0.25509(6) -0.02281(6) 0.57399(12) 0.0434(3) Uani 1 1 d . . . H1WA H 0.2559 -0.0341 0.6452 0.065 Uiso 1 1 d R . . H1WB H 0.2362 -0.0487 0.5218 0.065 Uiso 1 1 d 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 Cd1 0.03836(9) 0.03088(8) 0.02555(9) -0.00041(5) -0.00021(5) 0.01692(6) C1 0.0383(10) 0.0342(10) 0.0315(9) -0.0004(7) -0.0043(8) 0.0224(9) C2 0.0371(10) 0.0318(9) 0.0366(9) -0.0002(7) -0.0022(8) 0.0201(8) C3 0.0483(12) 0.0408(11) 0.0505(12) -0.0010(9) 0.0101(10) 0.0196(10) C4 0.0511(14) 0.0394(12) 0.0775(17) 0.0006(11) 0.0181(12) 0.0116(11) C5 0.0524(14) 0.0318(11) 0.0806(17) -0.0113(11) 0.0042(12) 0.0131(10) C6 0.0489(12) 0.0350(10) 0.0536(12) -0.0098(9) -0.0009(9) 0.0229(10) C7 0.0370(10) 0.0315(9) 0.0368(9) -0.0008(7) -0.0030(7) 0.0217(8) C8 0.0376(10) 0.0302(9) 0.0336(9) 0.0039(7) -0.0030(7) 0.0172(8) C9 0.0479(12) 0.0333(10) 0.0532(12) -0.0003(9) -0.0041(9) 0.0207(9) C10 0.0560(14) 0.0298(11) 0.0729(16) 0.0091(10) -0.0006(12) 0.0124(10) C11 0.0578(15) 0.0449(13) 0.0637(15) 0.0180(11) 0.0148(12) 0.0094(11) C12 0.0538(13) 0.0472(12) 0.0420(11) 0.0080(9) 0.0121(10) 0.0175(11) C13 0.0395(10) 0.0334(10) 0.0310(9) 0.0052(7) 0.0004(7) 0.0167(8) C14 0.0361(10) 0.0379(10) 0.0283(9) 0.0006(7) 0.0005(7) 0.0192(8) N1 0.0410(9) 0.0324(8) 0.0302(7) -0.0025(6) -0.0027(6) 0.0213(7) N2 0.0382(8) 0.0302(8) 0.0315(7) -0.0014(6) -0.0011(6) 0.0186(7) O1 0.0446(8) 0.0410(8) 0.0362(7) -0.0070(6) 0.0025(6) 0.0211(6) O2 0.0397(7) 0.0342(7) 0.0371(7) -0.0032(5) 0.0013(6) 0.0158(6) O3 0.0520(8) 0.0295(7) 0.0268(6) 0.0002(5) 0.0008(6) 0.0140(6) O4 0.0778(11) 0.0459(8) 0.0296(7) -0.0006(6) 0.0102(7) 0.0280(8) O1W 0.0422(8) 0.0357(7) 0.0386(7) 0.0043(6) -0.0099(6) 0.0091(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 Cd1 O1W 2.2026(14) . ? Cd1 O3 2.2427(13) 13_556 ? Cd1 O1 2.2830(14) . ? Cd1 O2 2.4061(13) . ? Cd1 O3 2.4216(13) 18_546 ? Cd1 O4 2.4266(15) 18_546 ? Cd1 N2 2.6534(15) 13_556 ? Cd1 C1 2.6731(19) . ? C1 O2 1.259(2) . ? C1 O1 1.260(2) . ? C1 C2 1.498(3) . ? C2 C3 1.388(3) . ? C2 C7 1.400(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9300 . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 C6 1.381(3) . ? C5 H5 0.9300 . ? C6 C7 1.388(3) . ? C6 H6 0.9300 . ? C7 N1 1.433(2) . ? C8 C9 1.386(3) . ? C8 C13 1.397(3) . ? C8 N2 1.441(2) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.377(4) . ? C10 H10 0.9300 . ? C11 C12 1.380(3) . ? C11 H11 0.9300 . ? C12 C13 1.390(3) . ? C12 H12 0.9300 . ? C13 C14 1.499(3) . ? C14 O4 1.246(2) . ? C14 O3 1.263(2) . ? N1 N2 1.247(2) . ? N2 Cd1 2.6534(15) 13_556 ? O3 Cd1 2.2427(13) 13_556 ? O3 Cd1 2.4215(13) 17_556 ? O4 Cd1 2.4265(15) 17_556 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? 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 O1W Cd1 O3 97.12(5) . 13_556 ? O1W Cd1 O1 155.57(5) . . ? O3 Cd1 O1 104.46(5) 13_556 . ? O1W Cd1 O2 99.70(5) . . ? O3 Cd1 O2 141.18(5) 13_556 . ? O1 Cd1 O2 56.08(4) . . ? O1W Cd1 O3 87.83(5) . 18_546 ? O3 Cd1 O3 132.27(4) 13_556 18_546 ? O1 Cd1 O3 86.10(5) . 18_546 ? O2 Cd1 O3 83.26(5) . 18_546 ? O1W Cd1 O4 95.48(6) . 18_546 ? O3 Cd1 O4 79.26(5) 13_556 18_546 ? O1 Cd1 O4 99.65(5) . 18_546 ? O2 Cd1 O4 132.96(5) . 18_546 ? O3 Cd1 O4 53.01(5) 18_546 18_546 ? O1W Cd1 N2 102.84(5) . 13_556 ? O3 Cd1 N2 67.27(5) 13_556 13_556 ? O1 Cd1 N2 75.75(5) . 13_556 ? O2 Cd1 N2 74.96(5) . 13_556 ? O3 Cd1 N2 157.01(5) 18_546 13_556 ? O4 Cd1 N2 143.35(5) 18_546 13_556 ? O1W Cd1 C1 127.78(5) . . ? O3 Cd1 C1 124.65(5) 13_556 . ? O1 Cd1 C1 28.06(5) . . ? O2 Cd1 C1 28.08(5) . . ? O3 Cd1 C1 85.34(5) 18_546 . ? O4 Cd1 C1 119.81(5) 18_546 . ? N2 Cd1 C1 71.99(5) 13_556 . ? O2 C1 O1 122.37(17) . . ? O2 C1 C2 120.20(16) . . ? O1 C1 C2 117.43(16) . . ? O2 C1 Cd1 64.09(9) . . ? O1 C1 Cd1 58.49(9) . . ? C2 C1 Cd1 173.21(12) . . ? C3 C2 C7 118.34(17) . . ? C3 C2 C1 118.39(17) . . ? C7 C2 C1 123.25(17) . . ? C4 C3 C2 121.1(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 119.92(19) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.40(18) . . ? C6 C7 N1 118.51(17) . . ? C2 C7 N1 120.60(16) . . ? C9 C8 C13 120.97(18) . . ? C9 C8 N2 120.07(17) . . ? C13 C8 N2 118.94(16) . . ? C10 C9 C8 119.5(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.9(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 118.18(18) . . ? C12 C13 C14 118.60(18) . . ? C8 C13 C14 123.19(17) . . ? O4 C14 O3 119.20(17) . . ? O4 C14 C13 119.77(16) . . ? O3 C14 C13 121.04(16) . . ? N2 N1 C7 113.75(14) . . ? N1 N2 C8 113.19(15) . . ? N1 N2 Cd1 135.35(12) . 13_556 ? C8 N2 Cd1 108.61(11) . 13_556 ? C1 O1 Cd1 93.45(11) . . ? C1 O2 Cd1 87.83(10) . . ? C14 O3 Cd1 131.55(12) . 13_556 ? C14 O3 Cd1 93.63(11) . 17_556 ? Cd1 O3 Cd1 131.96(6) 13_556 17_556 ? C14 O4 Cd1 93.86(12) . 17_556 ? Cd1 O1W H1WA 111.4 . . ? Cd1 O1W H1WB 117.2 . . ? H1WA O1W H1WB 117.1 . . ? 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 O1W H1WA O4 0.85 1.85 2.682(2) 167.3 11_557 O1W H1WB O2 0.85 2.11 2.911(2) 156.2 8_544 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.214 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.054 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.003 292 41 ' ' 2 0.333 0.667 0.671 290 41 ' ' 3 0.667 0.333 0.337 290 41 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 934515' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H16 N4 O9 Pb3' _chemical_formula_sum 'C28 H16 N4 O9 Pb3' _chemical_formula_weight 1174.02 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' 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' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8805(4) _cell_length_b 12.1427(5) _cell_length_c 13.0895(6) _cell_angle_alpha 89.271(3) _cell_angle_beta 70.875(4) _cell_angle_gamma 80.560(3) _cell_volume 1462.24(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8895 _cell_measurement_theta_min 2.9910 _cell_measurement_theta_max 28.9380 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2 -15 -8 0.1078 -1.5407 -15.0761 -8.2287 0.5028 -0.4769 0.7210 -14 0 -5 0.0441 -13.7577 -0.2751 -5.1802 0.7169 -0.1719 -0.6756 -8 0 11 0.0793 -7.9523 0.2544 10.6366 -0.0657 -0.4996 -0.8637 14 -1 9 0.0400 13.5032 -0.6473 8.5100 -0.8138 0.0211 0.5808 -4 15 -3 0.0070 -4.0482 15.3419 -2.6626 0.0913 0.6947 -0.7134 13 -1 7 0.0338 13.4728 -1.3330 7.4974 -0.7702 0.0200 0.6375 5 6 -13 0.0623 5.3845 5.8144 -13.1841 0.1914 0.7980 0.5714 -4 10 10 0.0223 -4.0613 10.2016 9.9192 -0.2943 0.0707 -0.9531 5 -15 1 0.0479 4.8826 -14.7545 1.2205 -0.0794 -0.6040 0.7930 9 -4 16 0.0612 8.6582 -3.6598 16.3613 -0.8689 -0.4714 0.1220 13 -3 10 0.0614 12.6606 -2.9816 9.9286 -0.8065 -0.1496 0.5641 -1 11 12 0.0506 -1.4719 10.9693 11.6943 -0.4646 0.1114 -0.8785 5 -10 -9 0.0727 4.9295 -9.8453 -9.2183 0.2325 -0.0557 0.9710 13 7 5 0.0183 13.4659 6.6741 4.9240 -0.7628 0.4677 0.4366 -3 -2 15 0.0523 -3.3693 -1.7805 15.3909 -0.3883 -0.6335 -0.6643 -5 0 14 0.0571 -4.5839 0.3432 14.2856 -0.3246 -0.5298 -0.7792 -14 -1 -6 0.0653 -13.8594 -1.0956 -6.1274 0.7624 -0.1829 -0.6207 -12 6 -7 0.0278 -12.1913 5.5456 -7.3504 0.6718 0.1992 -0.7134 1 16 6 0.0255 0.8228 15.9539 5.7361 -0.3970 0.5774 -0.7135 13 -4 8 0.0523 12.6650 -3.9282 8.0693 -0.7320 -0.1359 0.6609 1 -1 -17 0.0441 1.0259 -1.3460 -16.7217 0.5579 0.4762 0.6747 14 0 4 0.0070 13.6386 -0.3230 4.4720 -0.6814 0.1634 0.7134 -3 -17 -3 0.0673 -2.6499 -16.7886 -3.3853 0.3944 -0.7304 0.5502 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 17.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2596 _exptl_absorpt_correction_T_max 0.4714 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18011 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_unetI/netI 0.0250 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5159 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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^)+(0.0195P)^2^+0.3550P] 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 5159 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0423 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.484873(18) 0.359626(14) 0.460191(14) 0.02877(5) Uani 1 1 d . . . Pb2 Pb 0.804816(18) 0.410205(15) 0.565576(14) 0.03035(5) Uani 1 1 d . . . Pb3 Pb 0.429786(19) 0.407704(15) 0.746294(14) 0.03279(6) Uani 1 1 d . . . C1 C 0.7675(5) 0.3067(4) 0.2898(4) 0.0385(12) Uani 1 1 d . . . C2 C 0.8782(5) 0.2133(4) 0.2187(4) 0.0385(12) Uani 1 1 d . . . C3 C 0.8431(7) 0.1076(5) 0.2338(5) 0.0559(16) Uani 1 1 d . . . H3 H 0.7569 0.0972 0.2864 0.067 Uiso 1 1 calc R . . C4 C 0.9351(7) 0.0171(5) 0.1717(6) 0.072(2) Uani 1 1 d . . . H4 H 0.9100 -0.0537 0.1819 0.086 Uiso 1 1 calc R . . C5 C 1.0627(8) 0.0313(5) 0.0952(6) 0.077(2) Uani 1 1 d . . . H5 H 1.1248 -0.0302 0.0545 0.092 Uiso 1 1 calc R . . C6 C 1.1004(7) 0.1354(5) 0.0778(5) 0.0619(17) Uani 1 1 d . . . H6 H 1.1866 0.1445 0.0244 0.074 Uiso 1 1 calc R . . C7 C 1.0092(6) 0.2277(4) 0.1404(4) 0.0418(13) Uani 1 1 d . . . C8 C 1.0306(5) 0.5141(4) 0.1586(4) 0.0371(12) Uani 1 1 d . . . C9 C 1.1210(5) 0.5394(5) 0.0567(4) 0.0455(14) Uani 1 1 d . . . H9 H 1.1608 0.4841 0.0016 0.055 Uiso 1 1 calc R . . C10 C 1.1502(6) 0.6446(5) 0.0388(5) 0.0557(16) Uani 1 1 d . . . H10 H 1.2082 0.6618 -0.0293 0.067 Uiso 1 1 calc R . . C11 C 1.0942(6) 0.7266(5) 0.1210(5) 0.0675(19) Uani 1 1 d . . . H11 H 1.1178 0.7978 0.1089 0.081 Uiso 1 1 calc R . . C12 C 1.0027(6) 0.7028(5) 0.2220(5) 0.0560(16) Uani 1 1 d . . . H12 H 0.9650 0.7581 0.2772 0.067 Uiso 1 1 calc R . . C13 C 0.9682(5) 0.5972(4) 0.2398(4) 0.0358(12) Uani 1 1 d . . . C14 C 0.8711(5) 0.5684(4) 0.3495(3) 0.0287(10) Uani 1 1 d . . . C15 C 0.6024(6) 0.1849(4) 0.6523(4) 0.0352(11) Uani 1 1 d . . . C16 C 0.6878(5) 0.0704(4) 0.6110(4) 0.0351(11) Uani 1 1 d . . . C17 C 0.8077(6) 0.0307(4) 0.6435(4) 0.0458(13) Uani 1 1 d . . . H17 H 0.8333 0.0762 0.6883 0.055 Uiso 1 1 calc R . . C18 C 0.8898(6) -0.0749(5) 0.6105(5) 0.0557(15) Uani 1 1 d . . . H18 H 0.9692 -0.0994 0.6331 0.067 Uiso 1 1 calc R . . C19 C 0.8533(6) -0.1424(5) 0.5448(5) 0.0530(15) Uani 1 1 d . . . H19 H 0.9081 -0.2132 0.5230 0.064 Uiso 1 1 calc R . . C20 C 0.7354(6) -0.1070(4) 0.5102(4) 0.0451(13) Uani 1 1 d . . . H20 H 0.7119 -0.1535 0.4650 0.054 Uiso 1 1 calc R . . C21 C 0.6528(5) -0.0020(4) 0.5433(4) 0.0351(11) Uani 1 1 d . . . C22 C 0.6743(5) 0.5737(4) 0.7437(4) 0.0298(11) Uani 1 1 d . . . C23 C 0.6034(5) 0.6598(4) 0.8350(4) 0.0323(11) Uani 1 1 d . . . C24 C 0.6168(6) 0.7714(4) 0.8172(5) 0.0511(15) Uani 1 1 d . . . H24 H 0.6678 0.7925 0.7486 0.061 Uiso 1 1 calc R . . C25 C 0.5542(7) 0.8514(5) 0.9018(5) 0.0665(19) Uani 1 1 d . . . H25 H 0.5629 0.9259 0.8892 0.080 Uiso 1 1 calc R . . C26 C 0.4799(7) 0.8219(5) 1.0033(5) 0.0585(17) Uani 1 1 d . . . H26 H 0.4391 0.8762 1.0593 0.070 Uiso 1 1 calc R . . C27 C 0.4654(5) 0.7123(4) 1.0230(4) 0.0425(13) Uani 1 1 d . . . H27 H 0.4151 0.6926 1.0923 0.051 Uiso 1 1 calc R . . C28 C 0.5258(5) 0.6307(4) 0.9396(4) 0.0329(11) Uani 1 1 d . . . N1 N 1.0566(5) 0.3312(4) 0.1151(3) 0.0474(12) Uani 1 1 d . . . N2 N 0.9893(4) 0.4077(4) 0.1845(3) 0.0416(11) Uani 1 1 d . . . N3 N 0.5371(4) 0.0367(3) 0.4999(3) 0.0370(10) Uani 1 1 d . . . N4 N 0.4915(4) 0.5194(3) 0.9574(3) 0.0327(9) Uani 1 1 d . . . O1 O 0.7583(4) 0.3090(3) 0.3889(3) 0.0483(9) Uani 1 1 d . . . O2 O 0.6797(4) 0.3660(3) 0.2519(3) 0.0455(9) Uani 1 1 d . . . O3 O 0.9283(4) 0.5374(3) 0.4190(3) 0.0439(9) Uani 1 1 d . . . O4 O 0.7362(3) 0.5811(3) 0.3661(3) 0.0396(8) Uani 1 1 d . . . O5 O 0.6618(4) 0.2501(3) 0.6912(3) 0.0482(9) Uani 1 1 d . . . O6 O 0.4773(4) 0.2140(3) 0.6457(3) 0.0500(10) Uani 1 1 d . . . O7 O 0.6736(3) 0.4715(3) 0.7619(2) 0.0356(8) Uani 1 1 d . . . O8 O 0.7325(4) 0.6061(3) 0.6495(3) 0.0408(8) Uani 1 1 d . . . O9 O 0.5596(3) 0.4535(2) 0.5819(2) 0.0237(6) 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 0.02827(10) 0.03017(10) 0.03094(10) -0.00115(7) -0.01415(8) -0.00423(7) Pb2 0.02344(10) 0.03531(11) 0.03336(10) -0.00164(8) -0.01183(8) -0.00262(7) Pb3 0.03125(10) 0.04075(11) 0.02648(10) 0.00148(8) -0.00839(8) -0.00880(8) C1 0.031(3) 0.039(3) 0.044(3) -0.006(2) -0.009(2) -0.010(2) C2 0.037(3) 0.042(3) 0.037(3) -0.008(2) -0.017(2) 0.001(2) C3 0.061(4) 0.047(4) 0.055(4) -0.004(3) -0.013(3) -0.008(3) C4 0.076(5) 0.044(4) 0.084(5) -0.008(3) -0.014(4) -0.005(3) C5 0.084(5) 0.045(4) 0.081(5) -0.021(3) -0.011(4) 0.015(4) C6 0.055(4) 0.064(4) 0.054(4) -0.018(3) -0.009(3) 0.007(3) C7 0.042(3) 0.044(3) 0.038(3) -0.002(2) -0.015(3) -0.001(2) C8 0.031(3) 0.051(3) 0.036(3) 0.004(2) -0.019(2) -0.011(2) C9 0.031(3) 0.073(4) 0.031(3) 0.004(3) -0.007(2) -0.008(3) C10 0.033(3) 0.079(5) 0.047(3) 0.027(3) -0.005(3) -0.009(3) C11 0.053(4) 0.047(4) 0.084(5) 0.023(3) 0.001(4) -0.004(3) C12 0.050(4) 0.043(3) 0.059(4) 0.004(3) 0.003(3) -0.006(3) C13 0.022(2) 0.048(3) 0.037(3) 0.008(2) -0.009(2) -0.006(2) C14 0.025(3) 0.032(3) 0.030(3) -0.005(2) -0.010(2) -0.006(2) C15 0.046(3) 0.033(3) 0.032(3) 0.004(2) -0.018(2) -0.009(2) C16 0.037(3) 0.033(3) 0.040(3) 0.006(2) -0.018(2) -0.008(2) C17 0.049(3) 0.045(3) 0.055(3) 0.008(3) -0.032(3) -0.012(3) C18 0.044(3) 0.054(4) 0.072(4) 0.013(3) -0.027(3) 0.000(3) C19 0.045(3) 0.041(3) 0.067(4) -0.003(3) -0.015(3) 0.005(3) C20 0.043(3) 0.033(3) 0.055(3) -0.006(2) -0.012(3) -0.003(2) C21 0.033(3) 0.033(3) 0.040(3) 0.006(2) -0.012(2) -0.009(2) C22 0.026(2) 0.037(3) 0.031(3) -0.003(2) -0.016(2) -0.006(2) C23 0.038(3) 0.031(3) 0.033(3) 0.001(2) -0.017(2) -0.010(2) C24 0.066(4) 0.040(3) 0.050(3) 0.004(3) -0.017(3) -0.018(3) C25 0.090(5) 0.029(3) 0.077(5) -0.003(3) -0.019(4) -0.020(3) C26 0.069(4) 0.040(3) 0.063(4) -0.024(3) -0.016(3) -0.007(3) C27 0.040(3) 0.048(3) 0.041(3) -0.009(2) -0.015(2) -0.006(2) C28 0.033(3) 0.033(3) 0.036(3) -0.002(2) -0.016(2) -0.005(2) N1 0.040(3) 0.055(3) 0.041(3) -0.009(2) -0.009(2) 0.002(2) N2 0.034(2) 0.056(3) 0.034(2) -0.002(2) -0.007(2) -0.014(2) N3 0.040(2) 0.034(2) 0.041(2) -0.0035(19) -0.019(2) -0.0075(18) N4 0.031(2) 0.036(2) 0.030(2) -0.0048(17) -0.0093(19) -0.0040(18) O1 0.043(2) 0.064(3) 0.032(2) -0.0127(17) -0.0065(17) -0.0064(18) O2 0.037(2) 0.043(2) 0.052(2) -0.0084(17) -0.0130(18) 0.0027(17) O3 0.036(2) 0.067(3) 0.0364(19) 0.0147(17) -0.0197(16) -0.0146(17) O4 0.0212(17) 0.061(2) 0.0362(19) -0.0042(16) -0.0111(15) -0.0021(16) O5 0.062(2) 0.039(2) 0.058(2) -0.0051(17) -0.037(2) -0.0111(18) O6 0.047(2) 0.037(2) 0.070(3) -0.0079(18) -0.029(2) 0.0015(17) O7 0.045(2) 0.032(2) 0.0318(18) -0.0013(14) -0.0152(16) -0.0070(15) O8 0.045(2) 0.042(2) 0.036(2) 0.0011(16) -0.0119(17) -0.0131(17) O9 0.0193(15) 0.0288(16) 0.0234(15) -0.0013(12) -0.0083(12) -0.0019(12) _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 O9 2.334(3) 2_666 ? Pb1 O9 2.339(3) . ? Pb1 O1 2.523(3) . ? Pb1 O4 2.595(3) 2_666 ? Pb1 Pb3 3.6438(3) . ? Pb1 Pb1 3.6641(4) 2_666 ? Pb2 O9 2.332(3) . ? Pb2 O8 2.524(3) . ? Pb2 O7 2.528(3) . ? Pb2 O3 2.562(3) . ? Pb2 Pb3 3.6903(3) . ? Pb3 O9 2.232(3) . ? Pb3 O4 2.525(3) 2_666 ? Pb3 O6 2.607(3) . ? Pb3 O5 2.637(4) . ? Pb3 O7 2.717(3) . ? C1 O1 1.270(6) . ? C1 O2 1.259(6) . ? C1 C2 1.517(6) . ? C2 C3 1.379(7) . ? C2 C7 1.398(7) . ? C3 C4 1.381(7) . ? C3 H3 0.9300 . ? C4 C5 1.364(9) . ? C4 H4 0.9300 . ? C5 C6 1.371(9) . ? C5 H5 0.9300 . ? C6 C7 1.396(7) . ? C6 H6 0.9300 . ? C7 N1 1.410(7) . ? C8 C13 1.386(6) . ? C8 N2 1.422(6) . ? C8 C9 1.404(6) . ? C9 C10 1.356(8) . ? C9 H9 0.9300 . ? C10 C11 1.383(8) . ? C10 H10 0.9300 . ? C11 C12 1.393(8) . ? C11 H11 0.9300 . ? C12 C13 1.378(7) . ? C12 H12 0.9300 . ? C13 C14 1.516(6) . ? C14 O3 1.244(5) . ? C14 O4 1.261(5) . ? C15 O5 1.260(6) . ? C15 O6 1.260(6) . ? C15 C16 1.508(6) . ? C16 C17 1.398(7) . ? C16 C21 1.413(7) . ? C17 C18 1.390(7) . ? C17 H17 0.9300 . ? C18 C19 1.364(8) . ? C18 H18 0.9300 . ? C19 C20 1.387(8) . ? C19 H19 0.9300 . ? C20 C21 1.386(6) . ? C20 H20 0.9300 . ? C21 N3 1.446(6) . ? C22 O7 1.261(5) . ? C22 O8 1.266(5) . ? C22 C23 1.502(6) . ? C23 C24 1.393(7) . ? C23 C28 1.406(6) . ? C24 C25 1.391(7) . ? C24 H24 0.9300 . ? C25 C26 1.366(8) . ? C25 H25 0.9300 . ? C26 C27 1.374(7) . ? C26 H26 0.9300 . ? C27 C28 1.392(6) . ? C27 H27 0.9300 . ? C28 N4 1.444(6) . ? N1 N2 1.246(5) . ? N3 N3 1.243(7) 2_656 ? N4 N4 1.255(7) 2_667 ? O4 Pb3 2.525(3) 2_666 ? O4 Pb1 2.595(3) 2_666 ? O9 Pb1 2.334(3) 2_666 ? 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 O9 Pb1 O9 76.72(11) 2_666 . ? O9 Pb1 O1 103.69(11) 2_666 . ? O9 Pb1 O1 76.33(10) . . ? O9 Pb1 O4 84.28(10) 2_666 2_666 ? O9 Pb1 O4 71.10(10) . 2_666 ? O1 Pb1 O4 143.67(11) . 2_666 ? O9 Pb1 Pb3 97.29(6) 2_666 . ? O9 Pb1 Pb3 36.13(7) . . ? O1 Pb1 Pb3 99.82(8) . . ? O4 Pb1 Pb3 43.86(7) 2_666 . ? O9 Pb1 Pb1 38.42(7) 2_666 2_666 ? O9 Pb1 Pb1 38.31(7) . 2_666 ? O1 Pb1 Pb1 89.99(8) . 2_666 ? O4 Pb1 Pb1 74.32(8) 2_666 2_666 ? Pb3 Pb1 Pb1 64.225(6) . 2_666 ? O9 Pb2 O8 77.23(10) . . ? O9 Pb2 O7 74.64(10) . . ? O8 Pb2 O7 51.79(10) . . ? O9 Pb2 O3 104.16(10) . . ? O8 Pb2 O3 73.45(11) . . ? O7 Pb2 O3 124.51(10) . . ? O9 Pb2 Pb3 35.14(7) . . ? O8 Pb2 Pb3 78.13(7) . . ? O7 Pb2 Pb3 47.41(7) . . ? O3 Pb2 Pb3 135.37(8) . . ? O9 Pb3 O4 74.13(10) . 2_666 ? O9 Pb3 O6 81.63(11) . . ? O4 Pb3 O6 72.19(11) 2_666 . ? O9 Pb3 O5 76.62(11) . . ? O4 Pb3 O5 117.53(10) 2_666 . ? O6 Pb3 O5 49.67(11) . . ? O9 Pb3 O7 72.44(10) . . ? O4 Pb3 O7 144.52(10) 2_666 . ? O6 Pb3 O7 113.78(10) . . ? O5 Pb3 O7 65.25(10) . . ? O9 Pb3 Pb1 38.18(7) . . ? O4 Pb3 Pb1 45.41(7) 2_666 . ? O6 Pb3 Pb1 53.77(9) . . ? O5 Pb3 Pb1 79.02(8) . . ? O7 Pb3 Pb1 107.80(6) . . ? O9 Pb3 Pb2 36.97(7) . . ? O4 Pb3 Pb2 109.04(7) 2_666 . ? O6 Pb3 Pb2 81.26(8) . . ? O5 Pb3 Pb2 48.91(8) . . ? O7 Pb3 Pb2 43.23(6) . . ? Pb1 Pb3 Pb2 65.607(6) . . ? O1 C1 O2 124.3(4) . . ? O1 C1 C2 115.9(5) . . ? O2 C1 C2 119.0(5) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 115.9(5) . . ? C7 C2 C1 124.9(5) . . ? C4 C3 C2 120.5(6) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 120.2(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.7(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.9(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 119.5(5) . . ? C6 C7 N1 115.5(5) . . ? C2 C7 N1 125.0(4) . . ? C13 C8 N2 115.7(4) . . ? C13 C8 C9 120.0(5) . . ? N2 C8 C9 124.2(4) . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.4(5) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 119.6(5) . . ? C12 C13 C14 121.0(4) . . ? C8 C13 C14 119.3(4) . . ? O3 C14 O4 123.8(4) . . ? O3 C14 C13 118.2(4) . . ? O4 C14 C13 117.9(4) . . ? O5 C15 O6 121.9(5) . . ? O5 C15 C16 117.7(5) . . ? O6 C15 C16 120.5(4) . . ? C17 C16 C21 117.1(5) . . ? C17 C16 C15 118.5(5) . . ? C21 C16 C15 124.4(5) . . ? C16 C17 C18 121.8(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 119.7(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.7(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 120.9(5) . . ? C20 C21 N3 118.9(4) . . ? C16 C21 N3 120.0(4) . . ? O7 C22 O8 121.6(4) . . ? O7 C22 C23 119.7(4) . . ? O8 C22 C23 118.7(4) . . ? C24 C23 C28 118.5(4) . . ? C24 C23 C22 119.7(4) . . ? C28 C23 C22 121.8(4) . . ? C23 C24 C25 120.1(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C23 120.1(4) . . ? C27 C28 N4 119.4(4) . . ? C23 C28 N4 119.9(4) . . ? N2 N1 C7 113.9(4) . . ? N1 N2 C8 115.0(4) . . ? N3 N3 C21 111.9(5) 2_656 . ? N4 N4 C28 112.7(5) 2_667 . ? C1 O1 Pb1 95.2(3) . . ? C14 O3 Pb2 118.8(3) . . ? C14 O4 Pb3 137.3(3) . 2_666 ? C14 O4 Pb1 131.3(3) . 2_666 ? Pb3 O4 Pb1 90.74(10) 2_666 2_666 ? C15 O5 Pb3 93.4(3) . . ? C15 O6 Pb3 94.8(3) . . ? C22 O7 Pb2 93.3(3) . . ? C22 O7 Pb3 111.1(3) . . ? Pb2 O7 Pb3 89.37(9) . . ? C22 O8 Pb2 93.4(3) . . ? Pb3 O9 Pb2 107.89(11) . . ? Pb3 O9 Pb1 116.61(11) . 2_666 ? Pb2 O9 Pb1 107.19(11) . 2_666 ? Pb3 O9 Pb1 105.69(11) . . ? Pb2 O9 Pb1 116.55(11) . . ? Pb1 O9 Pb1 103.28(11) 2_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Pb1 Pb3 O9 -55.40(16) 2_666 . . . ? O1 Pb1 Pb3 O9 49.93(14) . . . . ? O4 Pb1 Pb3 O9 -129.25(16) 2_666 . . . ? Pb1 Pb1 Pb3 O9 -35.27(11) 2_666 . . . ? O9 Pb1 Pb3 O4 73.85(13) 2_666 . . 2_666 ? O9 Pb1 Pb3 O4 129.25(16) . . . 2_666 ? O1 Pb1 Pb3 O4 179.18(14) . . . 2_666 ? Pb1 Pb1 Pb3 O4 93.98(11) 2_666 . . 2_666 ? O9 Pb1 Pb3 O6 174.80(12) 2_666 . . . ? O9 Pb1 Pb3 O6 -129.80(15) . . . . ? O1 Pb1 Pb3 O6 -79.87(13) . . . . ? O4 Pb1 Pb3 O6 100.95(15) 2_666 . . . ? Pb1 Pb1 Pb3 O6 -165.07(10) 2_666 . . . ? O9 Pb1 Pb3 O5 -137.66(10) 2_666 . . . ? O9 Pb1 Pb3 O5 -82.26(14) . . . . ? O1 Pb1 Pb3 O5 -32.34(12) . . . . ? O4 Pb1 Pb3 O5 148.48(14) 2_666 . . . ? Pb1 Pb1 Pb3 O5 -117.53(8) 2_666 . . . ? O9 Pb1 Pb3 O7 -78.34(10) 2_666 . . . ? O9 Pb1 Pb3 O7 -22.95(13) . . . . ? O1 Pb1 Pb3 O7 26.98(11) . . . . ? O4 Pb1 Pb3 O7 -152.20(13) 2_666 . . . ? Pb1 Pb1 Pb3 O7 -58.22(7) 2_666 . . . ? O9 Pb1 Pb3 Pb2 -87.99(7) 2_666 . . . ? O9 Pb1 Pb3 Pb2 -32.59(11) . . . . ? O1 Pb1 Pb3 Pb2 17.33(9) . . . . ? O4 Pb1 Pb3 Pb2 -161.84(11) 2_666 . . . ? Pb1 Pb1 Pb3 Pb2 -67.862(6) 2_666 . . . ? O8 Pb2 Pb3 O9 84.62(14) . . . . ? O7 Pb2 Pb3 O9 132.92(15) . . . . ? O3 Pb2 Pb3 O9 33.47(16) . . . . ? O9 Pb2 Pb3 O4 20.04(14) . . . 2_666 ? O8 Pb2 Pb3 O4 104.66(12) . . . 2_666 ? O7 Pb2 Pb3 O4 152.95(13) . . . 2_666 ? O3 Pb2 Pb3 O4 53.50(14) . . . 2_666 ? O9 Pb2 Pb3 O6 87.68(14) . . . . ? O8 Pb2 Pb3 O6 172.30(12) . . . . ? O7 Pb2 Pb3 O6 -139.41(13) . . . . ? O3 Pb2 Pb3 O6 121.14(14) . . . . ? O9 Pb2 Pb3 O5 130.38(15) . . . . ? O8 Pb2 Pb3 O5 -144.99(13) . . . . ? O7 Pb2 Pb3 O5 -96.70(14) . . . . ? O3 Pb2 Pb3 O5 163.85(14) . . . . ? O9 Pb2 Pb3 O7 -132.92(15) . . . . ? O8 Pb2 Pb3 O7 -48.29(13) . . . . ? O3 Pb2 Pb3 O7 -99.45(15) . . . . ? O9 Pb2 Pb3 Pb1 33.61(11) . . . . ? O8 Pb2 Pb3 Pb1 118.24(8) . . . . ? O7 Pb2 Pb3 Pb1 166.53(10) . . . . ? O3 Pb2 Pb3 Pb1 67.08(11) . . . . ? O1 C1 C2 C3 72.3(6) . . . . ? O2 C1 C2 C3 -98.4(6) . . . . ? O1 C1 C2 C7 -108.4(6) . . . . ? O2 C1 C2 C7 80.9(7) . . . . ? C7 C2 C3 C4 -0.8(9) . . . . ? C1 C2 C3 C4 178.6(6) . . . . ? C2 C3 C4 C5 0.7(11) . . . . ? C3 C4 C5 C6 -1.1(12) . . . . ? C4 C5 C6 C7 1.4(11) . . . . ? C5 C6 C7 C2 -1.5(9) . . . . ? C5 C6 C7 N1 -179.1(6) . . . . ? C3 C2 C7 C6 1.2(8) . . . . ? C1 C2 C7 C6 -178.2(5) . . . . ? C3 C2 C7 N1 178.6(5) . . . . ? C1 C2 C7 N1 -0.8(8) . . . . ? C13 C8 C9 C10 1.7(8) . . . . ? N2 C8 C9 C10 177.7(5) . . . . ? C8 C9 C10 C11 1.5(9) . . . . ? C9 C10 C11 C12 -2.5(10) . . . . ? C10 C11 C12 C13 0.1(10) . . . . ? C11 C12 C13 C8 3.1(9) . . . . ? C11 C12 C13 C14 178.9(5) . . . . ? N2 C8 C13 C12 179.7(5) . . . . ? C9 C8 C13 C12 -4.0(8) . . . . ? N2 C8 C13 C14 3.8(7) . . . . ? C9 C8 C13 C14 -179.9(4) . . . . ? C12 C13 C14 O3 -86.2(6) . . . . ? C8 C13 C14 O3 89.6(6) . . . . ? C12 C13 C14 O4 91.3(6) . . . . ? C8 C13 C14 O4 -92.9(5) . . . . ? O5 C15 C16 C17 17.3(7) . . . . ? O6 C15 C16 C17 -164.1(5) . . . . ? O5 C15 C16 C21 -164.5(5) . . . . ? O6 C15 C16 C21 14.1(7) . . . . ? C21 C16 C17 C18 0.3(8) . . . . ? C15 C16 C17 C18 178.6(5) . . . . ? C16 C17 C18 C19 -0.1(9) . . . . ? C17 C18 C19 C20 0.2(9) . . . . ? C18 C19 C20 C21 -0.5(8) . . . . ? C19 C20 C21 C16 0.7(8) . . . . ? C19 C20 C21 N3 175.5(5) . . . . ? C17 C16 C21 C20 -0.6(7) . . . . ? C15 C16 C21 C20 -178.8(4) . . . . ? C17 C16 C21 N3 -175.3(4) . . . . ? C15 C16 C21 N3 6.5(7) . . . . ? O7 C22 C23 C24 173.6(5) . . . . ? O8 C22 C23 C24 -7.1(7) . . . . ? O7 C22 C23 C28 -5.0(7) . . . . ? O8 C22 C23 C28 174.3(4) . . . . ? C28 C23 C24 C25 0.0(9) . . . . ? C22 C23 C24 C25 -178.6(5) . . . . ? C23 C24 C25 C26 0.5(10) . . . . ? C24 C25 C26 C27 -0.4(10) . . . . ? C25 C26 C27 C28 -0.2(9) . . . . ? C26 C27 C28 C23 0.8(8) . . . . ? C26 C27 C28 N4 -170.8(5) . . . . ? C24 C23 C28 C27 -0.6(7) . . . . ? C22 C23 C28 C27 178.0(4) . . . . ? C24 C23 C28 N4 170.9(5) . . . . ? C22 C23 C28 N4 -10.5(7) . . . . ? C6 C7 N1 N2 -166.8(5) . . . . ? C2 C7 N1 N2 15.6(8) . . . . ? C7 N1 N2 C8 -177.3(4) . . . . ? C13 C8 N2 N1 -173.2(4) . . . . ? C9 C8 N2 N1 10.6(7) . . . . ? C20 C21 N3 N3 44.9(7) . . . 2_656 ? C16 C21 N3 N3 -140.3(5) . . . 2_656 ? C27 C28 N4 N4 -50.0(7) . . . 2_667 ? C23 C28 N4 N4 138.4(5) . . . 2_667 ? O2 C1 O1 Pb1 30.3(5) . . . . ? C2 C1 O1 Pb1 -139.9(4) . . . . ? O9 Pb1 O1 C1 -72.9(3) 2_666 . . . ? O9 Pb1 O1 C1 -145.3(3) . . . . ? O4 Pb1 O1 C1 -172.0(3) 2_666 . . . ? Pb3 Pb1 O1 C1 -173.0(3) . . . . ? Pb1 Pb1 O1 C1 -109.2(3) 2_666 . . . ? O4 C14 O3 Pb2 29.3(6) . . . . ? C13 C14 O3 Pb2 -153.3(3) . . . . ? O9 Pb2 O3 C14 -27.1(4) . . . . ? O8 Pb2 O3 C14 -98.9(3) . . . . ? O7 Pb2 O3 C14 -108.0(3) . . . . ? Pb3 Pb2 O3 C14 -46.2(4) . . . . ? O3 C14 O4 Pb3 -160.7(3) . . . 2_666 ? C13 C14 O4 Pb3 21.9(7) . . . 2_666 ? O3 C14 O4 Pb1 31.3(7) . . . 2_666 ? C13 C14 O4 Pb1 -146.0(3) . . . 2_666 ? O6 C15 O5 Pb3 4.8(5) . . . . ? C16 C15 O5 Pb3 -176.6(4) . . . . ? O9 Pb3 O5 C15 -92.9(3) . . . . ? O4 Pb3 O5 C15 -29.1(3) 2_666 . . . ? O6 Pb3 O5 C15 -2.6(3) . . . . ? O7 Pb3 O5 C15 -169.5(3) . . . . ? Pb1 Pb3 O5 C15 -53.9(3) . . . . ? Pb2 Pb3 O5 C15 -121.0(3) . . . . ? O5 C15 O6 Pb3 -4.8(5) . . . . ? C16 C15 O6 Pb3 176.6(4) . . . . ? O9 Pb3 O6 C15 82.1(3) . . . . ? O4 Pb3 O6 C15 158.0(3) 2_666 . . . ? O5 Pb3 O6 C15 2.6(3) . . . . ? O7 Pb3 O6 C15 15.5(3) . . . . ? Pb1 Pb3 O6 C15 110.8(3) . . . . ? Pb2 Pb3 O6 C15 44.7(3) . . . . ? O8 C22 O7 Pb2 -0.9(5) . . . . ? C23 C22 O7 Pb2 178.4(4) . . . . ? O8 C22 O7 Pb3 -91.5(4) . . . . ? C23 C22 O7 Pb3 87.8(4) . . . . ? O9 Pb2 O7 C22 -85.2(3) . . . . ? O8 Pb2 O7 C22 0.5(2) . . . . ? O3 Pb2 O7 C22 11.7(3) . . . . ? Pb3 Pb2 O7 C22 -111.1(3) . . . . ? O9 Pb2 O7 Pb3 25.92(9) . . . . ? O8 Pb2 O7 Pb3 111.60(15) . . . . ? O3 Pb2 O7 Pb3 122.76(11) . . . . ? O9 Pb3 O7 C22 65.8(3) . . . . ? O4 Pb3 O7 C22 45.5(3) 2_666 . . . ? O6 Pb3 O7 C22 137.9(3) . . . . ? O5 Pb3 O7 C22 148.8(3) . . . . ? Pb1 Pb3 O7 C22 80.4(3) . . . . ? Pb2 Pb3 O7 C22 93.3(3) . . . . ? O9 Pb3 O7 Pb2 -27.51(9) . . . . ? O4 Pb3 O7 Pb2 -47.8(2) 2_666 . . . ? O6 Pb3 O7 Pb2 44.65(14) . . . . ? O5 Pb3 O7 Pb2 55.51(10) . . . . ? Pb1 Pb3 O7 Pb2 -12.87(9) . . . . ? O7 C22 O8 Pb2 0.9(5) . . . . ? C23 C22 O8 Pb2 -178.4(4) . . . . ? O9 Pb2 O8 C22 79.9(3) . . . . ? O7 Pb2 O8 C22 -0.5(2) . . . . ? O3 Pb2 O8 C22 -170.9(3) . . . . ? Pb3 Pb2 O8 C22 43.9(3) . . . . ? O4 Pb3 O9 Pb2 -160.32(13) 2_666 . . . ? O6 Pb3 O9 Pb2 -86.56(12) . . . . ? O5 Pb3 O9 Pb2 -36.16(11) . . . . ? O7 Pb3 O9 Pb2 31.74(10) . . . . ? Pb1 Pb3 O9 Pb2 -125.35(16) . . . . ? O4 Pb3 O9 Pb1 79.07(13) 2_666 . . 2_666 ? O6 Pb3 O9 Pb1 152.84(15) . . . 2_666 ? O5 Pb3 O9 Pb1 -156.77(15) . . . 2_666 ? O7 Pb3 O9 Pb1 -88.86(13) . . . 2_666 ? Pb1 Pb3 O9 Pb1 114.05(17) . . . 2_666 ? Pb2 Pb3 O9 Pb1 -120.61(18) . . . 2_666 ? O4 Pb3 O9 Pb1 -34.98(11) 2_666 . . . ? O6 Pb3 O9 Pb1 38.79(12) . . . . ? O5 Pb3 O9 Pb1 89.18(12) . . . . ? O7 Pb3 O9 Pb1 157.09(13) . . . . ? Pb2 Pb3 O9 Pb1 125.35(16) . . . . ? O8 Pb2 O9 Pb3 -87.45(12) . . . . ? O7 Pb2 O9 Pb3 -34.00(11) . . . . ? O3 Pb2 O9 Pb3 -156.45(11) . . . . ? O8 Pb2 O9 Pb1 38.89(11) . . . 2_666 ? O7 Pb2 O9 Pb1 92.34(12) . . . 2_666 ? O3 Pb2 O9 Pb1 -30.11(13) . . . 2_666 ? Pb3 Pb2 O9 Pb1 126.34(16) . . . 2_666 ? O8 Pb2 O9 Pb1 153.93(15) . . . . ? O7 Pb2 O9 Pb1 -152.61(15) . . . . ? O3 Pb2 O9 Pb1 84.93(14) . . . . ? Pb3 Pb2 O9 Pb1 -118.62(18) . . . . ? O9 Pb1 O9 Pb3 122.98(15) 2_666 . . . ? O1 Pb1 O9 Pb3 -129.11(14) . . . . ? O4 Pb1 O9 Pb3 34.55(11) 2_666 . . . ? Pb1 Pb1 O9 Pb3 122.98(15) 2_666 . . . ? O9 Pb1 O9 Pb2 -117.22(16) 2_666 . . . ? O1 Pb1 O9 Pb2 -9.30(13) . . . . ? O4 Pb1 O9 Pb2 154.35(15) 2_666 . . . ? Pb3 Pb1 O9 Pb2 119.81(18) . . . . ? Pb1 Pb1 O9 Pb2 -117.22(16) 2_666 . . . ? O9 Pb1 O9 Pb1 0.0 2_666 . . 2_666 ? O1 Pb1 O9 Pb1 107.92(12) . . . 2_666 ? O4 Pb1 O9 Pb1 -88.43(11) 2_666 . . 2_666 ? Pb3 Pb1 O9 Pb1 -122.98(15) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.903 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 972480'