# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_lxh20121016 _database_code_depnum_ccdc_archive 'CCDC 928609' #TrackingRef 'Cd.cif' _audit_creation_date 2012-11-22 _audit_creation_method ; Olex2 1.2 (compiled Nov 5 2012 18:22:26, GUI svn.r4372) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H12 Cd2 O11, O' _chemical_formula_sum 'C16 H14 Cd2 O12' _chemical_formula_weight 623.07 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Cd1Cl2 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' Cd Cd -0.8075 1.2024 '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' _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_H-M_alt 'P 1 2/c 1' _space_group_name_Hall '-P 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 '-x, -y, -z' 4 'x, -y, z-1/2' _cell_length_a 12.8567(3) _cell_length_b 8.9378(2) _cell_length_c 16.0555(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.613(2) _cell_angle_gamma 90.00 _cell_volume 1807.17(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3890 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 28.9531 _cell_measurement_theta_min 2.9343 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.290 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 7811 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.94 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -63.00 -13.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 107.0000 78.0000 50 #__ type_ start__ end____ width___ exp.time_ 2 omega 14.00 60.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 -107.0000 -78.0000 46 #__ type_ start__ end____ width___ exp.time_ 3 omega -48.00 73.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 0.0000 -180.0000 121 #__ type_ start__ end____ width___ exp.time_ 4 omega -10.00 15.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 77.0000 -150.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0235313000 _diffrn_orient_matrix_UB_12 -0.0672186000 _diffrn_orient_matrix_UB_13 -0.0183269000 _diffrn_orient_matrix_UB_21 0.0492118000 _diffrn_orient_matrix_UB_22 -0.0375513000 _diffrn_orient_matrix_UB_23 0.0127941000 _diffrn_orient_matrix_UB_31 -0.0140141000 _diffrn_orient_matrix_UB_32 -0.0191786000 _diffrn_orient_matrix_UB_33 0.0391845000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3156 _reflns_number_total 3680 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.884 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.119 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 3680 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0301 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+1.3864P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.0661 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H9 of C9, H12 of C12, H2 of C2, H11 of C11, H8 of C8, H4 of C4, {H10A,H11A, H10B,H11B} of O12 At 1.5 times of: {H9A,H9B} of O9 2. Restrained distances O10-H10A 0.85 with sigma of 0.02 O10-H10B 0.85 with sigma of 0.02 O11-H11B 0.85 with sigma of 0.02 O11-H11A 0.85 with sigma of 0.02 3.a Riding coordinates: O12(H10A,H11A,H10B,H11B) 3.b Rotating group: O9(H9A,H9B) 3.c Aromatic/amide H refined with riding coordinates: C4(H4), C2(H2), C12(H12), C8(H8), C11(H11), C9(H9) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cd2 Cd 0.90852(2) 1.71388(3) 0.506854(15) 0.01921(9) Uani 1 1 d . . . Cd1 Cd 0.57973(2) 0.68661(3) 0.493402(16) 0.02096(9) Uani 1 1 d . . . O4 O 0.8698(2) 1.5267(3) 0.58608(16) 0.0264(6) Uani 1 1 d . . . O1 O 0.6130(2) 0.9052(3) 0.57511(15) 0.0241(6) Uani 1 1 d . . . O2 O 0.74777(19) 0.8149(3) 0.52787(16) 0.0218(6) Uani 1 1 d . . . C3 C 0.8583(3) 1.2685(4) 0.6117(2) 0.0157(7) Uani 1 1 d . . . C4 C 0.8683(3) 1.2842(4) 0.6990(2) 0.0174(8) Uani 1 1 d . . . H4 H 0.8946 1.3733 0.7250 0.021 Uiso 1 1 calc R . . C14 C 0.8866(3) 1.3965(4) 0.5597(2) 0.0187(8) Uani 1 1 d . . . C13 C 0.7097(3) 0.9077(4) 0.57256(19) 0.0160(7) Uani 1 1 d . . . C1 C 0.7767(3) 1.0284(4) 0.6205(2) 0.0141(7) Uani 1 1 d . . . C5 C 0.8398(3) 1.1692(4) 0.7481(2) 0.0156(7) Uani 1 1 d . . . C2 C 0.8154(3) 1.1379(4) 0.5731(2) 0.0166(8) Uani 1 1 d . . . H2 H 0.8123 1.1233 0.5154 0.020 Uiso 1 1 calc R . . O3 O 0.9213(2) 1.3703(3) 0.49403(15) 0.0242(6) Uani 1 1 d . . . O6 O 0.9064(2) 1.0971(3) 0.89408(15) 0.0276(6) Uani 1 1 d . . . C15 C 0.8640(3) 1.1953(4) 0.8429(2) 0.0178(8) Uani 1 1 d . . . O5 O 0.8438(3) 1.3228(3) 0.86737(15) 0.0364(8) Uani 1 1 d . . . C12 C 0.7785(3) 0.7763(4) 0.7607(2) 0.0194(8) Uani 1 1 d . . . H12 H 0.8266 0.7468 0.7277 0.023 Uiso 1 1 calc R . . C6 C 0.7894(3) 1.0407(4) 0.7096(2) 0.0141(7) Uani 1 1 d . . . C7 C 0.7466(3) 0.9250(4) 0.76003(19) 0.0149(7) Uani 1 1 d . . . C8 C 0.6717(3) 0.9655(5) 0.8083(2) 0.0263(9) Uani 1 1 d . . . H8 H 0.6491 1.0643 0.8082 0.032 Uiso 1 1 calc R . . C11 C 0.7390(3) 0.6713(4) 0.8105(2) 0.0229(8) Uani 1 1 d . . . H11 H 0.7627 0.5729 0.8119 0.027 Uiso 1 1 calc R . . C10 C 0.6647(3) 0.7124(4) 0.8581(2) 0.0189(8) Uani 1 1 d . . . C9 C 0.6312(3) 0.8605(5) 0.8560(2) 0.0275(9) Uani 1 1 d . . . H9 H 0.5809 0.8891 0.8872 0.033 Uiso 1 1 calc R . . C16 C 0.6199(3) 0.6006(5) 0.9119(2) 0.0232(9) Uani 1 1 d . . . O10 O 0.4893(2) 0.8322(3) 0.38623(17) 0.0347(7) Uani 1 1 d D . . O11 O 0.9943(2) 1.8390(3) 0.62326(18) 0.0364(7) Uani 1 1 d D . . O8 O 0.6330(3) 0.4651(3) 0.90076(17) 0.0416(8) Uani 1 1 d . . . O9 O 0.6629(2) 0.5481(4) 0.61038(17) 0.0412(8) Uani 1 1 d . . . H9A H 0.6440 0.4543 0.6051 0.062 Uiso 1 1 d R . . H9B H 0.7317 0.5525 0.6152 0.062 Uiso 1 1 d R . . O7 O 0.5749(2) 0.6515(4) 0.96828(19) 0.0422(8) Uani 1 1 d . . . O12 O 0.6054(3) 0.3628(4) 0.73546(19) 0.0578(10) Uani 1 1 d . . . H10A H 0.4492 0.7815 0.3483 0.069 Uiso 1 1 d RD . . H11A H 1.0187 1.9262 0.6150 0.069 Uiso 1 1 d RD . . H10B H 0.4529 0.8996 0.4049 0.069 Uiso 1 1 d RD . . H11B H 1.0522 1.7907 0.6367 0.069 Uiso 1 1 d RD . . 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 Cd2 0.02354(15) 0.01978(16) 0.01551(14) 0.00368(11) 0.00677(11) -0.00014(12) Cd1 0.02035(15) 0.02064(16) 0.02329(15) -0.00880(11) 0.00771(11) -0.00392(12) O4 0.0383(16) 0.0110(14) 0.0341(15) 0.0038(11) 0.0174(13) -0.0005(13) O1 0.0198(13) 0.0221(15) 0.0301(14) -0.0116(12) 0.0039(11) -0.0020(13) O2 0.0228(14) 0.0186(15) 0.0255(13) -0.0089(11) 0.0086(11) -0.0007(12) C3 0.0175(18) 0.0120(19) 0.0186(17) 0.0039(14) 0.0061(14) -0.0022(15) C4 0.0189(18) 0.0127(19) 0.0196(17) -0.0003(14) 0.0019(15) -0.0031(16) C14 0.0150(17) 0.019(2) 0.0210(18) 0.0049(16) 0.0013(15) -0.0040(17) C13 0.0213(18) 0.0152(19) 0.0122(16) 0.0032(14) 0.0053(14) 0.0011(16) C1 0.0166(17) 0.0093(18) 0.0163(16) -0.0005(14) 0.0027(14) -0.0032(15) C5 0.0171(17) 0.0129(19) 0.0170(17) 0.0009(14) 0.0037(14) 0.0021(15) C2 0.0207(18) 0.017(2) 0.0133(16) 0.0009(14) 0.0071(14) 0.0005(16) O3 0.0248(14) 0.0270(16) 0.0229(13) 0.0062(12) 0.0096(11) 0.0008(13) O6 0.0405(17) 0.0234(16) 0.0178(12) 0.0037(12) 0.0033(12) 0.0041(14) C15 0.0183(18) 0.018(2) 0.0177(17) -0.0008(15) 0.0055(15) -0.0045(17) O5 0.071(2) 0.0216(16) 0.0152(13) -0.0022(11) 0.0065(14) 0.0100(16) C12 0.026(2) 0.016(2) 0.0185(17) -0.0003(15) 0.0096(16) -0.0001(17) C6 0.0130(16) 0.0133(19) 0.0165(16) 0.0014(14) 0.0040(14) -0.0001(15) C7 0.0195(18) 0.0141(19) 0.0110(15) 0.0006(14) 0.0028(14) -0.0054(16) C8 0.031(2) 0.020(2) 0.031(2) 0.0040(17) 0.0151(18) 0.0050(19) C11 0.029(2) 0.015(2) 0.0256(19) 0.0029(16) 0.0085(17) -0.0021(18) C10 0.0207(19) 0.020(2) 0.0158(17) 0.0039(15) 0.0037(15) -0.0034(17) C9 0.028(2) 0.028(2) 0.031(2) 0.0055(18) 0.0182(18) 0.005(2) C16 0.0205(19) 0.025(2) 0.0228(19) 0.0093(17) 0.0021(16) -0.0043(18) O10 0.0395(17) 0.0272(17) 0.0343(16) -0.0063(13) 0.0000(14) 0.0059(15) O11 0.0369(17) 0.0307(18) 0.0364(16) -0.0043(14) -0.0050(14) -0.0078(15) O8 0.074(2) 0.0250(18) 0.0312(16) 0.0040(13) 0.0238(16) -0.0132(17) O9 0.0365(17) 0.045(2) 0.0427(17) 0.0142(15) 0.0084(14) -0.0009(16) O7 0.0354(17) 0.050(2) 0.0507(18) 0.0229(16) 0.0306(15) 0.0119(16) O12 0.087(3) 0.046(2) 0.0408(18) -0.0074(17) 0.0150(19) -0.023(2) _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 Cd2 O4 2.218(2) . ? Cd2 O2 2.341(2) 1_565 ? Cd2 O3 2.316(3) 3_786 ? Cd2 O6 2.473(3) 4_585 ? Cd2 C15 2.703(3) 4_585 ? Cd2 O5 2.251(3) 4_585 ? Cd2 O11 2.265(3) . ? Cd1 O1 2.344(3) . ? Cd1 O2 2.410(2) . ? Cd1 C13 2.731(4) . ? Cd1 O10 2.280(3) . ? Cd1 O8 2.220(3) 4_565 ? Cd1 O9 2.323(3) . ? Cd1 O7 2.219(3) 2_656 ? O4 C14 1.271(4) . ? O1 C13 1.253(4) . ? O2 Cd2 2.341(2) 1_545 ? O2 C13 1.259(4) . ? C3 C4 1.388(5) . ? C3 C14 1.504(5) . ? C3 C2 1.383(5) . ? C4 H4 0.9300 . ? C4 C5 1.390(5) . ? C14 O3 1.248(4) . ? C13 C1 1.493(5) . ? C1 C2 1.391(5) . ? C1 C6 1.411(4) . ? C5 C15 1.509(5) . ? C5 C6 1.399(5) . ? C2 H2 0.9300 . ? O3 Cd2 2.316(2) 3_786 ? O6 Cd2 2.473(3) 4_586 ? O6 C15 1.249(4) . ? C15 Cd2 2.703(3) 4_586 ? C15 O5 1.249(4) . ? O5 Cd2 2.251(3) 4_586 ? C12 H12 0.9300 . ? C12 C7 1.390(5) . ? C12 C11 1.393(5) . ? C6 C7 1.486(5) . ? C7 C8 1.399(5) . ? C8 H8 0.9300 . ? C8 C9 1.378(5) . ? C11 H11 0.9300 . ? C11 C10 1.388(5) . ? C10 C9 1.390(5) . ? C10 C16 1.509(5) . ? C9 H9 0.9300 . ? C16 O8 1.241(5) . ? C16 O7 1.254(4) . ? O10 H10A 0.8469 . ? O10 H10B 0.8534 . ? O11 H11A 0.8601 . ? O11 H11B 0.8501 . ? O8 Cd1 2.220(3) 4_566 ? O9 H9A 0.8723 . ? O9 H9B 0.8730 . ? O7 Cd1 2.219(3) 2_656 ? 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 O4 Cd2 O2 84.37(10) . 1_565 ? O4 Cd2 O3 94.57(10) . 3_786 ? O4 Cd2 O6 164.72(10) . 4_585 ? O4 Cd2 C15 139.19(11) . 4_585 ? O4 Cd2 O5 112.34(10) . 4_585 ? O4 Cd2 O11 91.58(10) . . ? O2 Cd2 O6 87.81(9) 1_565 4_585 ? O2 Cd2 C15 90.24(10) 1_565 4_585 ? O3 Cd2 O2 171.28(9) 3_786 1_565 ? O3 Cd2 O6 95.11(9) 3_786 4_585 ? O3 Cd2 C15 96.14(9) 3_786 4_585 ? O6 Cd2 C15 27.48(10) 4_585 4_585 ? O5 Cd2 O2 92.26(10) 4_585 1_565 ? O5 Cd2 O3 96.14(10) 4_585 3_786 ? O5 Cd2 O6 54.79(9) 4_585 4_585 ? O5 Cd2 C15 27.31(10) 4_585 4_585 ? O5 Cd2 O11 156.07(11) 4_585 . ? O11 Cd2 O2 89.30(10) . 1_565 ? O11 Cd2 O3 82.07(10) . 3_786 ? O11 Cd2 O6 101.46(10) . 4_585 ? O11 Cd2 C15 128.87(11) . 4_585 ? O1 Cd1 O2 54.60(8) . . ? O1 Cd1 C13 27.23(9) . . ? O2 Cd1 C13 27.44(9) . . ? O10 Cd1 O1 87.39(10) . . ? O10 Cd1 O2 101.46(10) . . ? O10 Cd1 C13 96.27(10) . . ? O10 Cd1 O9 174.93(10) . . ? O8 Cd1 O1 146.91(11) 4_565 . ? O8 Cd1 O2 93.52(11) 4_565 . ? O8 Cd1 C13 120.76(11) 4_565 . ? O8 Cd1 O10 91.26(10) 4_565 . ? O8 Cd1 O9 93.58(11) 4_565 . ? O9 Cd1 O1 89.39(10) . . ? O9 Cd1 O2 79.77(10) . . ? O9 Cd1 C13 82.55(11) . . ? O7 Cd1 O1 92.02(10) 2_656 . ? O7 Cd1 O2 144.64(10) 2_656 . ? O7 Cd1 C13 118.15(10) 2_656 . ? O7 Cd1 O10 86.61(12) 2_656 . ? O7 Cd1 O8 120.92(12) 2_656 4_565 ? O7 Cd1 O9 89.60(12) 2_656 . ? C14 O4 Cd2 115.3(2) . . ? C13 O1 Cd1 93.9(2) . . ? Cd2 O2 Cd1 124.04(10) 1_545 . ? C13 O2 Cd2 142.4(2) . 1_545 ? C13 O2 Cd1 90.6(2) . . ? C4 C3 C14 119.9(3) . . ? C2 C3 C4 119.0(3) . . ? C2 C3 C14 120.9(3) . . ? C3 C4 H4 119.5 . . ? C3 C4 C5 121.1(3) . . ? C5 C4 H4 119.5 . . ? O4 C14 C3 115.8(3) . . ? O3 C14 O4 124.5(3) . . ? O3 C14 C3 119.6(3) . . ? O1 C13 Cd1 58.91(19) . . ? O1 C13 O2 120.6(3) . . ? O1 C13 C1 118.0(3) . . ? O2 C13 Cd1 61.93(18) . . ? O2 C13 C1 121.3(3) . . ? C1 C13 Cd1 176.2(2) . . ? C2 C1 C13 117.4(3) . . ? C2 C1 C6 121.2(3) . . ? C6 C1 C13 121.1(3) . . ? C4 C5 C15 115.7(3) . . ? C4 C5 C6 120.5(3) . . ? C6 C5 C15 123.8(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C14 O3 Cd2 124.4(2) . 3_786 ? C15 O6 Cd2 86.6(2) . 4_586 ? C5 C15 Cd2 171.4(3) . 4_586 ? O6 C15 Cd2 65.94(18) . 4_586 ? O6 C15 C5 121.9(3) . . ? O6 C15 O5 121.7(3) . . ? O5 C15 Cd2 55.73(18) . 4_586 ? O5 C15 C5 116.4(3) . . ? C15 O5 Cd2 97.0(2) . 4_586 ? C7 C12 H12 119.8 . . ? C7 C12 C11 120.5(3) . . ? C11 C12 H12 119.8 . . ? C1 C6 C7 121.2(3) . . ? C5 C6 C1 117.5(3) . . ? C5 C6 C7 121.3(3) . . ? C12 C7 C6 121.9(3) . . ? C12 C7 C8 118.5(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C12 C11 H11 119.7 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.7 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 C16 121.6(3) . . ? C9 C10 C16 119.5(3) . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? O8 C16 C10 119.1(3) . . ? O8 C16 O7 123.7(4) . . ? O7 C16 C10 117.2(4) . . ? Cd1 O10 H10A 112.4 . . ? Cd1 O10 H10B 111.7 . . ? H10A O10 H10B 109.4 . . ? Cd2 O11 H11A 116.9 . . ? Cd2 O11 H11B 102.4 . . ? H11A O11 H11B 99.9 . . ? C16 O8 Cd1 115.5(2) . 4_566 ? Cd1 O9 H9A 111.1 . . ? Cd1 O9 H9B 110.0 . . ? H9A O9 H9B 108.0 . . ? C16 O7 Cd1 145.2(3) . 2_656 ? 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 O9 H9B O4 0.87 1.94 2.771(4) 159.0 1_545 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 Cd2 O4 C14 C3 -178.6(2) . . . . ? Cd2 O4 C14 O3 -0.7(5) . . . . ? Cd2 O2 C13 Cd1 -158.7(4) 1_545 . . . ? Cd2 O2 C13 O1 -164.2(3) 1_545 . . . ? Cd2 O2 C13 C1 18.9(6) 1_545 . . . ? Cd2 O6 C15 C5 175.9(3) 4_586 . . . ? Cd2 O6 C15 O5 -0.8(4) 4_586 . . . ? Cd1 O1 C13 O2 5.6(3) . . . . ? Cd1 O1 C13 C1 -177.4(3) . . . . ? Cd1 O2 C13 O1 -5.4(3) . . . . ? Cd1 O2 C13 C1 177.7(3) . . . . ? Cd1 C13 C1 C2 -147(4) . . . . ? Cd1 C13 C1 C6 26(4) . . . . ? O4 C14 O3 Cd2 107.4(4) . . . 3_786 ? O1 Cd1 O2 Cd2 167.57(18) . . . 1_545 ? O1 Cd1 O2 C13 3.05(19) . . . . ? O1 Cd1 C13 O2 -174.6(3) . . . . ? O1 Cd1 C13 C1 37(4) . . . . ? O1 C13 C1 C2 -111.0(4) . . . . ? O1 C13 C1 C6 61.5(5) . . . . ? O2 Cd2 O4 C14 136.9(3) 1_565 . . . ? O2 Cd1 O1 C13 -3.07(19) . . . . ? O2 Cd1 C13 O1 174.6(3) . . . . ? O2 Cd1 C13 C1 -149(4) . . . . ? O2 C13 C1 C2 66.0(4) . . . . ? O2 C13 C1 C6 -121.5(4) . . . . ? C3 C4 C5 C15 174.6(3) . . . . ? C3 C4 C5 C6 -7.0(5) . . . . ? C3 C14 O3 Cd2 -74.7(4) . . . 3_786 ? C4 C3 C14 O4 -32.4(5) . . . . ? C4 C3 C14 O3 149.6(3) . . . . ? C4 C3 C2 C1 4.0(5) . . . . ? C4 C5 C15 Cd2 20.1(18) . . . 4_586 ? C4 C5 C15 O6 -134.2(4) . . . . ? C4 C5 C15 O5 42.6(5) . . . . ? C4 C5 C6 C1 4.7(5) . . . . ? C4 C5 C6 C7 -172.5(3) . . . . ? C14 C3 C4 C5 178.1(3) . . . . ? C14 C3 C2 C1 -171.5(3) . . . . ? C13 Cd1 O2 Cd2 164.5(3) . . . 1_545 ? C13 C1 C2 C3 166.4(3) . . . . ? C13 C1 C6 C5 -170.5(3) . . . . ? C13 C1 C6 C7 6.7(5) . . . . ? C1 C6 C7 C12 59.7(5) . . . . ? C1 C6 C7 C8 -120.1(4) . . . . ? C5 C15 O5 Cd2 -176.0(3) . . . 4_586 ? C5 C6 C7 C12 -123.2(4) . . . . ? C5 C6 C7 C8 57.0(5) . . . . ? C2 C3 C4 C5 2.5(5) . . . . ? C2 C3 C14 O4 143.1(4) . . . . ? C2 C3 C14 O3 -34.9(5) . . . . ? C2 C1 C6 C5 1.7(5) . . . . ? C2 C1 C6 C7 179.0(3) . . . . ? O3 Cd2 O4 C14 -51.8(3) 3_786 . . . ? O6 Cd2 O4 C14 77.3(4) 4_585 . . . ? O6 C15 O5 Cd2 0.8(4) . . . 4_586 ? C15 Cd2 O4 C14 53.1(3) 4_585 . . . ? C15 C5 C6 C1 -176.9(3) . . . . ? C15 C5 C6 C7 5.8(5) . . . . ? O5 Cd2 O4 C14 46.8(3) 4_585 . . . ? C12 C7 C8 C9 0.5(6) . . . . ? C12 C11 C10 C9 -0.8(6) . . . . ? C12 C11 C10 C16 179.4(3) . . . . ? C6 C1 C2 C3 -6.2(5) . . . . ? C6 C5 C15 Cd2 -158.3(14) . . . 4_586 ? C6 C5 C15 O6 47.4(5) . . . . ? C6 C5 C15 O5 -135.8(4) . . . . ? C6 C7 C8 C9 -179.6(4) . . . . ? C7 C12 C11 C10 2.1(6) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C11 C12 C7 C6 178.2(3) . . . . ? C11 C12 C7 C8 -1.9(5) . . . . ? C11 C10 C9 C8 -0.6(6) . . . . ? C11 C10 C16 O8 -14.5(6) . . . . ? C11 C10 C16 O7 162.6(4) . . . . ? C10 C16 O8 Cd1 173.3(2) . . . 4_566 ? C10 C16 O7 Cd1 107.9(5) . . . 2_656 ? C9 C10 C16 O8 165.7(4) . . . . ? C9 C10 C16 O7 -17.2(5) . . . . ? C16 C10 C9 C8 179.2(4) . . . . ? O10 Cd1 O1 C13 -109.1(2) . . . . ? O10 Cd1 O2 Cd2 -114.03(13) . . . 1_545 ? O10 Cd1 O2 C13 81.4(2) . . . . ? O10 Cd1 C13 O1 71.7(2) . . . . ? O10 Cd1 C13 O2 -102.8(2) . . . . ? O10 Cd1 C13 C1 109(4) . . . . ? O11 Cd2 O4 C14 -134.0(3) . . . . ? O8 Cd1 O1 C13 -20.8(3) 4_565 . . . ? O8 Cd1 O2 Cd2 -22.03(14) 4_565 . . 1_545 ? O8 Cd1 O2 C13 173.4(2) 4_565 . . . ? O8 Cd1 C13 O1 166.95(19) 4_565 . . . ? O8 Cd1 C13 O2 -7.6(2) 4_565 . . . ? O8 Cd1 C13 C1 -156(4) 4_565 . . . ? O8 C16 O7 Cd1 -75.1(6) . . . 2_656 ? O9 Cd1 O1 C13 74.8(2) . . . . ? O9 Cd1 O2 Cd2 70.98(14) . . . 1_545 ? O9 Cd1 O2 C13 -93.5(2) . . . . ? O9 Cd1 C13 O1 -103.3(2) . . . . ? O9 Cd1 C13 O2 82.1(2) . . . . ? O9 Cd1 C13 C1 -66(4) . . . . ? O7 Cd1 O1 C13 164.4(2) 2_656 . . . ? O7 Cd1 O2 Cd2 145.51(18) 2_656 . . 1_545 ? O7 Cd1 O2 C13 -19.0(3) 2_656 . . . ? O7 Cd1 C13 O1 -17.8(2) 2_656 . . . ? O7 Cd1 C13 O2 167.7(2) 2_656 . . . ? O7 Cd1 C13 C1 19(4) 2_656 . . . ? O7 C16 O8 Cd1 -3.6(5) . . . 4_566 ? data_a _database_code_depnum_ccdc_archive 'CCDC 928610' #TrackingRef 'Pb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H42 N4 O12 Pb2' _chemical_formula_weight 1089.08 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1447(7) _cell_length_b 13.8559(9) _cell_length_c 26.1423(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3674.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.87 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 9.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2878 _exptl_absorpt_correction_T_max 0.4305 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27493 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6834 _reflns_number_gt 6413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+6.1549P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.459(9) _refine_ls_number_reflns 6834 _refine_ls_number_parameters 435 _refine_ls_number_restraints 188 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.050 _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 O9 O 0.6644(7) 0.1696(4) 0.8961(2) 0.072(2) Uani 0.763(8) 1 d PGU A 1 N1 N 0.6343(6) 0.0424(4) 0.9446(2) 0.057(2) Uani 0.763(8) 1 d PGU A 1 C17 C 0.7071(5) 0.0877(4) 0.90848(19) 0.051(2) Uani 0.763(8) 1 d PGU A 1 C18 C 0.8252(7) 0.0401(6) 0.8871(3) 0.078(3) Uani 0.763(8) 1 d PGU A 1 H18A H 0.8495 0.0712 0.8556 0.117 Uiso 0.763(8) 1 d PR A 1 H18B H 0.8062 -0.0267 0.8806 0.117 Uiso 0.763(8) 1 d PR A 1 H18C H 0.8966 0.0449 0.9110 0.117 Uiso 0.763(8) 1 d PR A 1 C19 C 0.5155(7) 0.0896(6) 0.9659(3) 0.059(3) Uani 0.763(8) 1 d PGU A 1 H19A H 0.5195 0.1577 0.9594 0.089 Uiso 0.763(8) 1 d PR A 1 H19B H 0.5117 0.0786 1.0021 0.089 Uiso 0.763(8) 1 d PR A 1 H19C H 0.4383 0.0631 0.9500 0.089 Uiso 0.763(8) 1 d PR A 1 C20 C 0.6729(9) -0.0550(5) 0.9632(3) 0.099(4) Uani 0.763(8) 1 d PGU A 1 H20A H 0.6753 -0.0991 0.9349 0.149 Uiso 0.763(8) 1 d PR A 1 H20B H 0.6098 -0.0770 0.9879 0.149 Uiso 0.763(8) 1 d PR A 1 H20C H 0.7585 -0.0517 0.9787 0.149 Uiso 0.763(8) 1 d PR A 1 O9' O 0.712(2) 0.1620(14) 0.8951(9) 0.072(2) Uani 0.237(8) 1 d PG A 2 N1' N 0.7107(19) 0.0230(13) 0.9330(7) 0.057(2) Uani 0.237(8) 1 d PG A 2 C17' C 0.6494(19) 0.1065(12) 0.9238(7) 0.051(2) Uani 0.237(8) 1 d PG A 2 C18' C 0.521(3) 0.126(2) 0.9465(12) 0.078(3) Uani 0.237(8) 1 d PG A 2 H18D H 0.5243 0.1881 0.9644 0.117 Uiso 0.237(8) 1 d PR A 2 H18E H 0.4995 0.0749 0.9708 0.117 Uiso 0.237(8) 1 d PR A 2 H18F H 0.4545 0.1286 0.9196 0.117 Uiso 0.237(8) 1 d PR A 2 C19' C 0.839(2) 0.0039(18) 0.9100(10) 0.059(3) Uani 0.237(8) 1 d PG A 2 H19D H 0.8395 0.0258 0.8745 0.089 Uiso 0.237(8) 1 d PR A 2 H19E H 0.8575 -0.0655 0.9111 0.089 Uiso 0.237(8) 1 d PR A 2 H19F H 0.9076 0.0384 0.9291 0.089 Uiso 0.237(8) 1 d PR A 2 C20' C 0.649(3) -0.049(2) 0.9660(12) 0.099(4) Uani 0.237(8) 1 d PG A 2 H20D H 0.5864 -0.0175 0.9890 0.149 Uiso 0.237(8) 1 d PR A 2 H20E H 0.7168 -0.0818 0.9862 0.149 Uiso 0.237(8) 1 d PR A 2 H20F H 0.6024 -0.0965 0.9449 0.149 Uiso 0.237(8) 1 d PR A 2 O10 O 0.6522(8) 0.3956(5) 0.7496(3) 0.071(2) Uani 0.694(8) 1 d PGU A 1 N2 N 0.6434(8) 0.4974(5) 0.6853(3) 0.081(3) Uani 0.694(8) 1 d PGU A 1 C21 C 0.7143(7) 0.4582(5) 0.7240(2) 0.064(3) Uani 0.694(8) 1 d PGU A 1 C22 C 0.8515(8) 0.4896(9) 0.7329(4) 0.099(4) Uani 0.694(8) 1 d PGU A 1 H22A H 0.8527 0.5395 0.7584 0.148 Uiso 0.694(8) 1 d PR A 1 H22B H 0.8881 0.5139 0.7016 0.148 Uiso 0.694(8) 1 d PR A 1 H22C H 0.9029 0.4358 0.7446 0.148 Uiso 0.694(8) 1 d PR A 1 C23 C 0.5048(8) 0.4657(8) 0.6761(4) 0.088(4) Uani 0.694(8) 1 d PGU A 1 H23A H 0.5033 0.4184 0.6492 0.133 Uiso 0.694(8) 1 d PR A 1 H23B H 0.4523 0.5203 0.6663 0.133 Uiso 0.694(8) 1 d PR A 1 H23C H 0.4696 0.4379 0.7068 0.133 Uiso 0.694(8) 1 d PR A 1 C24 C 0.7022(13) 0.5725(7) 0.6514(4) 0.124(5) Uani 0.694(8) 1 d PGU A 1 H24A H 0.7393 0.6231 0.6720 0.186 Uiso 0.694(8) 1 d PR A 1 H24B H 0.6351 0.5988 0.6296 0.186 Uiso 0.694(8) 1 d PR A 1 H24C H 0.7702 0.5440 0.6309 0.186 Uiso 0.694(8) 1 d PR A 1 O10' O 0.699(2) 0.3911(13) 0.7461(7) 0.071(2) Uani 0.306(8) 1 d PG A 2 N2' N 0.7070(19) 0.5200(12) 0.6975(7) 0.081(3) Uani 0.306(8) 1 d PG A 2 C21' C 0.6385(17) 0.4416(11) 0.7136(6) 0.064(3) Uani 0.306(8) 1 d PG A 2 C22' C 0.506(2) 0.4223(19) 0.6929(11) 0.099(4) Uani 0.306(8) 1 d PG A 2 H22D H 0.5044 0.3591 0.6778 0.148 Uiso 0.306(8) 1 d PR A 2 H22E H 0.4852 0.4698 0.6673 0.148 Uiso 0.306(8) 1 d PR A 2 H22F H 0.4424 0.4256 0.7200 0.148 Uiso 0.306(8) 1 d PR A 2 C23' C 0.841(2) 0.5393(17) 0.7186(10) 0.088(4) Uani 0.306(8) 1 d PG A 2 H23D H 0.8359 0.5459 0.7551 0.133 Uiso 0.306(8) 1 d PR A 2 H23E H 0.8754 0.5978 0.7040 0.133 Uiso 0.306(8) 1 d PR A 2 H23F H 0.8987 0.4864 0.7102 0.133 Uiso 0.306(8) 1 d PR A 2 C24' C 0.647(3) 0.5861(19) 0.6589(10) 0.124(5) Uani 0.306(8) 1 d PG A 2 H24D H 0.6691 0.5644 0.6251 0.186 Uiso 0.306(8) 1 d PR A 2 H24E H 0.6795 0.6505 0.6639 0.186 Uiso 0.306(8) 1 d PR A 2 H24F H 0.5524 0.5859 0.6628 0.186 Uiso 0.306(8) 1 d PR A 2 O11 O 0.8217(14) 0.6115(7) 1.0174(4) 0.080(3) Uani 0.468(8) 1 d PGU B 1 N4 N 0.8695(13) 0.7668(7) 1.0404(5) 0.075(3) Uani 0.468(8) 1 d PGU B 1 C41 C 0.8063(11) 0.6816(7) 1.0481(4) 0.064(3) Uani 0.468(8) 1 d PGU B 1 C42 C 0.7177(17) 0.6711(11) 1.0935(5) 0.089(4) Uani 0.468(8) 1 d PGU B 1 H42A H 0.6745 0.6095 1.0922 0.134 Uiso 0.468(8) 1 d PR B 1 H42B H 0.6528 0.7215 1.0931 0.134 Uiso 0.468(8) 1 d PR B 1 H42C H 0.7690 0.6755 1.1243 0.134 Uiso 0.468(8) 1 d PR B 1 C43 C 0.855(2) 0.8488(9) 1.0743(6) 0.120(5) Uani 0.468(8) 1 d PGU B 1 H43A H 0.7650 0.8540 1.0850 0.180 Uiso 0.468(8) 1 d PR B 1 H43B H 0.8806 0.9066 1.0566 0.180 Uiso 0.468(8) 1 d PR B 1 H43C H 0.9106 0.8401 1.1037 0.180 Uiso 0.468(8) 1 d PR B 1 C44 C 0.9570(18) 0.7833(10) 0.9976(7) 0.120(6) Uani 0.468(8) 1 d PGU B 1 H44A H 1.0309 0.7402 0.9999 0.180 Uiso 0.468(8) 1 d PR B 1 H44B H 0.9877 0.8488 0.9983 0.180 Uiso 0.468(8) 1 d PR B 1 H44C H 0.9105 0.7717 0.9662 0.180 Uiso 0.468(8) 1 d PR B 1 O11' O 0.7914(13) 0.6281(8) 1.0120(4) 0.080(3) Uani 0.532(8) 1 d PG B 2 N4' N 0.8339(11) 0.7528(7) 1.0642(4) 0.075(3) Uani 0.532(8) 1 d PG B 2 C41' C 0.8541(10) 0.7038(6) 1.0209(3) 0.064(3) Uani 0.532(8) 1 d PG B 2 C42' C 0.9524(16) 0.7430(11) 0.9848(5) 0.089(4) Uani 0.532(8) 1 d PG B 2 H42D H 0.9881 0.6914 0.9646 0.134 Uiso 0.532(8) 1 d PR B 2 H42E H 1.0220 0.7736 1.0036 0.134 Uiso 0.532(8) 1 d PR B 2 H42F H 0.9110 0.7892 0.9628 0.134 Uiso 0.532(8) 1 d PR B 2 C43' C 0.9031(17) 0.8397(11) 1.0763(6) 0.120(5) Uani 0.532(8) 1 d PG B 2 H43D H 0.9894 0.8240 1.0887 0.180 Uiso 0.532(8) 1 d PR B 2 H43E H 0.8557 0.8745 1.1021 0.180 Uiso 0.532(8) 1 d PR B 2 H43F H 0.9105 0.8787 1.0462 0.180 Uiso 0.532(8) 1 d PR B 2 C44' C 0.7420(17) 0.7236(11) 1.1023(6) 0.120(6) Uani 0.532(8) 1 d PG B 2 H44D H 0.6950 0.6678 1.0906 0.180 Uiso 0.532(8) 1 d PR B 2 H44E H 0.6810 0.7751 1.1086 0.180 Uiso 0.532(8) 1 d PR B 2 H44F H 0.7882 0.7084 1.1332 0.180 Uiso 0.532(8) 1 d PR B 2 O13 O 0.7660(11) 0.7197(7) 0.8749(3) 0.098(3) Uani 0.623(9) 1 d PGU B 1 N3 N 0.8296(9) 0.7778(6) 0.8022(3) 0.068(3) Uani 0.623(9) 1 d PGU B 1 C27 C 0.7342(8) 0.7300(6) 0.8280(3) 0.079(3) Uani 0.623(9) 1 d PGU B 1 C28 C 0.6119(11) 0.6964(12) 0.8013(4) 0.117(5) Uani 0.623(9) 1 d PGU B 1 H28A H 0.5587 0.6597 0.8246 0.175 Uiso 0.623(9) 1 d PR B 1 H28B H 0.6357 0.6568 0.7726 0.175 Uiso 0.623(9) 1 d PR B 1 H28C H 0.5629 0.7514 0.7895 0.175 Uiso 0.623(9) 1 d PR B 1 C29 C 0.9539(10) 0.8131(11) 0.8255(4) 0.097(4) Uani 0.623(9) 1 d PGU B 1 H29A H 0.9496 0.8819 0.8295 0.145 Uiso 0.623(9) 1 d PR B 1 H29B H 1.0267 0.7968 0.8037 0.145 Uiso 0.623(9) 1 d PR B 1 H29C H 0.9659 0.7834 0.8584 0.145 Uiso 0.623(9) 1 d PR B 1 C30 C 0.8243(13) 0.8021(10) 0.7470(3) 0.098(4) Uani 0.623(9) 1 d PGU B 1 H30A H 0.8458 0.7459 0.7272 0.147 Uiso 0.623(9) 1 d PR B 1 H30B H 0.8864 0.8525 0.7397 0.147 Uiso 0.623(9) 1 d PR B 1 H30C H 0.7371 0.8235 0.7383 0.147 Uiso 0.623(9) 1 d PR B 1 O13' O 0.7205(19) 0.7179(14) 0.8713(5) 0.098(3) Uani 0.377(9) 1 d PG B 2 N3' N 0.7405(15) 0.7482(11) 0.7922(5) 0.068(3) Uani 0.377(9) 1 d PG B 2 C27' C 0.7956(15) 0.7527(11) 0.8383(5) 0.079(3) Uani 0.377(9) 1 d PG B 2 C28' C 0.927(2) 0.794(2) 0.8454(8) 0.117(5) Uani 0.377(9) 1 d PG B 2 H28D H 0.9233 0.8443 0.8708 0.175 Uiso 0.377(9) 1 d PR B 2 H28E H 0.9576 0.8209 0.8135 0.175 Uiso 0.377(9) 1 d PR B 2 H28F H 0.9872 0.7445 0.8564 0.175 Uiso 0.377(9) 1 d PR B 2 C29' C 0.611(2) 0.708(2) 0.7824(7) 0.097(4) Uani 0.377(9) 1 d PG B 2 H29D H 0.6090 0.6418 0.7932 0.145 Uiso 0.377(9) 1 d PR B 2 H29E H 0.5921 0.7120 0.7464 0.145 Uiso 0.377(9) 1 d PR B 2 H29F H 0.5459 0.7445 0.8012 0.145 Uiso 0.377(9) 1 d PR B 2 C30' C 0.803(2) 0.7829(17) 0.7458(7) 0.098(4) Uani 0.377(9) 1 d PG B 2 H30D H 0.8888 0.8082 0.7538 0.147 Uiso 0.377(9) 1 d PR B 2 H30E H 0.7496 0.8331 0.7309 0.147 Uiso 0.377(9) 1 d PR B 2 H30F H 0.8115 0.7304 0.7219 0.147 Uiso 0.377(9) 1 d PR B 2 Pb1 Pb 0.70884(2) 0.301856(17) 0.834036(9) 0.03177(6) Uani 1 1 d . . . Pb2 Pb 0.73223(2) 0.535887(16) 0.928644(9) 0.02975(6) Uani 1 1 d . . . O1 O 0.4724(4) 0.3237(3) 0.8368(2) 0.0441(12) Uani 1 1 d . A . O2 O 0.5567(4) 0.4610(4) 0.86593(19) 0.0463(12) Uani 1 1 d . A . O3 O 0.3472(5) 0.6748(4) 0.72310(19) 0.0469(13) Uani 1 1 d . . . O4 O 0.1314(5) 0.6955(5) 0.7271(2) 0.0644(17) Uani 1 1 d . . . O5 O -0.1269(4) 0.4770(4) 0.85621(17) 0.0414(12) Uani 1 1 d . . . O6 O -0.0210(4) 0.5280(4) 0.92429(17) 0.0455(12) Uani 1 1 d . . . O7 O 0.2611(5) 0.1218(3) 1.04284(19) 0.0487(13) Uani 1 1 d . . . O8 O 0.0881(6) 0.0634(4) 1.0000(2) 0.0571(15) Uani 1 1 d . . . C1 C 0.2159(6) 0.4452(4) 0.8637(2) 0.0264(12) Uani 1 1 d . . . C2 C 0.3359(5) 0.4630(5) 0.8384(2) 0.0284(13) Uani 1 1 d . A . C3 C 0.3414(6) 0.5330(5) 0.8001(2) 0.0340(15) Uani 1 1 d . . . H3 H 0.4218 0.5462 0.7845 0.041 Uiso 1 1 calc R . . C4 C 0.2297(6) 0.5836(4) 0.7847(2) 0.0345(14) Uani 1 1 d . . . C5 C 0.1120(6) 0.5653(4) 0.8097(2) 0.0311(15) Uani 1 1 d . . . H5 H 0.0359 0.5973 0.7994 0.037 Uiso 1 1 calc R . . C6 C 0.1061(6) 0.4994(5) 0.8501(2) 0.0301(14) Uani 1 1 d . . . C7 C 0.2057(6) 0.3665(4) 0.9027(2) 0.0292(13) Uani 1 1 d . . . C8 C 0.2943(7) 0.3568(5) 0.9423(2) 0.0354(15) Uani 1 1 d . . . H8 H 0.3622 0.4013 0.9459 0.043 Uiso 1 1 calc R . . C9 C 0.2832(7) 0.2811(5) 0.9768(2) 0.0365(15) Uani 1 1 d . . . H9 H 0.3432 0.2756 1.0035 0.044 Uiso 1 1 calc R . . C10 C 0.1835(7) 0.2139(5) 0.9717(3) 0.0372(16) Uani 1 1 d . . . C11 C 0.0944(7) 0.2219(5) 0.9322(3) 0.0377(15) Uani 1 1 d . . . H11 H 0.0282 0.1760 0.9284 0.045 Uiso 1 1 calc R . . C12 C 0.1036(6) 0.2990(5) 0.8979(3) 0.0355(15) Uani 1 1 d . . . H12 H 0.0419 0.3055 0.8718 0.043 Uiso 1 1 calc R . . C13 C 0.4633(6) 0.4111(5) 0.8488(2) 0.0301(14) Uani 1 1 d . . . C14 C 0.2363(7) 0.6570(5) 0.7417(3) 0.0396(16) Uani 1 1 d . . . C15 C -0.0223(6) 0.4993(4) 0.8794(2) 0.0294(14) Uani 1 1 d . . . C16 C 0.1740(7) 0.1265(5) 1.0068(3) 0.0390(16) 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 O9 0.091(6) 0.064(4) 0.063(4) 0.015(3) 0.008(4) 0.006(4) N1 0.062(5) 0.051(4) 0.058(4) 0.001(3) 0.002(4) -0.004(4) C17 0.060(5) 0.056(4) 0.036(4) -0.003(4) -0.003(4) -0.006(4) C18 0.073(6) 0.086(7) 0.076(6) 0.002(6) 0.012(5) 0.006(5) C19 0.059(5) 0.072(6) 0.047(5) 0.004(5) 0.008(4) -0.007(4) C20 0.114(8) 0.077(5) 0.107(7) 0.026(5) 0.006(6) 0.011(5) O9' 0.091(6) 0.064(4) 0.063(4) 0.015(3) 0.008(4) 0.006(4) N1' 0.062(5) 0.051(4) 0.058(4) 0.001(3) 0.002(4) -0.004(4) C17' 0.060(5) 0.056(4) 0.036(4) -0.003(4) -0.003(4) -0.006(4) C18' 0.073(6) 0.086(7) 0.076(6) 0.002(6) 0.012(5) 0.006(5) C19' 0.059(5) 0.072(6) 0.047(5) 0.004(5) 0.008(4) -0.007(4) C20' 0.114(8) 0.077(5) 0.107(7) 0.026(5) 0.006(6) 0.011(5) O10 0.073(6) 0.080(4) 0.062(4) 0.022(3) 0.000(4) -0.004(4) N2 0.109(6) 0.069(6) 0.065(5) 0.005(4) -0.016(5) -0.005(5) C21 0.075(6) 0.067(5) 0.048(5) -0.006(4) 0.003(4) -0.008(5) C22 0.090(6) 0.105(8) 0.101(8) 0.004(7) -0.011(6) -0.019(6) C23 0.091(6) 0.089(7) 0.085(7) 0.009(6) -0.021(5) 0.014(6) C24 0.143(9) 0.115(8) 0.113(7) 0.042(6) -0.006(7) -0.010(7) O10' 0.073(6) 0.080(4) 0.062(4) 0.022(3) 0.000(4) -0.004(4) N2' 0.109(6) 0.069(6) 0.065(5) 0.005(4) -0.016(5) -0.005(5) C21' 0.075(6) 0.067(5) 0.048(5) -0.006(4) 0.003(4) -0.008(5) C22' 0.090(6) 0.105(8) 0.101(8) 0.004(7) -0.011(6) -0.019(6) C23' 0.091(6) 0.089(7) 0.085(7) 0.009(6) -0.021(5) 0.014(6) C24' 0.143(9) 0.115(8) 0.113(7) 0.042(6) -0.006(7) -0.010(7) O11 0.086(6) 0.073(4) 0.083(4) -0.023(4) -0.010(4) -0.011(4) N4 0.078(6) 0.073(5) 0.073(7) -0.019(5) -0.009(5) 0.000(4) C41 0.060(6) 0.074(5) 0.058(6) -0.011(5) -0.014(4) 0.005(5) C42 0.089(8) 0.091(8) 0.087(7) -0.002(6) 0.008(6) 0.003(6) C43 0.128(10) 0.104(6) 0.128(7) -0.055(6) -0.018(7) 0.002(7) C44 0.113(9) 0.126(9) 0.121(8) 0.003(7) 0.020(7) -0.016(7) O11' 0.086(6) 0.073(4) 0.083(4) -0.023(4) -0.010(4) -0.011(4) N4' 0.078(6) 0.073(5) 0.073(7) -0.019(5) -0.009(5) 0.000(4) C41' 0.060(6) 0.074(5) 0.058(6) -0.011(5) -0.014(4) 0.005(5) C42' 0.089(8) 0.091(8) 0.087(7) -0.002(6) 0.008(6) 0.003(6) C43' 0.128(10) 0.104(6) 0.128(7) -0.055(6) -0.018(7) 0.002(7) C44' 0.113(9) 0.126(9) 0.121(8) 0.003(7) 0.020(7) -0.016(7) O13 0.124(7) 0.097(5) 0.074(4) 0.025(4) -0.010(5) -0.009(6) N3 0.073(5) 0.063(6) 0.068(5) 0.011(4) -0.009(5) 0.003(4) C27 0.100(7) 0.062(6) 0.075(5) 0.005(5) -0.007(5) -0.016(6) C28 0.098(7) 0.130(9) 0.121(9) 0.001(8) -0.019(6) -0.026(7) C29 0.084(6) 0.105(8) 0.101(7) -0.012(7) -0.003(6) -0.014(6) C30 0.108(8) 0.104(7) 0.083(5) 0.032(5) 0.002(5) -0.009(6) O13' 0.124(7) 0.097(5) 0.074(4) 0.025(4) -0.010(5) -0.009(6) N3' 0.073(5) 0.063(6) 0.068(5) 0.011(4) -0.009(5) 0.003(4) C27' 0.100(7) 0.062(6) 0.075(5) 0.005(5) -0.007(5) -0.016(6) C28' 0.098(7) 0.130(9) 0.121(9) 0.001(8) -0.019(6) -0.026(7) C29' 0.084(6) 0.105(8) 0.101(7) -0.012(7) -0.003(6) -0.014(6) C30' 0.108(8) 0.104(7) 0.083(5) 0.032(5) 0.002(5) -0.009(6) Pb1 0.02619(11) 0.03072(11) 0.03839(12) -0.00868(10) 0.00121(10) 0.00163(10) Pb2 0.02750(11) 0.02794(11) 0.03383(11) 0.00341(9) 0.00552(9) 0.00200(9) O1 0.032(2) 0.036(3) 0.064(3) -0.001(3) 0.003(2) 0.0048(19) O2 0.033(2) 0.047(3) 0.059(3) -0.005(3) -0.009(2) 0.003(2) O3 0.033(2) 0.054(3) 0.054(3) 0.023(2) 0.008(2) 0.005(2) O4 0.034(3) 0.084(4) 0.076(4) 0.051(3) 0.009(3) 0.010(3) O5 0.030(2) 0.054(3) 0.040(2) -0.003(2) 0.0047(19) -0.006(2) O6 0.035(2) 0.068(3) 0.033(2) -0.007(3) 0.005(2) 0.004(2) O7 0.047(3) 0.046(3) 0.054(3) 0.024(2) -0.012(2) -0.002(2) O8 0.060(3) 0.043(3) 0.069(4) 0.023(3) -0.014(3) -0.011(3) C1 0.028(3) 0.029(3) 0.023(3) 0.000(2) 0.002(2) -0.002(3) C2 0.027(3) 0.029(3) 0.028(3) -0.004(3) -0.001(2) 0.000(3) C3 0.024(3) 0.041(4) 0.037(3) -0.002(3) 0.004(2) -0.003(3) C4 0.031(3) 0.036(3) 0.036(3) 0.004(3) 0.001(3) -0.002(3) C5 0.027(3) 0.029(3) 0.037(3) 0.005(3) -0.004(3) 0.002(2) C6 0.028(3) 0.032(3) 0.030(3) 0.001(3) 0.001(3) -0.003(3) C7 0.030(3) 0.030(3) 0.028(3) 0.000(2) 0.006(3) 0.002(3) C8 0.030(3) 0.039(3) 0.037(3) 0.004(3) 0.003(3) -0.004(3) C9 0.035(3) 0.043(4) 0.032(3) 0.007(3) -0.004(3) 0.004(3) C10 0.036(4) 0.035(4) 0.041(4) 0.007(3) 0.003(3) 0.005(3) C11 0.038(3) 0.034(4) 0.041(4) 0.008(3) 0.001(3) -0.005(3) C12 0.027(3) 0.038(4) 0.041(4) 0.005(3) -0.006(3) 0.000(3) C13 0.024(3) 0.034(4) 0.033(3) 0.006(3) 0.005(2) 0.000(3) C14 0.039(4) 0.038(3) 0.042(4) 0.008(3) 0.002(3) -0.002(3) C15 0.028(3) 0.026(3) 0.034(3) 0.008(3) 0.004(3) 0.001(2) C16 0.039(4) 0.038(4) 0.040(4) 0.011(3) 0.005(3) 0.005(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 O9 C17 1.2580 . ? O9 Pb1 2.488(5) . ? N1 C17 1.3538 . ? N1 C19 1.4789 . ? N1 C20 1.4866 . ? C17 C18 1.4771 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O9' C17' 1.247(11) . ? O9' Pb1 2.511(19) . ? N1' C17' 1.335(12) . ? N1' C19' 1.462(13) . ? N1' C20' 1.463(13) . ? C17' C18' 1.453(13) . ? C18' H18D 0.9779 . ? C18' H18E 0.9778 . ? C18' H18F 0.9778 . ? C19' H18B 0.9398 . ? C19' H19D 0.9779 . ? C19' H19E 0.9778 . ? C19' H19F 0.9779 . ? C20' H20D 0.9779 . ? C20' H20E 0.9779 . ? C20' H20F 0.9778 . ? O10 C21 1.2630 . ? O10 Pb1 2.625(6) . ? N2 C21 1.3549 . ? N2 C24 1.4908 . ? N2 C23 1.4930 . ? C21 C22 1.4770 . ? C22 H22A 0.9600 . ? C22 H22B 0.9599 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O10' C21' 1.260(10) . ? O10' Pb1 2.612(17) . ? N2' C21' 1.356(10) . ? N2' C23' 1.492(12) . ? N2' C24' 1.494(11) . ? C21' C22' 1.472(11) . ? C22' H22D 0.9617 . ? C22' H22E 0.9616 . ? C22' H22F 0.9617 . ? C23' H23D 0.9617 . ? C23' H23E 0.9617 . ? C23' H23F 0.9617 . ? C24' H24D 0.9617 . ? C24' H24E 0.9617 . ? C24' H24F 0.9617 . ? O11 C41 1.2706 . ? O11 Pb2 2.703(11) . ? N4 C41 1.3582 . ? N4 C44 1.4463 . ? N4 C43 1.4467 . ? C41 C42 1.4954 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? O11' C41' 1.249(6) . ? O11' Pb2 2.597(10) . ? N4' C41' 1.335(6) . ? N4' C44' 1.422(6) . ? N4' C43' 1.429(7) . ? C41' C42' 1.477(7) . ? C42' H42D 0.9583 . ? C42' H42E 0.9584 . ? C42' H42F 0.9584 . ? C43' H43D 0.9584 . ? C43' H43E 0.9583 . ? C43' H43F 0.9583 . ? C44' H42B 0.9366 . ? C44' H42C 0.9223 . ? C44' H44D 0.9584 . ? C44' H44E 0.9584 . ? C44' H44F 0.9584 . ? O13 C27 1.2750 . ? O13 Pb2 2.929(9) . ? N3 C27 1.3530 . ? N3 C29 1.4830 . ? N3 C30 1.4838 . ? C27 C28 1.4983 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C28 H29F 0.9440 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C30 H30D 0.6841 . ? C30 H30E 0.9680 . ? O13' C27' 1.247(7) . ? O13' Pb2 2.936(17) . ? N3' C27' 1.329(8) . ? N3' C29' 1.448(9) . ? N3' C30' 1.450(9) . ? C27' C28' 1.466(9) . ? C28' H28D 0.9634 . ? C28' H28E 0.9634 . ? C28' H28F 0.9634 . ? C29' H29D 0.9634 . ? C29' H29E 0.9634 . ? C29' H29F 0.9634 . ? C30' H30D 0.9634 . ? C30' H30E 0.9634 . ? C30' H30F 0.9634 . ? Pb1 O3 2.378(5) 3_646 ? Pb1 O1 2.418(4) . ? Pb1 O4 2.712(5) 3_646 ? Pb2 O7 2.327(4) 4_557 ? Pb2 O5 2.508(4) 1_655 ? Pb2 O6 2.508(4) 1_655 ? Pb2 O2 2.634(5) . ? Pb2 O8 2.741(5) 4_557 ? Pb2 C15 2.848(6) 1_655 ? O1 C13 1.254(8) . ? O2 C13 1.255(8) . ? O3 C14 1.250(8) . ? O3 Pb1 2.378(5) 3_656 ? O4 C14 1.249(9) . ? O4 Pb1 2.712(5) 3_656 ? O5 C15 1.261(8) . ? O5 Pb2 2.508(4) 1_455 ? O6 C15 1.238(8) . ? O6 Pb2 2.508(4) 1_455 ? O7 C16 1.293(8) . ? O7 Pb2 2.327(4) 4_457 ? O8 C16 1.247(9) . ? O8 Pb2 2.741(5) 4_457 ? C1 C6 1.390(9) . ? C1 C2 1.406(8) . ? C1 C7 1.497(8) . ? C2 C3 1.396(9) . ? C2 C13 1.504(8) . ? C3 C4 1.392(9) . ? C3 H3 0.9300 . ? C4 C5 1.384(9) . ? C4 C14 1.517(9) . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 C15 1.513(8) . ? C7 C8 1.376(9) . ? C7 C12 1.401(9) . ? C8 C9 1.388(9) . ? C8 H8 0.9300 . ? C9 C10 1.380(9) . ? C9 H9 0.9300 . ? C10 C11 1.376(9) . ? C10 C16 1.523(9) . ? C11 C12 1.399(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C15 Pb2 2.848(6) 1_455 ? 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 C17 O9 Pb1 140.4(3) . . ? C17 N1 C19 120.2 . . ? C17 N1 C20 120.3 . . ? C19 N1 C20 119.6 . . ? C17 N1 H20D 165.6 . . ? C19 N1 H20D 72.1 . . ? C20 N1 H20D 48.2 . . ? O9 C17 N1 114.2 . . ? O9 C17 C18 125.7 . . ? N1 C17 C18 120.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C18 H19D 143.6 . . ? H18A C18 H19D 55.9 . . ? H18B C18 H19D 57.7 . . ? H18C C18 H19D 106.9 . . ? C17 C18 H19F 101.4 . . ? H18A C18 H19F 122.3 . . ? H18B C18 H19F 104.1 . . ? H18C C18 H19F 12.9 . . ? H19D C18 H19F 114.6 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C19 H18D 112.1 . . ? H19A C19 H18D 8.7 . . ? H19B C19 H18D 100.9 . . ? H19C C19 H18D 115.0 . . ? N1 C19 H18E 108.1 . . ? H19A C19 H18E 142.4 . . ? H19B C19 H18E 55.6 . . ? H19C C19 H18E 57.4 . . ? H18D C19 H18E 138.6 . . ? N1 C19 H18F 101.4 . . ? H19A C19 H18F 60.5 . . ? H19B C19 H18F 149.1 . . ? H19C C19 H18F 55.8 . . ? H18D C19 H18F 68.6 . . ? H18E C19 H18F 112.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C20 H20D 66.8 . . ? H20A C20 H20D 135.5 . . ? H20B C20 H20D 44.3 . . ? H20C C20 H20D 113.3 . . ? N1 C20 H20E 141.2 . . ? H20A C20 H20E 104.9 . . ? H20B C20 H20E 74.3 . . ? H20C C20 H20E 40.0 . . ? H20D C20 H20E 100.1 . . ? N1 C20 H20F 100.0 . . ? H20A C20 H20F 46.2 . . ? H20B C20 H20F 70.9 . . ? H20C C20 H20F 147.9 . . ? H20D C20 H20F 89.7 . . ? H20E C20 H20F 116.9 . . ? C17' O9' Pb1 148.4(11) . . ? C17' N1' C19' 120.0 . . ? C17' N1' C20' 120.0 . . ? C19' N1' C20' 120.0 . . ? O9' C17' N1' 113.9 . . ? O9' C17' C18' 125.8 . . ? N1' C17' C18' 120.3 . . ? C17' C18' H19A 115.4 . . ? C17' C18' H19C 121.1 . . ? H19A C18' H19C 119.8 . . ? C17' C18' H18D 109.5 . . ? H19A C18' H18D 9.7 . . ? H19C C18' H18D 127.8 . . ? C17' C18' H18E 109.5 . . ? H19A C18' H18E 99.9 . . ? H19C C18' H18E 43.3 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H19A C18' H18F 112.7 . . ? H19C C18' H18F 66.3 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? N1' C19' H18B 95.5 . . ? N1' C19' H18C 119.8 . . ? H18B C19' H18C 126.7 . . ? N1' C19' H19D 109.5 . . ? H18B C19' H19D 50.4 . . ? H18C C19' H19D 79.2 . . ? N1' C19' H19E 109.5 . . ? H18B C19' H19E 69.5 . . ? H18C C19' H19E 123.6 . . ? H19D C19' H19E 109.5 . . ? N1' C19' H19F 109.5 . . ? H18B C19' H19F 153.1 . . ? H18C C19' H19F 30.3 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? N1' C20' H20A 83.6 . . ? N1' C20' H20B 165.7 . . ? H20A C20' H20B 110.4 . . ? N1' C20' H20C 77.3 . . ? H20A C20' H20C 87.7 . . ? H20B C20' H20C 104.9 . . ? N1' C20' H20D 109.5 . . ? H20A C20' H20D 153.4 . . ? H20B C20' H20D 56.8 . . ? H20C C20' H20D 117.3 . . ? N1' C20' H20E 109.5 . . ? H20A C20' H20E 86.4 . . ? H20B C20' H20E 74.9 . . ? H20C C20' H20E 32.6 . . ? H20D C20' H20E 109.5 . . ? N1' C20' H20F 109.5 . . ? H20A C20' H20F 44.0 . . ? H20B C20' H20F 80.8 . . ? H20C C20' H20F 127.2 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C21 O10 Pb1 132.6(4) . . ? C21 N2 C24 120.7 . . ? C21 N2 C23 120.2 . . ? C24 N2 C23 119.1 . . ? O10 C21 N2 114.0 . . ? O10 C21 C22 126.0 . . ? N2 C21 C22 120.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C22 H23D 100.1 . . ? H22A C22 H23D 12.3 . . ? H22B C22 H23D 106.6 . . ? H22C C22 H23D 121.1 . . ? C21 C22 H23F 116.7 . . ? H22A C22 H23F 125.0 . . ? H22B C22 H23F 27.8 . . ? H22C C22 H23F 82.0 . . ? H23D C22 H23F 127.2 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C23 H22D 107.0 . . ? H23A C23 H22D 48.7 . . ? H23B C23 H22D 142.6 . . ? H23C C23 H22D 64.7 . . ? N2 C23 H22E 132.1 . . ? H23A C23 H22E 64.5 . . ? H23B C23 H22E 45.6 . . ? H23C C23 H22E 117.3 . . ? H22D C23 H22E 101.8 . . ? N2 C23 H22F 113.8 . . ? H23A C23 H22F 108.5 . . ? H23B C23 H22F 106.0 . . ? H23C C23 H22F 4.5 . . ? H22D C23 H22F 65.5 . . ? H22E C23 H22F 112.8 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C24 H24D 104.7 . . ? H24A C24 H24D 140.6 . . ? H24B C24 H24D 38.6 . . ? H24C C24 H24D 75.7 . . ? N2 C24 H24E 114.0 . . ? H24A C24 H24E 40.1 . . ? H24B C24 H24E 70.8 . . ? H24C C24 H24E 133.5 . . ? H24D C24 H24E 107.5 . . ? N2 C24 H24F 65.1 . . ? H24A C24 H24F 100.8 . . ? H24B C24 H24F 51.4 . . ? H24C C24 H24F 148.9 . . ? H24D C24 H24F 76.4 . . ? H24E C24 H24F 68.9 . . ? C21' O10' Pb1 151.2(11) . . ? C21' N2' C23' 119.7 . . ? C21' N2' C24' 119.3 . . ? C23' N2' C24' 120.9 . . ? O10' C21' N2' 113.9 . . ? O10' C21' C22' 126.2 . . ? N2' C21' C22' 119.9 . . ? C21' C22' H23A 113.5 . . ? C21' C22' H23C 107.1 . . ? H23A C22' H23C 130.4 . . ? C21' C22' H22D 109.5 . . ? H23A C22' H22D 63.0 . . ? H23C C22' H22D 127.0 . . ? C21' C22' H22E 109.5 . . ? H23A C22' H22E 48.1 . . ? H23C C22' H22E 92.5 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H23A C22' H22F 136.3 . . ? H23C C22' H22F 20.0 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? N2' C23' H22A 118.0 . . ? N2' C23' H22B 106.4 . . ? H22A C23' H22B 121.7 . . ? N2' C23' H23D 109.5 . . ? H22A C23' H23D 10.9 . . ? H22B C23' H23D 132.6 . . ? N2' C23' H23E 109.5 . . ? H22A C23' H23E 110.6 . . ? H22B C23' H23E 86.0 . . ? H23D C23' H23E 109.5 . . ? N2' C23' H23F 109.5 . . ? H22A C23' H23F 99.3 . . ? H22B C23' H23F 27.2 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? N2' C24' H24A 74.3 . . ? N2' C24' H24B 147.9 . . ? H24A C24' H24B 108.5 . . ? N2' C24' H24C 76.1 . . ? H24A C24' H24C 69.1 . . ? H24B C24' H24C 75.5 . . ? N2' C24' H24D 109.5 . . ? H24A C24' H24D 103.0 . . ? H24B C24' H24D 38.5 . . ? H24C C24' H24D 42.5 . . ? N2' C24' H24E 109.5 . . ? H24A C24' H24E 41.0 . . ? H24B C24' H24E 88.7 . . ? H24C C24' H24E 97.6 . . ? H24D C24' H24E 109.5 . . ? N2' C24' H24F 109.5 . . ? H24A C24' H24F 143.1 . . ? H24B C24' H24F 87.6 . . ? H24C C24' H24F 147.7 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C41 O11 Pb2 142.9(7) . . ? C41 N4 C44 122.8 . . ? C41 N4 C43 123.0 . . ? C44 N4 C43 114.3 . . ? O11 C41 N4 120.9 . . ? O11 C41 C42 120.0 . . ? N4 C41 C42 119.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C42 H44D 109.6 . . ? H42A C42 H44D 53.2 . . ? H42B C42 H44D 59.3 . . ? H42C C42 H44D 140.8 . . ? C41 C42 H44E 104.9 . . ? H42A C42 H44E 136.9 . . ? H42B C42 H44E 32.4 . . ? H42C C42 H44E 81.7 . . ? H44D C42 H44E 91.4 . . ? C41 C42 H44F 104.6 . . ? H42A C42 H44F 127.1 . . ? H42B C42 H44F 95.3 . . ? H42C C42 H44F 18.7 . . ? H44D C42 H44F 142.5 . . ? H44E C42 H44F 65.0 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C43 H43D 83.1 . . ? H43A C43 H43D 146.6 . . ? H43B C43 H43D 94.0 . . ? H43C C43 H43D 38.3 . . ? N4 C43 H43E 153.4 . . ? H43A C43 H43E 73.2 . . ? H43B C43 H43E 93.6 . . ? H43C C43 H43E 48.1 . . ? H43D C43 H43E 82.2 . . ? N4 C43 H43F 79.8 . . ? H43A C43 H43F 135.1 . . ? H43B C43 H43F 32.9 . . ? H43C C43 H43F 107.9 . . ? H43D C43 H43F 76.4 . . ? H43E C43 H43F 117.8 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N4 C44 H42D 114.9 . . ? H44A C44 H42D 51.2 . . ? H44B C44 H42D 135.4 . . ? H44C C44 H42D 59.6 . . ? N4 C44 H42E 112.4 . . ? H44A C44 H42E 28.3 . . ? H44B C44 H42E 82.5 . . ? H44C C44 H42E 129.0 . . ? H42D C44 H42E 77.0 . . ? N4 C44 H42F 114.8 . . ? H44A C44 H42F 117.4 . . ? H44B C44 H42F 95.1 . . ? H44C C44 H42F 14.5 . . ? H42D C44 H42F 70.7 . . ? H42E C44 H42F 130.5 . . ? C41' O11' Pb2 133.4(5) . . ? C41' N4' C44' 123.3 . . ? C41' N4' C43' 122.7 . . ? C44' N4' C43' 114.0 . . ? O11' C41' N4' 120.5 . . ? O11' C41' C42' 122.3 . . ? N4' C41' C42' 117.3 . . ? C41' C42' H44A 107.8 . . ? C41' C42' H44B 111.0 . . ? H44A C42' H44B 74.5 . . ? C41' C42' H44C 102.9 . . ? H44A C42' H44C 144.0 . . ? H44B C42' H44C 77.2 . . ? C41' C42' H42D 109.5 . . ? H44A C42' H42D 82.8 . . ? H44B C42' H42D 138.0 . . ? H44C C42' H42D 104.5 . . ? C41' C42' H42E 109.5 . . ? H44A C42' H42E 29.9 . . ? H44B C42' H42E 45.1 . . ? H44C C42' H42E 120.5 . . ? H42D C42' H42E 109.5 . . ? C41' C42' H42F 109.5 . . ? H44A C42' H42F 133.4 . . ? H44B C42' H42F 66.7 . . ? H44C C42' H42F 11.1 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? N4' C43' H43A 70.8 . . ? N4' C43' H43B 120.8 . . ? H43A C43' H43B 75.6 . . ? N4' C43' H43C 106.2 . . ? H43A C43' H43C 86.8 . . ? H43B C43' H43C 119.2 . . ? N4' C43' H43D 109.5 . . ? H43A C43' H43D 150.5 . . ? H43B C43' H43D 123.1 . . ? H43C C43' H43D 64.5 . . ? N4' C43' H43E 109.5 . . ? H43A C43' H43E 47.8 . . ? H43B C43' H43E 78.4 . . ? H43C C43' H43E 49.4 . . ? H43D C43' H43E 109.5 . . ? N4' C43' H43F 109.5 . . ? H43A C43' H43F 97.5 . . ? H43B C43' H43F 31.1 . . ? H43C C43' H43F 143.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? N4' C44' H42B 117.7 . . ? N4' C44' H42C 116.6 . . ? H42B C44' H42C 115.0 . . ? N4' C44' H44D 109.5 . . ? H42B C44' H44D 54.0 . . ? H42C C44' H44D 76.3 . . ? N4' C44' H44E 109.5 . . ? H42B C44' H44E 56.2 . . ? H42C C44' H44E 128.3 . . ? H44D C44' H44E 109.5 . . ? N4' C44' H44F 109.5 . . ? H42B C44' H44F 132.8 . . ? H42C C44' H44F 33.7 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C27 O13 Pb2 121.9(4) . . ? C27 N3 C29 124.4 . . ? C27 N3 C30 124.7 . . ? C29 N3 C30 110.8 . . ? C27 N3 H28E 137.5 . . ? C29 N3 H28E 13.1 . . ? C30 N3 H28E 97.8 . . ? C27 N3 H30D 150.0 . . ? C29 N3 H30D 84.9 . . ? C30 N3 H30D 26.8 . . ? H28E N3 H30D 72.0 . . ? O13 C27 N3 110.6 . . ? O13 C27 C28 128.6 . . ? N3 C27 C28 120.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C28 H29D 117.0 . . ? H28A C28 H29D 68.8 . . ? H28B C28 H29D 41.4 . . ? H28C C28 H29D 131.1 . . ? C27 C28 H29E 121.7 . . ? H28A C28 H29E 128.5 . . ? H28B C28 H29E 49.8 . . ? H28C C28 H29E 59.9 . . ? H29D C28 H29E 82.8 . . ? C27 C28 H29F 111.7 . . ? H28A C28 H29F 88.7 . . ? H28B C28 H29F 125.4 . . ? H28C C28 H29F 22.0 . . ? H29D C28 H29F 130.7 . . ? H29E C28 H29F 78.3 . . ? N3 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C29 H28D 106.3 . . ? H29A C29 H28D 63.8 . . ? H29B C29 H28D 143.5 . . ? H29C C29 H28D 49.9 . . ? N3 C29 H28E 79.4 . . ? H29A C29 H28E 77.6 . . ? H29B C29 H28E 55.5 . . ? H29C C29 H28E 164.9 . . ? H28D C29 H28E 140.9 . . ? N3 C29 H28F 103.7 . . ? H29A C29 H28F 132.4 . . ? H29B C29 H28F 89.8 . . ? H29C C29 H28F 24.9 . . ? H28D C29 H28F 74.7 . . ? H28E C29 H28F 142.8 . . ? N3 C30 H30A 109.5 . . ? N3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C30 H30D 74.9 . . ? H30A C30 H30D 91.3 . . ? H30B C30 H30D 48.1 . . ? H30C C30 H30D 154.8 . . ? N3 C30 H30E 123.6 . . ? H30A C30 H30E 107.7 . . ? H30B C30 H30E 96.0 . . ? H30C C30 H30E 16.0 . . ? H30D C30 H30E 143.9 . . ? N3 C30 H30F 110.5 . . ? H30A C30 H30F 19.4 . . ? H30B C30 H30F 124.5 . . ? H30C C30 H30F 91.6 . . ? H30D C30 H30F 110.5 . . ? H30E C30 H30F 92.6 . . ? C27' O13' Pb2 131.3(10) . . ? C27' N3' C29' 124.0 . . ? C27' N3' C30' 124.1 . . ? C29' N3' C30' 112.0 . . ? O13' C27' N3' 110.6 . . ? O13' C27' C28' 128.3 . . ? N3' C27' C28' 121.0 . . ? C27' C28' H29A 119.0 . . ? C27' C28' H29B 122.5 . . ? H29A C28' H29B 68.0 . . ? C27' C28' H29C 129.3 . . ? H29A C28' H29C 109.3 . . ? H29B C28' H29C 88.6 . . ? C27' C28' H28D 109.5 . . ? H29A C28' H28D 63.5 . . ? H29B C28' H28D 121.1 . . ? H29C C28' H28D 78.0 . . ? C27' C28' H28E 109.5 . . ? H29A C28' H28E 46.4 . . ? H29B C28' H28E 30.5 . . ? H29C C28' H28E 114.8 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 109.5 . . ? H29A C28' H28F 130.7 . . ? H29B C28' H28F 79.0 . . ? H29C C28' H28F 32.4 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? N3' C29' H28A 112.9 . . ? N3' C29' H28B 96.6 . . ? H28A C29' H28B 86.7 . . ? N3' C29' H28C 103.3 . . ? H28A C29' H28C 86.9 . . ? H28B C29' H28C 160.1 . . ? N3' C29' H29D 109.5 . . ? H28A C29' H29D 45.5 . . ? H28B C29' H29D 41.2 . . ? H28C C29' H29D 129.6 . . ? N3' C29' H29E 109.5 . . ? H28A C29' H29E 136.2 . . ? H28B C29' H29E 78.2 . . ? H28C C29' H29E 93.7 . . ? H29D C29' H29E 109.5 . . ? N3' C29' H29F 109.5 . . ? H28A C29' H29F 65.7 . . ? H28B C29' H29F 147.5 . . ? H28C C29' H29F 21.2 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? N3' C30' H30A 121.0 . . ? N3' C30' H30B 129.4 . . ? H30A C30' H30B 92.5 . . ? N3' C30' H30C 93.8 . . ? H30A C30' H30C 130.7 . . ? H30B C30' H30C 89.6 . . ? N3' C30' H30D 109.5 . . ? H30A C30' H30D 82.9 . . ? H30B C30' H30D 33.1 . . ? H30C C30' H30D 119.6 . . ? N3' C30' H30E 109.5 . . ? H30A C30' H30E 120.2 . . ? H30B C30' H30E 77.3 . . ? H30C C30' H30E 16.0 . . ? H30D C30' H30E 109.5 . . ? N3' C30' H30F 109.5 . . ? H30A C30' H30F 26.6 . . ? H30B C30' H30F 115.0 . . ? H30C C30' H30F 113.7 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? O3 Pb1 O1 82.81(16) 3_646 . ? O3 Pb1 O9 79.7(2) 3_646 . ? O1 Pb1 O9 83.9(2) . . ? O3 Pb1 O9' 80.3(6) 3_646 . ? O1 Pb1 O9' 95.2(6) . . ? O9 Pb1 O9' 11.3(6) . . ? O3 Pb1 O10' 77.8(4) 3_646 . ? O1 Pb1 O10' 85.9(5) . . ? O9 Pb1 O10' 156.2(5) . . ? O9' Pb1 O10' 157.7(7) . . ? O3 Pb1 O10 77.6(2) 3_646 . ? O1 Pb1 O10 75.3(2) . . ? O9 Pb1 O10 150.8(2) . . ? O9' Pb1 O10 156.8(6) . . ? O10' Pb1 O10 10.6(5) . . ? O3 Pb1 O4 50.94(15) 3_646 3_646 ? O1 Pb1 O4 132.72(16) . 3_646 ? O9 Pb1 O4 95.3(2) . 3_646 ? O9' Pb1 O4 87.0(5) . 3_646 ? O10' Pb1 O4 76.2(5) . 3_646 ? O10 Pb1 O4 84.5(2) . 3_646 ? O7 Pb2 O5 82.23(17) 4_557 1_655 ? O7 Pb2 O6 81.24(18) 4_557 1_655 ? O5 Pb2 O6 51.91(15) 1_655 1_655 ? O7 Pb2 O11' 99.4(3) 4_557 . ? O5 Pb2 O11' 131.5(3) 1_655 . ? O6 Pb2 O11' 80.2(3) 1_655 . ? O7 Pb2 O2 85.11(18) 4_557 . ? O5 Pb2 O2 77.71(14) 1_655 . ? O6 Pb2 O2 129.00(15) 1_655 . ? O11' Pb2 O2 150.8(3) . . ? O7 Pb2 O11 92.7(3) 4_557 . ? O5 Pb2 O11 125.7(3) 1_655 . ? O6 Pb2 O11 73.8(3) 1_655 . ? O11' Pb2 O11 8.6(5) . . ? O2 Pb2 O11 156.1(3) . . ? O7 Pb2 O8 51.52(16) 4_557 4_557 ? O5 Pb2 O8 130.88(17) 1_655 4_557 ? O6 Pb2 O8 122.77(17) 1_655 4_557 ? O11' Pb2 O8 78.4(3) . 4_557 ? O2 Pb2 O8 82.26(17) . 4_557 ? O11 Pb2 O8 77.8(3) . 4_557 ? O7 Pb2 C15 82.39(17) 4_557 1_655 ? O5 Pb2 C15 26.27(16) 1_655 1_655 ? O6 Pb2 C15 25.73(16) 1_655 1_655 ? O11' Pb2 C15 105.3(3) . 1_655 ? O2 Pb2 C15 103.88(17) . 1_655 ? O11 Pb2 C15 99.4(3) . 1_655 ? O8 Pb2 C15 133.19(16) 4_557 1_655 ? O7 Pb2 O13 162.8(2) 4_557 . ? O5 Pb2 O13 81.6(2) 1_655 . ? O6 Pb2 O13 84.2(3) 1_655 . ? O11' Pb2 O13 87.0(3) . . ? O2 Pb2 O13 97.1(2) . . ? O11 Pb2 O13 92.0(3) . . ? O8 Pb2 O13 145.6(2) 4_557 . ? C15 Pb2 O13 80.5(2) 1_655 . ? O7 Pb2 O13' 167.2(4) 4_557 . ? O5 Pb2 O13' 85.2(4) 1_655 . ? O6 Pb2 O13' 93.1(4) 1_655 . ? O11' Pb2 O13' 90.9(4) . . ? O2 Pb2 O13' 89.6(4) . . ? O11 Pb2 O13' 96.9(4) . . ? O8 Pb2 O13' 139.2(4) 4_557 . ? C15 Pb2 O13' 87.6(4) 1_655 . ? O13 Pb2 O13' 9.2(4) . . ? C13 O1 Pb1 101.6(4) . . ? C13 O2 Pb2 161.7(5) . . ? C14 O3 Pb1 100.1(4) . 3_656 ? C14 O4 Pb1 84.4(4) . 3_656 ? C15 O5 Pb2 92.1(4) . 1_455 ? C15 O6 Pb2 92.7(4) . 1_455 ? C16 O7 Pb2 101.2(4) . 4_457 ? C16 O8 Pb2 83.2(4) . 4_457 ? C6 C1 C2 118.6(5) . . ? C6 C1 C7 120.8(5) . . ? C2 C1 C7 120.5(5) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 C13 115.3(5) . . ? C1 C2 C13 125.1(5) . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C14 120.6(6) . . ? C3 C4 C14 121.1(6) . . ? C4 C5 C6 120.8(6) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 120.8(6) . . ? C1 C6 C15 124.1(5) . . ? C5 C6 C15 114.9(5) . . ? C8 C7 C12 119.0(6) . . ? C8 C7 C1 122.6(6) . . ? C12 C7 C1 118.4(5) . . ? C7 C8 C9 120.6(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 C16 118.3(6) . . ? C9 C10 C16 121.6(6) . . ? C10 C11 C12 119.9(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.1(6) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O1 C13 O2 124.4(6) . . ? O1 C13 C2 118.7(6) . . ? O2 C13 C2 116.7(6) . . ? O4 C14 O3 124.3(6) . . ? O4 C14 C4 118.3(6) . . ? O3 C14 C4 117.4(6) . . ? O6 C15 O5 122.9(6) . . ? O6 C15 C6 118.1(6) . . ? O5 C15 C6 118.7(6) . . ? O6 C15 Pb2 61.6(3) . 1_455 ? O5 C15 Pb2 61.7(3) . 1_455 ? C6 C15 Pb2 169.2(4) . 1_455 ? O8 C16 O7 123.1(6) . . ? O8 C16 C10 121.0(6) . . ? O7 C16 C10 115.8(6) . . ? 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 Pb1 O9 C17 N1 -174.9(5) . . . . ? Pb1 O9 C17 C18 4.9(5) . . . . ? C19 N1 C17 O9 0.2 . . . . ? C20 N1 C17 O9 -179.9 . . . . ? C19 N1 C17 C18 -179.6 . . . . ? C20 N1 C17 C18 0.3 . . . . ? Pb1 O9' C17' N1' 158(2) . . . . ? Pb1 O9' C17' C18' -22(2) . . . . ? C19' N1' C17' O9' 0.0 . . . . ? C20' N1' C17' O9' 180.0 . . . . ? C19' N1' C17' C18' -179.9 . . . . ? C20' N1' C17' C18' 0.0 . . . . ? Pb1 O10 C21 N2 -172.7(5) . . . . ? Pb1 O10 C21 C22 7.4(5) . . . . ? C24 N2 C21 O10 179.9 . . . . ? C23 N2 C21 O10 -0.1 . . . . ? C24 N2 C21 C22 -0.1 . . . . ? C23 N2 C21 C22 179.8 . . . . ? Pb1 O10' C21' N2' 128.9(19) . . . . ? Pb1 O10' C21' C22' -51.1(19) . . . . ? C23' N2' C21' O10' 0.0 . . . . ? C24' N2' C21' O10' -180.0 . . . . ? C23' N2' C21' C22' -180.0 . . . . ? C24' N2' C21' C22' 0.1 . . . . ? Pb2 O11 C41 N4 -85.4(10) . . . . ? Pb2 O11 C41 C42 94.7(10) . . . . ? C44 N4 C41 O11 0.0 . . . . ? C43 N4 C41 O11 -180.0 . . . . ? C44 N4 C41 C42 179.9 . . . . ? C43 N4 C41 C42 0.0 . . . . ? Pb2 O11' C41' N4' 157.3(9) . . . . ? Pb2 O11' C41' C42' -22.7(9) . . . . ? C44' N4' C41' O11' -0.1 . . . . ? C43' N4' C41' O11' 179.9 . . . . ? C44' N4' C41' C42' 179.8 . . . . ? C43' N4' C41' C42' -0.1 . . . . ? Pb2 O13 C27 N3 -135.1(6) . . . . ? Pb2 O13 C27 C28 44.7(6) . . . . ? C29 N3 C27 O13 0.1 . . . . ? C30 N3 C27 O13 -179.9 . . . . ? C29 N3 C27 C28 -179.7 . . . . ? C30 N3 C27 C28 0.3 . . . . ? Pb2 O13' C27' N3' 107.2(10) . . . . ? Pb2 O13' C27' C28' -72.8(10) . . . . ? C29' N3' C27' O13' 0.0 . . . . ? C30' N3' C27' O13' 180.0 . . . . ? C29' N3' C27' C28' -180.0 . . . . ? C30' N3' C27' C28' 0.0 . . . . ? C17 O9 Pb1 O3 62.9(5) . . . 3_646 ? C17 O9 Pb1 O1 146.6(5) . . . . ? C17 O9 Pb1 O9' -29(3) . . . . ? C17 O9 Pb1 O10' 81.6(14) . . . . ? C17 O9 Pb1 O10 102.3(7) . . . . ? C17 O9 Pb1 O4 14.2(5) . . . 3_646 ? C17' O9' Pb1 O3 -84(2) . . . 3_646 ? C17' O9' Pb1 O1 -2(2) . . . . ? C17' O9' Pb1 O9 2.3(18) . . . . ? C17' O9' Pb1 O10' -94(3) . . . . ? C17' O9' Pb1 O10 -66(3) . . . . ? C17' O9' Pb1 O4 -135(2) . . . 3_646 ? C21' O10' Pb1 O3 96.8(18) . . . 3_646 ? C21' O10' Pb1 O1 13.3(18) . . . . ? C21' O10' Pb1 O9 78(2) . . . . ? C21' O10' Pb1 O9' 107(2) . . . . ? C21' O10' Pb1 O10 8.7(18) . . . . ? C21' O10' Pb1 O4 149.2(19) . . . 3_646 ? C21 O10 Pb1 O3 -127.6(6) . . . 3_646 ? C21 O10 Pb1 O1 146.7(6) . . . . ? C21 O10 Pb1 O9 -167.4(5) . . . . ? C21 O10 Pb1 O9' -145.4(14) . . . . ? C21 O10 Pb1 O10' -38(3) . . . . ? C21 O10 Pb1 O4 -76.4(6) . . . 3_646 ? C41' O11' Pb2 O7 140.4(8) . . . 4_557 ? C41' O11' Pb2 O5 52.5(10) . . . 1_655 ? C41' O11' Pb2 O6 61.1(8) . . . 1_655 ? C41' O11' Pb2 O2 -122.7(8) . . . . ? C41' O11' Pb2 O11 102(3) . . . . ? C41' O11' Pb2 O8 -172.3(9) . . . 4_557 ? C41' O11' Pb2 C15 55.8(9) . . . 1_655 ? C41' O11' Pb2 O13 -23.6(9) . . . . ? C41' O11' Pb2 O13' -32.0(9) . . . . ? C41 O11 Pb2 O7 -145.2(9) . . . 4_557 ? C41 O11 Pb2 O5 132.5(8) . . . 1_655 ? C41 O11 Pb2 O6 134.7(9) . . . 1_655 ? C41 O11 Pb2 O11' -3(2) . . . . ? C41 O11 Pb2 O2 -61.3(11) . . . . ? C41 O11 Pb2 O8 -95.5(9) . . . 4_557 ? C41 O11 Pb2 C15 132.1(8) . . . 1_655 ? C41 O11 Pb2 O13 51.3(9) . . . . ? C41 O11 Pb2 O13' 43.4(10) . . . . ? C27 O13 Pb2 O7 76.1(10) . . . 4_557 ? C27 O13 Pb2 O5 56.1(5) . . . 1_655 ? C27 O13 Pb2 O6 108.4(5) . . . 1_655 ? C27 O13 Pb2 O11' -171.2(6) . . . . ? C27 O13 Pb2 O2 -20.3(5) . . . . ? C27 O13 Pb2 O11 -178.1(5) . . . . ? C27 O13 Pb2 O8 -106.9(5) . . . 4_557 ? C27 O13 Pb2 C15 82.7(5) . . . 1_655 ? C27 O13 Pb2 O13' -56(3) . . . . ? C27' O13' Pb2 O7 -35(2) . . . 4_557 ? C27' O13' Pb2 O5 -23.0(8) . . . 1_655 ? C27' O13' Pb2 O6 28.4(9) . . . 1_655 ? C27' O13' Pb2 O11' 108.6(9) . . . . ? C27' O13' Pb2 O2 -100.7(9) . . . . ? C27' O13' Pb2 O11 102.4(9) . . . . ? C27' O13' Pb2 O8 -178.3(6) . . . 4_557 ? C27' O13' Pb2 C15 3.3(9) . . . 1_655 ? C27' O13' Pb2 O13 44(2) . . . . ? O3 Pb1 O1 C13 -154.8(4) 3_646 . . . ? O9 Pb1 O1 C13 124.8(4) . . . . ? O9' Pb1 O1 C13 125.7(7) . . . . ? O10' Pb1 O1 C13 -76.7(6) . . . . ? O10 Pb1 O1 C13 -75.8(4) . . . . ? O4 Pb1 O1 C13 -143.6(4) 3_646 . . . ? O7 Pb2 O2 C13 43.6(14) 4_557 . . . ? O5 Pb2 O2 C13 126.7(14) 1_655 . . . ? O6 Pb2 O2 C13 118.2(14) 1_655 . . . ? O11' Pb2 O2 C13 -57.0(16) . . . . ? O11 Pb2 O2 C13 -41.9(17) . . . . ? O8 Pb2 O2 C13 -8.2(14) 4_557 . . . ? C15 Pb2 O2 C13 124.5(14) 1_655 . . . ? O13 Pb2 O2 C13 -153.6(14) . . . . ? O13' Pb2 O2 C13 -148.1(15) . . . . ? C6 C1 C2 C3 -1.0(9) . . . . ? C7 C1 C2 C3 176.4(6) . . . . ? C6 C1 C2 C13 179.7(6) . . . . ? C7 C1 C2 C13 -2.9(9) . . . . ? C1 C2 C3 C4 -2.5(10) . . . . ? C13 C2 C3 C4 176.9(6) . . . . ? C2 C3 C4 C5 2.3(10) . . . . ? C2 C3 C4 C14 -177.9(6) . . . . ? C3 C4 C5 C6 1.4(10) . . . . ? C14 C4 C5 C6 -178.5(6) . . . . ? C2 C1 C6 C5 4.6(9) . . . . ? C7 C1 C6 C5 -172.8(5) . . . . ? C2 C1 C6 C15 -169.8(6) . . . . ? C7 C1 C6 C15 12.9(9) . . . . ? C4 C5 C6 C1 -4.9(10) . . . . ? C4 C5 C6 C15 170.0(6) . . . . ? C6 C1 C7 C8 -132.9(6) . . . . ? C2 C1 C7 C8 49.8(8) . . . . ? C6 C1 C7 C12 48.7(8) . . . . ? C2 C1 C7 C12 -128.6(6) . . . . ? C12 C7 C8 C9 0.2(9) . . . . ? C1 C7 C8 C9 -178.2(6) . . . . ? C7 C8 C9 C10 0.5(10) . . . . ? C8 C9 C10 C11 0.0(10) . . . . ? C8 C9 C10 C16 176.0(6) . . . . ? C9 C10 C11 C12 -1.2(10) . . . . ? C16 C10 C11 C12 -177.3(6) . . . . ? C10 C11 C12 C7 1.9(10) . . . . ? C8 C7 C12 C11 -1.4(9) . . . . ? C1 C7 C12 C11 177.0(6) . . . . ? Pb1 O1 C13 O2 -14.4(7) . . . . ? Pb1 O1 C13 C2 160.5(4) . . . . ? Pb2 O2 C13 O1 -78.8(16) . . . . ? Pb2 O2 C13 C2 106.2(14) . . . . ? C3 C2 C13 O1 -110.9(7) . . . . ? C1 C2 C13 O1 68.4(8) . . . . ? C3 C2 C13 O2 64.4(8) . . . . ? C1 C2 C13 O2 -116.3(7) . . . . ? Pb1 O4 C14 O3 -4.7(7) 3_656 . . . ? Pb1 O4 C14 C4 175.5(6) 3_656 . . . ? Pb1 O3 C14 O4 5.4(8) 3_656 . . . ? Pb1 O3 C14 C4 -174.8(5) 3_656 . . . ? C5 C4 C14 O4 -4.9(10) . . . . ? C3 C4 C14 O4 175.3(7) . . . . ? C5 C4 C14 O3 175.3(6) . . . . ? C3 C4 C14 O3 -4.5(10) . . . . ? Pb2 O6 C15 O5 -6.8(7) 1_455 . . . ? Pb2 O6 C15 C6 167.8(5) 1_455 . . . ? Pb2 O5 C15 O6 6.8(7) 1_455 . . . ? Pb2 O5 C15 C6 -167.8(5) 1_455 . . . ? C1 C6 C15 O6 62.1(9) . . . . ? C5 C6 C15 O6 -112.6(7) . . . . ? C1 C6 C15 O5 -123.1(7) . . . . ? C5 C6 C15 O5 62.3(8) . . . . ? C1 C6 C15 Pb2 148(2) . . . 1_455 ? C5 C6 C15 Pb2 -27(3) . . . 1_455 ? Pb2 O8 C16 O7 -9.1(7) 4_457 . . . ? Pb2 O8 C16 C10 169.6(6) 4_457 . . . ? Pb2 O7 C16 O8 10.9(8) 4_457 . . . ? Pb2 O7 C16 C10 -167.8(5) 4_457 . . . ? C11 C10 C16 O8 0.3(10) . . . . ? C9 C10 C16 O8 -175.8(7) . . . . ? C11 C10 C16 O7 179.0(6) . . . . ? C9 C10 C16 O7 3.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.622 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.089 data_bb _database_code_depnum_ccdc_archive 'CCDC 928611' #TrackingRef 'Zn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H6 O8 Zn2' _chemical_formula_weight 456.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.213(5) _cell_length_b 14.723(6) _cell_length_c 8.994(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.105(4) _cell_angle_gamma 90.00 _cell_volume 1537.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2220 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.17 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 3.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5296 _exptl_absorpt_correction_T_max 0.7221 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5276 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1440 _reflns_number_gt 1260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+2.3128P] 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 1440 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.64465(2) -0.462383(17) 0.89715(3) 0.01848(10) Uani 1 1 d . . . O1 O 0.59117(16) -0.34309(11) 0.8279(2) 0.0370(5) Uani 1 1 d . . . O2 O 0.80689(14) -0.03381(12) 0.87212(19) 0.0267(4) Uani 1 1 d . . . O3 O 0.70737(14) 0.02286(11) 0.6432(2) 0.0247(4) Uani 1 1 d . . . O4 O 0.56520(15) 0.42228(11) 0.8691(2) 0.0260(4) Uani 1 1 d . . . C1 C 0.5000 -0.3048(2) 0.7500 0.0229(8) Uani 1 2 d S . . C2 C 0.5000 -0.2029(2) 0.7500 0.0189(7) Uani 1 2 d S . . C3 C 0.6028(2) -0.15579(15) 0.7826(3) 0.0183(5) Uani 1 1 d . . . H3 H 0.6723 -0.1872 0.8103 0.022 Uiso 1 1 calc R . . C4 C 0.6024(2) -0.06116(15) 0.7740(3) 0.0168(5) Uani 1 1 d . . . C5 C 0.5000 -0.0114(2) 0.7500 0.0156(7) Uani 1 2 d S . . C6 C 0.5000 0.0902(2) 0.7500 0.0179(7) Uani 1 2 d S . . C7 C 0.5790(2) 0.13884(16) 0.8685(3) 0.0251(6) Uani 1 1 d . . . H7 H 0.6329 0.1077 0.9483 0.030 Uiso 1 1 calc R . . C8 C 0.5783(2) 0.23297(16) 0.8692(3) 0.0259(6) Uani 1 1 d . . . H8 H 0.6308 0.2643 0.9503 0.031 Uiso 1 1 calc R . . C9 C 0.5000 0.2810(2) 0.7500 0.0206(7) Uani 1 2 d S . . C10 C 0.5000 0.3830(2) 0.7500 0.0200(7) Uani 1 2 d S . . C11 C 0.7130(2) -0.01912(15) 0.7671(3) 0.0177(5) 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 Zn1 0.01692(16) 0.01144(15) 0.02441(16) -0.00042(12) 0.00254(11) 0.00125(11) O1 0.0279(11) 0.0131(9) 0.0616(14) 0.0055(9) 0.0018(10) 0.0045(8) O2 0.0174(9) 0.0393(11) 0.0216(9) -0.0022(8) 0.0034(7) -0.0026(8) O3 0.0210(9) 0.0249(10) 0.0277(9) 0.0056(8) 0.0067(7) -0.0024(7) O4 0.0313(10) 0.0134(8) 0.0288(10) -0.0038(7) 0.0027(8) -0.0066(8) C1 0.025(2) 0.0148(18) 0.032(2) 0.000 0.0132(16) 0.000 C2 0.0208(18) 0.0112(17) 0.0235(18) 0.000 0.0053(14) 0.000 C3 0.0151(12) 0.0150(12) 0.0229(12) 0.0000(10) 0.0034(10) 0.0024(9) C4 0.0178(12) 0.0134(12) 0.0171(11) 0.0000(9) 0.0025(10) -0.0011(9) C5 0.0178(17) 0.0127(16) 0.0153(16) 0.000 0.0036(13) 0.000 C6 0.0200(18) 0.0120(17) 0.0224(17) 0.000 0.0076(14) 0.000 C7 0.0256(14) 0.0152(12) 0.0264(14) 0.0017(10) -0.0037(11) 0.0011(10) C8 0.0279(15) 0.0163(13) 0.0247(13) -0.0019(10) -0.0045(11) -0.0024(11) C9 0.0217(19) 0.0113(16) 0.0277(19) 0.000 0.0063(15) 0.000 C10 0.0218(18) 0.0139(17) 0.0258(18) 0.000 0.0094(15) 0.000 C11 0.0193(12) 0.0113(12) 0.0225(12) -0.0067(9) 0.0065(10) -0.0014(9) _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 O1 1.9094(18) . ? Zn1 O4 1.9329(17) 1_545 ? Zn1 O3 1.9630(18) 4_646 ? Zn1 O2 1.9739(18) 7_647 ? O1 C1 1.250(2) . ? O2 C11 1.257(3) . ? O2 Zn1 1.9739(18) 7_647 ? O3 C11 1.257(3) . ? O3 Zn1 1.9630(18) 4_656 ? O4 C10 1.260(2) . ? O4 Zn1 1.9329(17) 1_565 ? C1 O1 1.250(2) 2_656 ? C1 C2 1.501(5) . ? C2 C3 1.384(3) . ? C2 C3 1.384(3) 2_656 ? C3 C4 1.395(3) . ? C3 H3 0.9300 . ? C4 C5 1.407(3) . ? C4 C11 1.504(3) . ? C5 C4 1.407(3) 2_656 ? C5 C6 1.495(4) . ? C6 C7 1.393(3) . ? C6 C7 1.393(3) 2_656 ? C7 C8 1.386(3) . ? C7 H7 0.9300 . ? C8 C9 1.388(3) . ? C8 H8 0.9300 . ? C9 C8 1.388(3) 2_656 ? C9 C10 1.501(5) . ? C10 O4 1.260(2) 2_656 ? 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 O1 Zn1 O4 131.19(8) . 1_545 ? O1 Zn1 O3 106.43(8) . 4_646 ? O4 Zn1 O3 109.41(7) 1_545 4_646 ? O1 Zn1 O2 109.23(8) . 7_647 ? O4 Zn1 O2 94.96(7) 1_545 7_647 ? O3 Zn1 O2 101.47(7) 4_646 7_647 ? C1 O1 Zn1 138.76(19) . . ? C11 O2 Zn1 134.42(16) . 7_647 ? C11 O3 Zn1 114.75(15) . 4_656 ? C10 O4 Zn1 132.32(17) . 1_565 ? O1 C1 O1 126.5(3) 2_656 . ? O1 C1 C2 116.77(16) 2_656 . ? O1 C1 C2 116.77(16) . . ? C3 C2 C3 119.8(3) . 2_656 ? C3 C2 C1 120.09(14) . . ? C3 C2 C1 120.09(14) 2_656 . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 121.1(2) . . ? C3 C4 C11 115.2(2) . . ? C5 C4 C11 123.1(2) . . ? C4 C5 C4 117.2(3) 2_656 . ? C4 C5 C6 121.40(14) 2_656 . ? C4 C5 C6 121.40(14) . . ? C7 C6 C7 118.1(3) . 2_656 ? C7 C6 C5 120.96(15) . . ? C7 C6 C5 120.96(15) 2_656 . ? C8 C7 C6 121.0(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.6(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C8 118.7(3) 2_656 . ? C8 C9 C10 120.64(15) 2_656 . ? C8 C9 C10 120.64(15) . . ? O4 C10 O4 125.3(3) . 2_656 ? O4 C10 C9 117.33(15) . . ? O4 C10 C9 117.33(15) 2_656 . ? O2 C11 O3 122.4(2) . . ? O2 C11 C4 121.3(2) . . ? O3 C11 C4 115.9(2) . . ? 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 O4 Zn1 O1 C1 -1.3(3) 1_545 . . . ? O3 Zn1 O1 C1 134.6(2) 4_646 . . . ? O2 Zn1 O1 C1 -116.6(2) 7_647 . . . ? Zn1 O1 C1 O1 -9.15(16) . . . 2_656 ? Zn1 O1 C1 C2 170.85(16) . . . . ? O1 C1 C2 C3 -156.81(15) 2_656 . . . ? O1 C1 C2 C3 23.19(15) . . . . ? O1 C1 C2 C3 23.19(15) 2_656 . . 2_656 ? O1 C1 C2 C3 -156.81(15) . . . 2_656 ? C3 C2 C3 C4 -3.60(16) 2_656 . . . ? C1 C2 C3 C4 176.40(16) . . . . ? C2 C3 C4 C5 7.3(3) . . . . ? C2 C3 C4 C11 -163.67(18) . . . . ? C3 C4 C5 C4 -3.63(16) . . . 2_656 ? C11 C4 C5 C4 166.6(2) . . . 2_656 ? C3 C4 C5 C6 176.37(16) . . . . ? C11 C4 C5 C6 -13.4(2) . . . . ? C4 C5 C6 C7 131.82(17) 2_656 . . . ? C4 C5 C6 C7 -48.18(17) . . . . ? C4 C5 C6 C7 -48.18(17) 2_656 . . 2_656 ? C4 C5 C6 C7 131.82(17) . . . 2_656 ? C7 C6 C7 C8 0.56(19) 2_656 . . . ? C5 C6 C7 C8 -179.44(19) . . . . ? C6 C7 C8 C9 -1.1(4) . . . . ? C7 C8 C9 C8 0.56(19) . . . 2_656 ? C7 C8 C9 C10 -179.44(19) . . . . ? Zn1 O4 C10 O4 -29.92(13) 1_565 . . 2_656 ? Zn1 O4 C10 C9 150.08(13) 1_565 . . . ? C8 C9 C10 O4 173.02(16) 2_656 . . . ? C8 C9 C10 O4 -6.98(16) . . . . ? C8 C9 C10 O4 -6.98(16) 2_656 . . 2_656 ? C8 C9 C10 O4 173.02(16) . . . 2_656 ? Zn1 O2 C11 O3 143.80(19) 7_647 . . . ? Zn1 O2 C11 C4 -44.0(3) 7_647 . . . ? Zn1 O3 C11 O2 14.0(3) 4_656 . . . ? Zn1 O3 C11 C4 -158.53(15) 4_656 . . . ? C3 C4 C11 O2 -57.0(3) . . . . ? C5 C4 C11 O2 132.2(2) . . . . ? C3 C4 C11 O3 115.7(2) . . . . ? C5 C4 C11 O3 -55.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.343 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.067