# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A # 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_1 #TrackingRef 'Pb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H42 O14 Pb3' _chemical_formula_sum 'C69 H42 O14 Pb3' _chemical_formula_weight 1716.60 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 26.4685(12) _cell_length_b 22.6646(11) _cell_length_c 40.1626(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.1710(10) _cell_angle_gamma 90.00 _cell_volume 23714.8(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7673 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 20.21 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6512 _exptl_absorpt_coefficient_mu 4.283 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2791 _exptl_absorpt_correction_T_max 0.2791 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60662 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.25 _reflns_number_total 21458 _reflns_number_gt 11144 _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^)+(0.1345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21458 _refine_ls_number_parameters 775 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2130 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.975 _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 C3 C 0.4421(3) 0.4019(4) 0.0570(3) 0.041(2) Uani 1 1 d . . . C4 C 0.4308(4) 0.4024(4) 0.0179(2) 0.047(2) Uani 1 1 d . . . C8 C 0.3951(4) 0.3179(5) 0.1272(3) 0.051(3) Uani 1 1 d . . . C9 C 0.4154(4) 0.3615(4) 0.0731(3) 0.050(3) Uani 1 1 d . . . C10 C 0.3942(4) 0.4365(4) 0.0008(3) 0.049(3) Uani 1 1 d . . . H10A H 0.3750 0.4603 0.0128 0.059 Uiso 1 1 calc R . . C12 C 0.4244(4) 0.3601(4) 0.1100(3) 0.044(2) Uani 1 1 d . . . C13 C 0.5227(3) 0.4811(4) 0.1305(3) 0.049(3) Uani 1 1 d . . . C14 C 0.3499(4) 0.3323(5) 0.1376(3) 0.062(3) Uani 1 1 d . . . H14A H 0.3357 0.3694 0.1323 0.075 Uiso 1 1 calc R . . C15 C 0.4609(4) 0.3671(5) 0.0008(3) 0.060(3) Uani 1 1 d . . . H15A H 0.4869 0.3444 0.0132 0.072 Uiso 1 1 calc R . . C16 C 0.5572(4) 0.6719(4) 0.1843(3) 0.070(4) Uani 1 1 d . . . H16A H 0.5917 0.6665 0.1830 0.084 Uiso 1 1 calc R . . C17 C 0.5386(4) 0.5707(4) 0.1616(3) 0.054(3) Uani 1 1 d . . . C18 C 0.4133(4) 0.4028(5) -0.0507(3) 0.059(3) Uani 1 1 d . . . H18A H 0.4070 0.4039 -0.0742 0.070 Uiso 1 1 calc R . . C19 C 0.7647(4) 0.4550(5) 0.1955(3) 0.068(3) Uani 1 1 d . . . C20 C 0.5227(4) 0.6288(5) 0.1747(3) 0.055(3) Uani 1 1 d . . . C21 C 0.4828(4) 0.3269(6) -0.0526(3) 0.077(4) Uani 1 1 d . . . C22 C 0.5065(4) 0.5329(4) 0.1419(3) 0.053(3) Uani 1 1 d U . . H22A H 0.4721 0.5429 0.1359 0.063 Uiso 1 1 calc R . . C23 C 0.5738(4) 0.4650(5) 0.1391(3) 0.061(3) Uani 1 1 d . . . H23A H 0.5852 0.4300 0.1309 0.073 Uiso 1 1 calc R . . C24 C 0.4132(4) 0.2599(5) 0.1327(3) 0.061(3) Uani 1 1 d . . . H24A H 0.4428 0.2482 0.1251 0.074 Uiso 1 1 calc R . . C25 C 0.4527(4) 0.3652(5) -0.0344(3) 0.059(3) Uani 1 1 d . . . C26 C 0.3759(4) 0.3196(5) 0.0537(3) 0.078(4) Uani 1 1 d . . . H26A H 0.3739 0.3258 0.0298 0.118 Uiso 1 1 calc R . . H26B H 0.3430 0.3271 0.0597 0.118 Uiso 1 1 calc R . . H26C H 0.3859 0.2796 0.0592 0.118 Uiso 1 1 calc R . . C27 C 0.3837(3) 0.4378(5) -0.0337(3) 0.051(3) Uani 1 1 d . . . C28 C 0.5907(4) 0.5546(5) 0.1711(3) 0.063(3) Uani 1 1 d . . . H28A H 0.6136 0.5793 0.1848 0.076 Uiso 1 1 calc R . . C29 C 0.4716(4) 0.6399(5) 0.1750(4) 0.087(5) Uani 1 1 d . . . H29A H 0.4472 0.6117 0.1664 0.104 Uiso 1 1 calc R . . C30 C 0.5399(4) 0.7265(5) 0.1968(3) 0.070(4) Uani 1 1 d . . . H30A H 0.5642 0.7552 0.2046 0.084 Uiso 1 1 calc R . . C31 C 0.8212(4) 0.4392(6) 0.2105(3) 0.068(3) Uani 1 1 d . . . C32 C 0.3865(4) 0.2193(5) 0.1500(3) 0.071(4) Uani 1 1 d . . . C33 C 0.3435(4) 0.4774(5) -0.0525(3) 0.059(3) Uani 1 1 d . . . C34 C 0.7496(4) 0.5115(6) 0.1947(5) 0.118(7) Uani 1 1 d . . . H34A H 0.7734 0.5400 0.2038 0.142 Uiso 1 1 calc R . . C35 C 0.4042(6) 0.1558(6) 0.1548(4) 0.101(5) Uani 1 1 d . . . C36 C 0.7319(4) 0.4132(5) 0.1803(3) 0.078(4) Uani 1 1 d . . . H36A H 0.7434 0.3749 0.1779 0.094 Uiso 1 1 calc R . . C37 C 0.3243(4) 0.2926(6) 0.1561(3) 0.072(4) Uani 1 1 d . . . C38 C 0.6075(4) 0.5005(5) 0.1596(3) 0.066(3) Uani 1 1 d . . . C39 C 0.4554(4) 0.6936(5) 0.1883(4) 0.081(4) Uani 1 1 d . . . H39A H 0.4212 0.6982 0.1905 0.097 Uiso 1 1 calc R . . C40 C 0.2610(5) 0.5460(7) -0.0856(3) 0.087(4) Uani 1 1 d . . . C41 C 0.2202(7) 0.5821(10) -0.1035(4) 0.112(6) Uani 1 1 d . . . C43 C 0.3737(6) 0.1113(7) 0.1575(4) 0.106(5) Uani 1 1 d . . . H43A H 0.3390 0.1192 0.1563 0.127 Uiso 1 1 calc R . . C44 C 0.3434(5) 0.2383(5) 0.1628(3) 0.081(4) Uani 1 1 d . . . H44A H 0.3279 0.2129 0.1762 0.097 Uiso 1 1 calc R . . C45 C 0.1886(5) 0.3479(6) 0.1918(4) 0.081(4) Uani 1 1 d . . . C46 C 0.2789(4) 0.3134(6) 0.1694(3) 0.068(3) Uani 1 1 d . . . C48 C 0.6637(4) 0.4841(5) 0.1720(3) 0.073(4) Uani 1 1 d . . . C49 C 0.1410(5) 0.3628(7) 0.2054(4) 0.077(4) Uani 1 1 d . . . C50 C 0.5406(5) 0.2532(7) -0.0871(3) 0.094(5) Uani 1 1 d . . . C51 C 0.2427(6) 0.3543(8) 0.1513(4) 0.111(6) Uani 1 1 d . . . H51A H 0.2489 0.3713 0.1313 0.133 Uiso 1 1 calc R . . C52 C 0.4570(5) 0.1463(7) 0.1575(5) 0.120(6) Uani 1 1 d . . . H52A H 0.4793 0.1774 0.1559 0.144 Uiso 1 1 calc R . . C53 C 0.5735(7) 0.2096(8) -0.1027(3) 0.114(7) Uani 1 1 d . . . C54 C 0.2708(5) 0.2955(7) 0.1998(4) 0.103(5) Uani 1 1 d . . . H54A H 0.2949 0.2715 0.2130 0.124 Uiso 1 1 calc R . . C56 C 0.6794(5) 0.4284(5) 0.1681(4) 0.090(5) Uani 1 1 d . . . H56A H 0.6565 0.4002 0.1575 0.109 Uiso 1 1 calc R . . C57 C 0.4755(6) 0.0879(8) 0.1627(5) 0.131(7) Uani 1 1 d . . . H57A H 0.5105 0.0807 0.1652 0.157 Uiso 1 1 calc R . . C59 C 0.2248(5) 0.3129(8) 0.2128(5) 0.124(7) Uani 1 1 d . . . H59 H 0.2196 0.3012 0.2342 0.149 Uiso 1 1 calc R . . C60 C 0.4964(6) 0.2731(9) -0.1008(3) 0.133(8) Uani 1 1 d . . . H60A H 0.4831 0.2608 -0.1227 0.159 Uiso 1 1 calc R . . C61 C 0.4677(6) 0.3107(8) -0.0859(3) 0.132(8) Uani 1 1 d . . . H61A H 0.4374 0.3258 -0.0982 0.158 Uiso 1 1 calc R . . C62 C 0.1998(4) 0.3681(6) 0.1633(4) 0.083(4) Uani 1 1 d . . . H62A H 0.1766 0.3937 0.1506 0.100 Uiso 1 1 calc R . . C63 C 0.3895(6) 0.0535(7) 0.1619(5) 0.113(6) Uani 1 1 d . . . H63A H 0.3657 0.0238 0.1634 0.136 Uiso 1 1 calc R . . C64 C 0.2982(5) 0.5697(8) -0.0600(4) 0.101(5) Uani 1 1 d . . . H64A H 0.2965 0.6091 -0.0536 0.121 Uiso 1 1 calc R . . C65 C 0.7004(5) 0.5296(7) 0.1810(4) 0.117(6) Uani 1 1 d . . . H65A H 0.6918 0.5693 0.1779 0.141 Uiso 1 1 calc R . . C66 C 0.5647(8) 0.2757(9) -0.0556(5) 0.145(7) Uani 1 1 d U . . H66 H 0.5978 0.2653 -0.0455 0.174 Uiso 1 1 calc R . . C67 C 0.4690(7) -0.0214(8) 0.1658(5) 0.175(7) Uani 1 1 d DU . . C68 C 0.3405(5) 0.5309(7) -0.0431(4) 0.095(5) Uani 1 1 d . . . H68A H 0.3648 0.5457 -0.0255 0.114 Uiso 1 1 calc R . . C69 C 0.3084(6) 0.4560(8) -0.0796(5) 0.126(6) Uani 1 1 d . . . H69A H 0.3124 0.4178 -0.0872 0.151 Uiso 1 1 calc R . . C70 C 0.2678(7) 0.4893(8) -0.0956(4) 0.119(6) Uani 1 1 d . . . H70A H 0.2448 0.4732 -0.1135 0.143 Uiso 1 1 calc R . . C71 C 0.4409(7) 0.0398(6) 0.1643(4) 0.112(5) Uani 1 1 d DU . . C72 C 0.5332(7) 0.3168(9) -0.0402(5) 0.136(6) Uani 1 1 d U . . H72A H 0.5484 0.3372 -0.0209 0.164 Uiso 1 1 calc R . . C75 C 0.5066(4) 0.4819(5) 0.0567(3) 0.060(3) Uani 1 1 d . . . H75A H 0.4966 0.4774 0.0327 0.091 Uiso 1 1 calc R . . H75B H 0.5427 0.4742 0.0630 0.091 Uiso 1 1 calc R . . H75C H 0.4995 0.5215 0.0630 0.091 Uiso 1 1 calc R . . C76 C 0.4767(3) 0.4387(4) 0.0746(2) 0.040(2) Uani 1 1 d . . . C79 C 0.4726(3) 0.7942(4) 0.2077(2) 0.043(2) Uani 1 1 d . . . C82 C 0.4856(4) 0.4380(4) 0.1091(3) 0.059(3) Uani 1 1 d . . . C83 C 0.4588(4) 0.3992(5) 0.1269(3) 0.050(3) Uani 1 1 d . . . C85 C 0.4891(3) 0.7382(4) 0.1977(2) 0.043(2) Uani 1 1 d . . . C86 C 0.4689(5) 0.3945(6) 0.1666(3) 0.087(4) Uani 1 1 d . . . H86A H 0.4466 0.3653 0.1735 0.130 Uiso 1 1 calc R . . H86B H 0.4623 0.4320 0.1761 0.130 Uiso 1 1 calc R . . H86C H 0.5040 0.3835 0.1745 0.130 Uiso 1 1 calc R . . O1 O 0.1800(4) 0.5569(6) -0.1187(4) 0.173(7) Uani 1 1 d . . . O2 O 0.2258(5) 0.6387(7) -0.1037(3) 0.158(6) Uani 1 1 d . . . O3 O 0.1117(3) 0.4009(4) 0.1914(3) 0.097(3) Uani 1 1 d . . . O4 O 0.1336(3) 0.3396(4) 0.2329(3) 0.090(3) Uani 1 1 d . . . O5 O 0.4318(4) -0.0617(5) 0.1723(3) 0.120(4) Uani 1 1 d DU . . O6 O 0.5111(4) -0.0569(8) 0.1636(3) 0.181(6) Uani 1 1 d DU . . O7 O 0.5703(7) 0.9134(11) 0.1056(4) 0.259(7) Uani 1 1 d DU . . O8 O 0.4269(2) 0.8016(3) 0.21257(18) 0.0545(18) Uani 1 1 d . . . O9 O 0.5040(3) 0.8399(3) 0.21037(18) 0.0544(17) Uani 1 1 d U . . O10 O 0.5510(4) 0.1848(5) -0.1291(3) 0.115(4) Uani 1 1 d . . . O11 O 0.6181(5) 0.2043(7) -0.0922(3) 0.162(6) Uani 1 1 d . . . O12 O 0.8092(4) 0.2612(5) 0.1669(5) 0.205(7) Uani 1 1 d DU . . O13 O 0.8467(3) 0.4719(4) 0.2295(3) 0.089(3) Uani 1 1 d . . . O14 O 0.8384(3) 0.3899(3) 0.2015(2) 0.068(2) Uani 1 1 d . . . Pb1 Pb 0.921314(14) 0.395874(18) 0.239222(11) 0.04877(15) Uani 1 1 d . . . Pb3 Pb 0.85873(2) 0.34940(3) 0.143269(15) 0.0992(3) Uani 1 1 d DU . . Pb2 Pb 0.52705(3) 0.87917(4) 0.154553(17) 0.1048(3) Uani 1 1 d DU . . 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 C3 0.036(5) 0.023(5) 0.072(7) 0.008(5) 0.028(5) 0.004(4) C4 0.049(6) 0.047(6) 0.046(6) -0.003(5) 0.008(5) -0.002(5) C8 0.048(6) 0.054(7) 0.057(7) 0.001(6) 0.026(5) -0.005(5) C9 0.049(6) 0.039(6) 0.063(7) -0.012(5) 0.011(5) 0.016(5) C10 0.050(6) 0.045(6) 0.051(7) -0.008(5) 0.005(5) 0.006(5) C12 0.046(6) 0.034(6) 0.060(7) 0.007(5) 0.029(5) 0.013(5) C13 0.036(5) 0.048(6) 0.059(7) -0.016(5) -0.001(5) 0.011(5) C14 0.036(6) 0.066(8) 0.088(8) -0.004(7) 0.021(6) 0.001(5) C15 0.068(7) 0.055(7) 0.059(7) 0.002(6) 0.019(6) 0.015(6) C16 0.040(6) 0.041(6) 0.127(11) -0.033(7) 0.012(6) 0.007(5) C17 0.044(6) 0.033(6) 0.082(8) -0.021(6) 0.005(5) 0.023(5) C18 0.060(7) 0.060(7) 0.053(7) -0.001(6) 0.004(5) 0.004(6) C19 0.041(6) 0.046(7) 0.115(10) -0.013(7) 0.008(6) 0.017(5) C20 0.039(6) 0.045(6) 0.076(8) -0.024(6) -0.001(5) 0.023(5) C21 0.051(7) 0.105(10) 0.073(8) -0.021(8) 0.008(6) 0.050(7) C22 0.036(5) 0.032(5) 0.084(6) -0.013(5) -0.004(5) 0.022(4) C23 0.048(6) 0.045(6) 0.089(8) -0.038(6) 0.011(6) 0.020(5) C24 0.053(6) 0.051(7) 0.093(9) 0.018(6) 0.049(6) 0.010(5) C25 0.066(7) 0.058(7) 0.056(7) -0.007(6) 0.022(6) 0.005(6) C26 0.068(8) 0.058(8) 0.110(10) -0.024(7) 0.016(7) -0.030(6) C27 0.033(5) 0.054(7) 0.067(8) -0.017(6) 0.009(5) 0.003(5) C28 0.031(5) 0.052(7) 0.099(9) -0.028(6) -0.010(5) 0.016(5) C29 0.038(6) 0.036(6) 0.186(15) -0.045(8) 0.016(7) 0.000(5) C30 0.027(5) 0.053(7) 0.124(10) -0.020(7) -0.003(6) 0.001(5) C31 0.035(6) 0.075(9) 0.090(9) -0.015(7) -0.002(6) 0.032(6) C32 0.070(8) 0.055(7) 0.100(9) 0.015(7) 0.047(7) 0.014(6) C33 0.038(6) 0.060(8) 0.078(8) -0.007(7) 0.009(6) 0.006(5) C34 0.041(7) 0.069(9) 0.226(18) -0.057(11) -0.028(9) 0.029(7) C35 0.098(10) 0.052(8) 0.173(15) 0.051(9) 0.085(11) 0.035(8) C36 0.046(7) 0.055(7) 0.129(12) -0.022(8) 0.001(7) 0.021(6) C37 0.055(7) 0.075(9) 0.099(9) 0.023(8) 0.046(7) 0.015(6) C38 0.039(6) 0.049(7) 0.104(9) -0.023(7) 0.001(6) 0.020(5) C39 0.035(6) 0.053(7) 0.149(12) -0.027(8) 0.006(7) 0.010(5) C40 0.076(9) 0.095(11) 0.081(10) -0.013(9) -0.008(7) 0.035(8) C41 0.114(14) 0.132(16) 0.086(11) -0.003(11) 0.005(10) 0.076(13) C43 0.083(10) 0.080(11) 0.162(15) 0.040(11) 0.040(10) 0.017(9) C44 0.092(9) 0.045(7) 0.117(11) 0.019(7) 0.052(8) 0.022(7) C45 0.051(7) 0.089(10) 0.112(11) -0.002(9) 0.036(8) 0.009(7) C46 0.061(7) 0.081(9) 0.074(8) 0.017(7) 0.041(7) 0.007(6) C48 0.041(6) 0.063(8) 0.112(10) -0.036(8) 0.003(6) 0.017(6) C49 0.066(9) 0.076(10) 0.095(11) -0.002(9) 0.029(8) -0.010(7) C50 0.088(10) 0.121(13) 0.067(9) -0.028(9) -0.005(7) 0.043(9) C51 0.089(11) 0.153(16) 0.096(11) 0.028(11) 0.034(9) 0.025(11) C52 0.073(9) 0.097(12) 0.202(18) 0.069(12) 0.057(11) 0.046(9) C53 0.133(14) 0.154(16) 0.045(8) -0.038(9) -0.010(9) 0.078(13) C54 0.062(8) 0.139(14) 0.121(12) 0.062(11) 0.049(8) 0.051(9) C56 0.073(8) 0.047(7) 0.140(12) -0.030(8) -0.010(8) 0.041(6) C57 0.103(12) 0.101(13) 0.21(2) 0.040(13) 0.081(13) 0.024(10) C59 0.064(9) 0.170(17) 0.158(15) 0.061(14) 0.071(10) 0.025(10) C60 0.116(12) 0.22(2) 0.050(8) -0.035(10) -0.014(8) 0.111(14) C61 0.153(15) 0.169(17) 0.068(10) -0.039(10) 0.003(10) 0.114(14) C62 0.052(7) 0.105(11) 0.103(10) 0.027(9) 0.042(7) 0.041(7) C63 0.072(10) 0.084(11) 0.190(17) 0.056(11) 0.042(10) 0.032(8) C64 0.075(10) 0.117(13) 0.109(12) -0.028(10) 0.011(9) -0.001(9) C65 0.062(8) 0.084(10) 0.188(16) -0.075(11) -0.029(9) 0.038(8) C66 0.143(10) 0.161(11) 0.134(10) -0.038(8) 0.028(8) 0.025(8) C67 0.168(14) 0.226(17) 0.138(12) 0.078(13) 0.049(12) 0.072(11) C68 0.056(8) 0.105(12) 0.112(11) -0.007(10) -0.015(7) 0.033(8) C69 0.112(13) 0.099(13) 0.147(15) 0.007(12) -0.031(12) 0.049(11) C70 0.140(15) 0.113(14) 0.093(11) -0.011(11) -0.012(10) 0.038(12) C71 0.134(15) 0.077(10) 0.122(13) 0.057(10) 0.015(11) 0.011(10) C72 0.136(10) 0.148(10) 0.123(9) -0.021(8) 0.017(8) 0.040(8) C75 0.058(7) 0.059(7) 0.064(7) 0.006(6) 0.009(6) -0.011(6) C76 0.038(5) 0.048(6) 0.037(6) 0.000(5) 0.012(4) 0.014(5) C79 0.037(5) 0.042(6) 0.049(6) -0.001(5) 0.003(5) 0.020(5) C82 0.033(5) 0.034(6) 0.111(10) -0.006(6) 0.021(6) 0.014(4) C83 0.050(6) 0.051(6) 0.053(6) -0.014(6) 0.014(5) 0.013(5) C85 0.025(5) 0.034(5) 0.068(7) 0.003(5) 0.002(4) 0.009(4) C86 0.086(10) 0.106(11) 0.071(9) -0.021(8) 0.022(7) -0.013(8) O1 0.070(7) 0.119(10) 0.295(19) 0.010(11) -0.063(10) 0.018(7) O2 0.123(10) 0.141(12) 0.177(12) -0.051(10) -0.066(9) 0.075(9) O3 0.064(6) 0.101(8) 0.135(8) 0.015(7) 0.041(6) 0.032(5) O4 0.063(5) 0.090(7) 0.129(8) 0.001(6) 0.050(6) 0.020(5) O5 0.121(8) 0.103(8) 0.128(9) 0.009(7) 0.004(7) 0.028(7) O6 0.064(6) 0.407(18) 0.083(7) 0.105(10) 0.043(5) 0.092(9) O7 0.233(14) 0.370(17) 0.186(12) 0.044(13) 0.072(11) 0.031(14) O8 0.030(4) 0.045(4) 0.090(5) -0.014(4) 0.014(3) 0.004(3) O9 0.049(4) 0.050(4) 0.066(4) -0.011(4) 0.015(3) 0.009(3) O10 0.107(8) 0.135(10) 0.105(8) -0.047(7) 0.028(6) 0.037(7) O11 0.114(9) 0.251(16) 0.112(9) -0.074(10) -0.009(7) 0.107(10) O12 0.073(7) 0.114(10) 0.43(2) -0.070(12) 0.043(11) -0.010(7) O13 0.043(5) 0.068(6) 0.141(8) -0.039(6) -0.026(5) 0.023(4) O14 0.047(4) 0.057(5) 0.095(6) -0.026(4) -0.003(4) 0.028(4) Pb1 0.0354(2) 0.0437(2) 0.0694(3) -0.0026(2) 0.01495(18) 0.00779(17) Pb3 0.0787(4) 0.1211(5) 0.0907(4) -0.0284(4) -0.0049(3) 0.0543(4) Pb2 0.0850(4) 0.1391(6) 0.0939(5) 0.0155(4) 0.0260(3) 0.0096(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C3 C76 1.345(13) . ? C3 C9 1.383(13) . ? C3 C4 1.548(14) . ? C4 C10 1.331(13) . ? C4 C15 1.391(13) . ? C8 C14 1.375(13) . ? C8 C24 1.402(14) . ? C8 C12 1.477(13) . ? C9 C12 1.461(14) . ? C9 C26 1.520(14) . ? C10 C27 1.367(14) . ? C10 H10A 0.9300 . ? C12 C83 1.362(14) . ? C13 C22 1.356(12) . ? C13 C23 1.384(12) . ? C13 C82 1.535(14) . ? C14 C37 1.413(15) . ? C14 H14A 0.9300 . ? C15 C25 1.393(14) . ? C15 H15A 0.9300 . ? C16 C20 1.347(14) . ? C16 C30 1.439(14) . ? C16 H16A 0.9300 . ? C17 C22 1.357(13) . ? C17 C28 1.414(12) . ? C17 C20 1.505(12) . ? C18 C27 1.377(13) . ? C18 C25 1.415(14) . ? C18 H18A 0.9300 . ? C19 C34 1.341(16) . ? C19 C36 1.355(15) . ? C19 C31 1.552(14) . ? C20 C29 1.378(13) . ? C21 C72 1.357(19) . ? C21 C61 1.375(17) . ? C21 C25 1.461(14) . ? C22 H22A 0.9300 . ? C23 C38 1.366(14) . ? C23 H23A 0.9300 . ? C24 C32 1.415(14) . ? C24 H24A 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C33 1.491(14) . ? C28 C38 1.408(13) . ? C28 H28A 0.9300 . ? C29 C39 1.426(14) . ? C29 H29A 0.9300 . ? C30 C85 1.378(12) . ? C30 H30A 0.9300 . ? C31 O13 1.186(13) . ? C31 O14 1.283(13) . ? C32 C44 1.399(15) . ? C32 C35 1.515(16) . ? C33 C68 1.276(17) . ? C33 C69 1.389(18) . ? C34 C65 1.384(15) . ? C34 H34A 0.9300 . ? C35 C43 1.309(18) . ? C35 C52 1.398(17) . ? C36 C56 1.431(15) . ? C36 H36A 0.9300 . ? C37 C44 1.339(15) . ? C37 C46 1.477(14) . ? C38 C48 1.528(13) . ? C39 C85 1.358(14) . ? C39 H39A 0.9300 . ? C40 C70 1.37(2) . ? C40 C64 1.399(18) . ? C40 C41 1.442(18) . ? C41 O1 1.26(2) . ? C41 O2 1.29(2) . ? C41 Pb3 2.854(15) 5_665 ? C43 C63 1.377(18) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C62 1.312(17) . ? C45 C59 1.405(19) . ? C45 C49 1.499(16) . ? C46 C54 1.343(16) . ? C46 C51 1.434(18) . ? C48 C56 1.348(15) . ? C48 C65 1.419(17) . ? C49 O3 1.228(16) . ? C49 O4 1.269(15) . ? C50 C60 1.284(16) . ? C50 C66 1.41(2) . ? C50 C53 1.522(18) . ? C51 C62 1.349(16) . ? C51 H51A 0.9300 . ? C52 C57 1.41(2) . ? C52 H52A 0.9300 . ? C53 O11 1.189(17) . ? C53 O10 1.254(16) . ? C54 C59 1.461(16) . ? C54 H54A 0.9300 . ? C56 H56A 0.9300 . ? C57 C71 1.43(2) . ? C57 H57A 0.9300 . ? C59 H59 0.9300 . ? C60 C61 1.349(17) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 H62A 0.9300 . ? C63 C71 1.382(19) . ? C63 H63A 0.9300 . ? C64 C68 1.490(18) . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? C66 C72 1.46(2) . ? C66 H66 0.9300 . ? C67 O6 1.390(15) . ? C67 O5 1.401(16) . ? C67 C71 1.570(16) . ? C67 Pb2 2.808(16) 1_545 ? C68 H68A 0.9300 . ? C69 C70 1.376(19) . ? C69 H69A 0.9300 . ? C70 H70A 0.9300 . ? C72 H72A 0.9300 . ? C75 C76 1.518(13) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 C82 1.363(15) . ? C79 O8 1.272(10) . ? C79 O9 1.321(11) . ? C79 C85 1.421(12) . ? C82 C83 1.403(15) . ? C83 C86 1.576(15) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? O1 Pb3 2.486(12) 5_665 ? O2 Pb3 2.519(10) 5_665 ? O3 Pb2 2.506(10) 3_445 ? O4 Pb1 2.361(8) 2_655 ? O6 Pb2 1.569(18) 1_545 ? O7 Pb2 2.565(13) . ? O8 Pb1 2.406(6) 3_455 ? O9 Pb2 2.583(7) . ? O10 Pb2 2.583(12) 5_665 ? O10 Pb3 2.666(9) 7_655 ? O11 Pb3 2.550(10) 7_655 ? O12 Pb3 2.655(12) . ? O13 Pb1 2.596(7) . ? O14 Pb1 2.441(7) . ? O14 Pb3 2.653(8) . ? Pb1 O4 2.361(8) 2_655 ? Pb1 O8 2.407(6) 3_545 ? Pb3 O1 2.486(12) 5_665 ? Pb3 O2 2.519(10) 5_665 ? Pb3 O11 2.550(10) 7_655 ? Pb3 O10 2.666(9) 7_655 ? Pb3 C41 2.854(15) 5_665 ? Pb2 O6 1.569(18) 1_565 ? Pb2 O3 2.506(10) 3 ? Pb2 O10 2.583(12) 5_665 ? Pb2 C67 2.808(16) 1_565 ? 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 C76 C3 C9 121.5(10) . . ? C76 C3 C4 121.4(8) . . ? C9 C3 C4 117.1(9) . . ? C10 C4 C15 120.6(10) . . ? C10 C4 C3 121.3(9) . . ? C15 C4 C3 118.1(9) . . ? C14 C8 C24 117.7(9) . . ? C14 C8 C12 123.1(10) . . ? C24 C8 C12 119.2(8) . . ? C3 C9 C12 118.8(9) . . ? C3 C9 C26 122.4(10) . . ? C12 C9 C26 118.8(10) . . ? C4 C10 C27 122.2(10) . . ? C4 C10 H10A 118.9 . . ? C27 C10 H10A 118.9 . . ? C83 C12 C9 117.8(9) . . ? C83 C12 C8 123.3(9) . . ? C9 C12 C8 118.8(9) . . ? C22 C13 C23 119.7(9) . . ? C22 C13 C82 122.0(8) . . ? C23 C13 C82 118.2(8) . . ? C8 C14 C37 122.1(11) . . ? C8 C14 H14A 118.9 . . ? C37 C14 H14A 118.9 . . ? C4 C15 C25 121.2(10) . . ? C4 C15 H15A 119.4 . . ? C25 C15 H15A 119.4 . . ? C20 C16 C30 118.8(9) . . ? C20 C16 H16A 120.6 . . ? C30 C16 H16A 120.6 . . ? C22 C17 C28 118.3(8) . . ? C22 C17 C20 124.9(8) . . ? C28 C17 C20 116.7(9) . . ? C27 C18 C25 123.7(10) . . ? C27 C18 H18A 118.1 . . ? C25 C18 H18A 118.1 . . ? C34 C19 C36 119.5(11) . . ? C34 C19 C31 119.5(11) . . ? C36 C19 C31 120.7(10) . . ? C16 C20 C29 118.8(9) . . ? C16 C20 C17 121.3(9) . . ? C29 C20 C17 119.8(9) . . ? C72 C21 C61 114.3(12) . . ? C72 C21 C25 120.1(13) . . ? C61 C21 C25 123.8(10) . . ? C13 C22 C17 122.8(8) . . ? C13 C22 H22A 118.6 . . ? C17 C22 H22A 118.6 . . ? C38 C23 C13 120.1(9) . . ? C38 C23 H23A 119.9 . . ? C13 C23 H23A 119.9 . . ? C8 C24 C32 120.0(9) . . ? C8 C24 H24A 120.0 . . ? C32 C24 H24A 120.0 . . ? C15 C25 C18 114.9(10) . . ? C15 C25 C21 121.8(11) . . ? C18 C25 C21 123.2(10) . . ? C9 C26 H26A 109.5 . . ? C9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C10 C27 C18 117.4(10) . . ? C10 C27 C33 121.6(9) . . ? C18 C27 C33 121.0(10) . . ? C38 C28 C17 119.0(9) . . ? C38 C28 H28A 120.5 . . ? C17 C28 H28A 120.5 . . ? C20 C29 C39 121.3(10) . . ? C20 C29 H29A 119.3 . . ? C39 C29 H29A 119.3 . . ? C85 C30 C16 123.3(10) . . ? C85 C30 H30A 118.4 . . ? C16 C30 H30A 118.4 . . ? O13 C31 O14 122.3(9) . . ? O13 C31 C19 120.5(10) . . ? O14 C31 C19 117.2(11) . . ? C44 C32 C24 119.5(10) . . ? C44 C32 C35 119.9(10) . . ? C24 C32 C35 120.6(10) . . ? C68 C33 C69 119.7(13) . . ? C68 C33 C27 120.0(11) . . ? C69 C33 C27 120.3(11) . . ? C19 C34 C65 123.3(13) . . ? C19 C34 H34A 118.4 . . ? C65 C34 H34A 118.4 . . ? C43 C35 C52 119.7(12) . . ? C43 C35 C32 124.1(12) . . ? C52 C35 C32 116.1(12) . . ? C19 C36 C56 119.5(10) . . ? C19 C36 H36A 120.3 . . ? C56 C36 H36A 120.3 . . ? C44 C37 C14 119.6(10) . . ? C44 C37 C46 121.5(11) . . ? C14 C37 C46 118.8(11) . . ? C23 C38 C28 120.0(9) . . ? C23 C38 C48 123.2(9) . . ? C28 C38 C48 116.8(9) . . ? C85 C39 C29 121.0(10) . . ? C85 C39 H39A 119.5 . . ? C29 C39 H39A 119.5 . . ? C70 C40 C64 117.8(14) . . ? C70 C40 C41 120.6(15) . . ? C64 C40 C41 121.2(16) . . ? O1 C41 O2 122.2(15) . . ? O1 C41 C40 118.5(19) . . ? O2 C41 C40 119.2(19) . . ? O1 C41 Pb3 60.4(8) . 5_665 ? O2 C41 Pb3 62.0(8) . 5_665 ? C40 C41 Pb3 176.1(11) . 5_665 ? C35 C43 C63 124.5(14) . . ? C35 C43 H43A 117.7 . . ? C63 C43 H43A 117.7 . . ? C37 C44 C32 120.6(11) . . ? C37 C44 H44A 119.7 . . ? C32 C44 H44A 119.7 . . ? C62 C45 C59 119.1(11) . . ? C62 C45 C49 124.9(13) . . ? C59 C45 C49 115.8(13) . . ? C54 C46 C51 117.2(11) . . ? C54 C46 C37 120.3(11) . . ? C51 C46 C37 122.5(11) . . ? C56 C48 C65 119.9(11) . . ? C56 C48 C38 119.5(11) . . ? C65 C48 C38 119.3(10) . . ? O3 C49 O4 120.6(12) . . ? O3 C49 C45 119.7(14) . . ? O4 C49 C45 119.4(14) . . ? C60 C50 C66 119.4(14) . . ? C60 C50 C53 126.7(13) . . ? C66 C50 C53 113.7(13) . . ? C62 C51 C46 119.8(13) . . ? C62 C51 H51A 120.1 . . ? C46 C51 H51A 120.1 . . ? C35 C52 C57 118.2(15) . . ? C35 C52 H52A 120.9 . . ? C57 C52 H52A 120.9 . . ? O11 C53 O10 123.2(14) . . ? O11 C53 C50 121.7(15) . . ? O10 C53 C50 114.7(14) . . ? C46 C54 C59 121.5(12) . . ? C46 C54 H54A 119.3 . . ? C59 C54 H54A 119.3 . . ? C48 C56 C36 119.1(12) . . ? C48 C56 H56A 120.4 . . ? C36 C56 H56A 120.4 . . ? C52 C57 C71 120.8(15) . . ? C52 C57 H57A 119.6 . . ? C71 C57 H57A 119.6 . . ? C45 C59 C54 117.3(13) . . ? C45 C59 H59 121.3 . . ? C54 C59 H59 121.3 . . ? C50 C60 C61 125.0(14) . . ? C50 C60 H60A 117.5 . . ? C61 C60 H60A 117.5 . . ? C60 C61 C21 120.7(13) . . ? C60 C61 H61A 119.7 . . ? C21 C61 H61A 119.7 . . ? C45 C62 C51 124.5(13) . . ? C45 C62 H62A 117.8 . . ? C51 C62 H62A 117.8 . . ? C43 C63 C71 119.7(14) . . ? C43 C63 H63A 120.2 . . ? C71 C63 H63A 120.2 . . ? C40 C64 C68 118.8(14) . . ? C40 C64 H64A 120.6 . . ? C68 C64 H64A 120.6 . . ? C34 C65 C48 116.1(13) . . ? C34 C65 H65A 121.9 . . ? C48 C65 H65A 121.9 . . ? C50 C66 C72 114.2(17) . . ? C50 C66 H66 122.9 . . ? C72 C66 H66 122.9 . . ? O6 C67 O5 103.4(14) . . ? O6 C67 C71 152.7(18) . . ? O5 C67 C71 103.9(13) . . ? O6 C67 Pb2 19.5(9) . 1_545 ? O5 C67 Pb2 85.9(9) . 1_545 ? C71 C67 Pb2 166.3(13) . 1_545 ? C33 C68 C64 120.5(13) . . ? C33 C68 H68A 119.7 . . ? C64 C68 H68A 119.7 . . ? C70 C69 C33 122.2(16) . . ? C70 C69 H69A 118.9 . . ? C33 C69 H69A 118.9 . . ? C40 C70 C69 120.7(16) . . ? C40 C70 H70A 119.7 . . ? C69 C70 H70A 119.7 . . ? C63 C71 C57 117.1(14) . . ? C63 C71 C67 130.9(16) . . ? C57 C71 C67 111.9(16) . . ? C21 C72 C66 123.2(17) . . ? C21 C72 H72A 118.4 . . ? C66 C72 H72A 118.4 . . ? C76 C75 H75A 109.5 . . ? C76 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C76 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C3 C76 C82 120.4(10) . . ? C3 C76 C75 121.0(9) . . ? C82 C76 C75 118.5(9) . . ? O8 C79 O9 119.1(8) . . ? O8 C79 C85 120.6(9) . . ? O9 C79 C85 120.2(8) . . ? C76 C82 C83 120.8(10) . . ? C76 C82 C13 122.7(10) . . ? C83 C82 C13 116.4(11) . . ? C12 C83 C82 120.6(10) . . ? C12 C83 C86 116.1(10) . . ? C82 C83 C86 123.2(10) . . ? C39 C85 C30 116.4(9) . . ? C39 C85 C79 121.6(9) . . ? C30 C85 C79 122.0(9) . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C41 O1 Pb3 93.4(11) . 5_665 ? C41 O2 Pb3 91.1(10) . 5_665 ? C49 O3 Pb2 123.9(9) . 3_445 ? C49 O4 Pb1 113.0(9) . 2_655 ? C67 O6 Pb2 143.2(15) . 1_545 ? C79 O8 Pb1 108.7(6) . 3_455 ? C79 O9 Pb2 116.1(6) . . ? C53 O10 Pb2 144.3(12) . 5_665 ? C53 O10 Pb3 90.1(9) . 7_655 ? Pb2 O10 Pb3 115.9(4) 5_665 7_655 ? C53 O11 Pb3 97.4(9) . 7_655 ? C31 O13 Pb1 90.9(6) . . ? C31 O14 Pb1 95.8(7) . . ? C31 O14 Pb3 133.5(8) . . ? Pb1 O14 Pb3 105.5(2) . . ? O4 Pb1 O8 79.8(3) 2_655 3_545 ? O4 Pb1 O14 72.8(3) 2_655 . ? O8 Pb1 O14 78.1(2) 3_545 . ? O4 Pb1 O13 85.1(3) 2_655 . ? O8 Pb1 O13 128.8(2) 3_545 . ? O14 Pb1 O13 50.7(2) . . ? O1 Pb3 O2 53.1(4) 5_665 5_665 ? O1 Pb3 O11 103.2(5) 5_665 7_655 ? O2 Pb3 O11 81.7(4) 5_665 7_655 ? O1 Pb3 O14 85.4(4) 5_665 . ? O2 Pb3 O14 102.9(4) 5_665 . ? O11 Pb3 O14 171.2(4) 7_655 . ? O1 Pb3 O12 126.2(4) 5_665 . ? O2 Pb3 O12 82.3(5) 5_665 . ? O11 Pb3 O12 97.6(5) 7_655 . ? O14 Pb3 O12 75.9(4) . . ? O1 Pb3 O10 119.1(4) 5_665 7_655 ? O2 Pb3 O10 128.7(4) 5_665 7_655 ? O11 Pb3 O10 48.6(3) 7_655 7_655 ? O14 Pb3 O10 128.1(3) . 7_655 ? O12 Pb3 O10 112.0(4) . 7_655 ? O1 Pb3 C41 26.2(5) 5_665 5_665 ? O2 Pb3 C41 26.9(5) 5_665 5_665 ? O11 Pb3 C41 93.8(4) 7_655 5_665 ? O14 Pb3 C41 93.6(3) . 5_665 ? O12 Pb3 C41 104.5(6) . 5_665 ? O10 Pb3 C41 129.4(4) 7_655 5_665 ? O6 Pb2 O3 86.0(5) 1_565 3 ? O6 Pb2 O7 94.2(6) 1_565 . ? O3 Pb2 O7 85.4(5) 3 . ? O6 Pb2 O9 90.2(4) 1_565 . ? O3 Pb2 O9 83.0(3) 3 . ? O7 Pb2 O9 167.3(5) . . ? O6 Pb2 O10 112.4(5) 1_565 5_665 ? O3 Pb2 O10 155.9(3) 3 5_665 ? O7 Pb2 O10 107.5(6) . 5_665 ? O9 Pb2 O10 81.6(3) . 5_665 ? O6 Pb2 C67 17.2(6) 1_565 1_565 ? O3 Pb2 C67 101.8(5) 3 1_565 ? O7 Pb2 C67 102.2(6) . 1_565 ? O9 Pb2 C67 85.2(4) . 1_565 ? O10 Pb2 C67 95.3(5) 5_665 1_565 ? 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 C76 C3 C4 C10 -90.5(12) . . . . ? C9 C3 C4 C10 90.2(12) . . . . ? C76 C3 C4 C15 87.9(12) . . . . ? C9 C3 C4 C15 -91.4(11) . . . . ? C76 C3 C9 C12 1.4(13) . . . . ? C4 C3 C9 C12 -179.3(8) . . . . ? C76 C3 C9 C26 179.7(9) . . . . ? C4 C3 C9 C26 -0.9(13) . . . . ? C15 C4 C10 C27 1.4(16) . . . . ? C3 C4 C10 C27 179.7(9) . . . . ? C3 C9 C12 C83 0.4(13) . . . . ? C26 C9 C12 C83 -178.0(9) . . . . ? C3 C9 C12 C8 178.7(8) . . . . ? C26 C9 C12 C8 0.2(13) . . . . ? C14 C8 C12 C83 84.6(14) . . . . ? C24 C8 C12 C83 -96.6(12) . . . . ? C14 C8 C12 C9 -93.5(12) . . . . ? C24 C8 C12 C9 85.3(12) . . . . ? C24 C8 C14 C37 5.8(17) . . . . ? C12 C8 C14 C37 -175.4(11) . . . . ? C10 C4 C15 C25 -1.8(17) . . . . ? C3 C4 C15 C25 179.8(10) . . . . ? C30 C16 C20 C29 4.1(19) . . . . ? C30 C16 C20 C17 -179.8(11) . . . . ? C22 C17 C20 C16 -158.2(12) . . . . ? C28 C17 C20 C16 22.6(17) . . . . ? C22 C17 C20 C29 17.9(19) . . . . ? C28 C17 C20 C29 -161.3(12) . . . . ? C23 C13 C22 C17 0.2(18) . . . . ? C82 C13 C22 C17 178.2(11) . . . . ? C28 C17 C22 C13 -1.3(18) . . . . ? C20 C17 C22 C13 179.6(11) . . . . ? C22 C13 C23 C38 1.6(18) . . . . ? C82 C13 C23 C38 -176.4(11) . . . . ? C14 C8 C24 C32 -2.9(17) . . . . ? C12 C8 C24 C32 178.2(11) . . . . ? C4 C15 C25 C18 1.9(16) . . . . ? C4 C15 C25 C21 -177.8(11) . . . . ? C27 C18 C25 C15 -1.7(17) . . . . ? C27 C18 C25 C21 178.0(11) . . . . ? C72 C21 C25 C15 -35(2) . . . . ? C61 C21 C25 C15 161.0(16) . . . . ? C72 C21 C25 C18 145.0(15) . . . . ? C61 C21 C25 C18 -19(2) . . . . ? C4 C10 C27 C18 -1.1(16) . . . . ? C4 C10 C27 C33 -178.3(10) . . . . ? C25 C18 C27 C10 1.3(16) . . . . ? C25 C18 C27 C33 178.5(10) . . . . ? C22 C17 C28 C38 0.6(18) . . . . ? C20 C17 C28 C38 179.8(11) . . . . ? C16 C20 C29 C39 -6(2) . . . . ? C17 C20 C29 C39 177.8(12) . . . . ? C20 C16 C30 C85 -3(2) . . . . ? C34 C19 C31 O13 22(2) . . . . ? C36 C19 C31 O13 -164.7(14) . . . . ? C34 C19 C31 O14 -158.3(14) . . . . ? C36 C19 C31 O14 15.3(19) . . . . ? C8 C24 C32 C44 -3.1(19) . . . . ? C8 C24 C32 C35 177.3(13) . . . . ? C10 C27 C33 C68 44.0(17) . . . . ? C18 C27 C33 C68 -133.1(14) . . . . ? C10 C27 C33 C69 -134.2(14) . . . . ? C18 C27 C33 C69 48.7(17) . . . . ? C36 C19 C34 C65 5(3) . . . . ? C31 C19 C34 C65 178.4(15) . . . . ? C44 C32 C35 C43 29(3) . . . . ? C24 C32 C35 C43 -151.5(16) . . . . ? C44 C32 C35 C52 -148.9(15) . . . . ? C24 C32 C35 C52 31(2) . . . . ? C34 C19 C36 C56 -9(2) . . . . ? C31 C19 C36 C56 177.2(12) . . . . ? C8 C14 C37 C44 -2(2) . . . . ? C8 C14 C37 C46 173.8(11) . . . . ? C13 C23 C38 C28 -2.3(19) . . . . ? C13 C23 C38 C48 176.2(12) . . . . ? C17 C28 C38 C23 1.2(19) . . . . ? C17 C28 C38 C48 -177.4(11) . . . . ? C20 C29 C39 C85 7(2) . . . . ? C70 C40 C41 O1 28(3) . . . . ? C64 C40 C41 O1 -159.2(17) . . . . ? C70 C40 C41 O2 -151.7(18) . . . . ? C64 C40 C41 O2 21(2) . . . . ? C70 C40 C41 Pb3 -45(26) . . . 5_665 ? C64 C40 C41 Pb3 128(24) . . . 5_665 ? C52 C35 C43 C63 -2(3) . . . . ? C32 C35 C43 C63 -179.8(16) . . . . ? C14 C37 C44 C32 -4(2) . . . . ? C46 C37 C44 C32 180.0(12) . . . . ? C24 C32 C44 C37 7(2) . . . . ? C35 C32 C44 C37 -173.7(14) . . . . ? C44 C37 C46 C54 34(2) . . . . ? C14 C37 C46 C54 -142.2(14) . . . . ? C44 C37 C46 C51 -147.9(15) . . . . ? C14 C37 C46 C51 36(2) . . . . ? C23 C38 C48 C56 -13(2) . . . . ? C28 C38 C48 C56 165.9(13) . . . . ? C23 C38 C48 C65 154.7(14) . . . . ? C28 C38 C48 C65 -26.8(19) . . . . ? C62 C45 C49 O3 -8(2) . . . . ? C59 C45 C49 O3 167.9(15) . . . . ? C62 C45 C49 O4 178.5(14) . . . . ? C59 C45 C49 O4 -6(2) . . . . ? C54 C46 C51 C62 -7(2) . . . . ? C37 C46 C51 C62 174.6(14) . . . . ? C43 C35 C52 C57 1(3) . . . . ? C32 C35 C52 C57 178.7(16) . . . . ? C60 C50 C53 O11 162(2) . . . . ? C66 C50 C53 O11 -13(3) . . . . ? C60 C50 C53 O10 -11(3) . . . . ? C66 C50 C53 O10 173.7(17) . . . . ? C51 C46 C54 C59 5(2) . . . . ? C37 C46 C54 C59 -176.6(14) . . . . ? C65 C48 C56 C36 14(2) . . . . ? C38 C48 C56 C36 -178.8(12) . . . . ? C19 C36 C56 C48 0(2) . . . . ? C35 C52 C57 C71 2(3) . . . . ? C62 C45 C59 C54 -7(2) . . . . ? C49 C45 C59 C54 177.7(14) . . . . ? C46 C54 C59 C45 2(3) . . . . ? C66 C50 C60 C61 -7(3) . . . . ? C53 C50 C60 C61 178(2) . . . . ? C50 C60 C61 C21 -6(3) . . . . ? C72 C21 C61 C60 18(3) . . . . ? C25 C21 C61 C60 -177.2(17) . . . . ? C59 C45 C62 C51 5(3) . . . . ? C49 C45 C62 C51 -179.8(15) . . . . ? C46 C51 C62 C45 2(3) . . . . ? C35 C43 C63 C71 1(3) . . . . ? C70 C40 C64 C68 -5(2) . . . . ? C41 C40 C64 C68 -178.0(15) . . . . ? C19 C34 C65 C48 9(3) . . . . ? C56 C48 C65 C34 -18(2) . . . . ? C38 C48 C65 C34 174.7(14) . . . . ? C60 C50 C66 C72 6(3) . . . . ? C53 C50 C66 C72 -179.0(17) . . . . ? C69 C33 C68 C64 3(2) . . . . ? C27 C33 C68 C64 -175.5(11) . . . . ? C40 C64 C68 C33 2(2) . . . . ? C68 C33 C69 C70 -4(3) . . . . ? C27 C33 C69 C70 173.8(15) . . . . ? C64 C40 C70 C69 4(3) . . . . ? C41 C40 C70 C69 176.5(17) . . . . ? C33 C69 C70 C40 1(3) . . . . ? C43 C63 C71 C57 2(3) . . . . ? C43 C63 C71 C67 -173.3(18) . . . . ? C52 C57 C71 C63 -3(3) . . . . ? C52 C57 C71 C67 173.1(17) . . . . ? O6 C67 C71 C63 164(3) . . . . ? O5 C67 C71 C63 -14(3) . . . . ? Pb2 C67 C71 C63 121(6) 1_545 . . . ? O6 C67 C71 C57 -11(5) . . . . ? O5 C67 C71 C57 171.4(16) . . . . ? Pb2 C67 C71 C57 -54(7) 1_545 . . . ? C61 C21 C72 C66 -20(3) . . . . ? C25 C21 C72 C66 175.3(16) . . . . ? C50 C66 C72 C21 8(3) . . . . ? C9 C3 C76 C82 -1.5(14) . . . . ? C4 C3 C76 C82 179.1(8) . . . . ? C9 C3 C76 C75 178.7(9) . . . . ? C4 C3 C76 C75 -0.6(13) . . . . ? C3 C76 C82 C83 -0.1(14) . . . . ? C75 C76 C82 C83 179.6(9) . . . . ? C3 C76 C82 C13 -176.9(8) . . . . ? C75 C76 C82 C13 2.9(13) . . . . ? C22 C13 C82 C76 93.1(13) . . . . ? C23 C13 C82 C76 -88.9(13) . . . . ? C22 C13 C82 C83 -83.8(13) . . . . ? C23 C13 C82 C83 94.2(12) . . . . ? C9 C12 C83 C82 -2.0(13) . . . . ? C8 C12 C83 C82 179.8(9) . . . . ? C9 C12 C83 C86 -177.8(9) . . . . ? C8 C12 C83 C86 4.0(14) . . . . ? C76 C82 C83 C12 2.0(14) . . . . ? C13 C82 C83 C12 178.9(8) . . . . ? C76 C82 C83 C86 177.4(10) . . . . ? C13 C82 C83 C86 -5.6(14) . . . . ? C29 C39 C85 C30 -5.9(19) . . . . ? C29 C39 C85 C79 173.4(12) . . . . ? C16 C30 C85 C39 4.3(18) . . . . ? C16 C30 C85 C79 -175.0(11) . . . . ? O8 C79 C85 C39 10.0(16) . . . . ? O9 C79 C85 C39 -166.8(11) . . . . ? O8 C79 C85 C30 -170.8(10) . . . . ? O9 C79 C85 C30 12.4(16) . . . . ? O2 C41 O1 Pb3 4(2) . . . 5_665 ? C40 C41 O1 Pb3 -175.7(13) . . . 5_665 ? O1 C41 O2 Pb3 -4(2) . . . 5_665 ? C40 C41 O2 Pb3 175.8(13) . . . 5_665 ? O4 C49 O3 Pb2 -81.1(16) . . . 3_445 ? C45 C49 O3 Pb2 105.0(12) . . . 3_445 ? O3 C49 O4 Pb1 -18.1(17) . . . 2_655 ? C45 C49 O4 Pb1 155.8(10) . . . 2_655 ? O5 C67 O6 Pb2 27(3) . . . 1_545 ? C71 C67 O6 Pb2 -151(3) . . . 1_545 ? O9 C79 O8 Pb1 -14.2(11) . . . 3_455 ? C85 C79 O8 Pb1 169.0(7) . . . 3_455 ? O8 C79 O9 Pb2 -108.7(9) . . . . ? C85 C79 O9 Pb2 68.1(10) . . . . ? O11 C53 O10 Pb2 130(2) . . . 5_665 ? C50 C53 O10 Pb2 -57(2) . . . 5_665 ? O11 C53 O10 Pb3 -9(2) . . . 7_655 ? C50 C53 O10 Pb3 164.2(14) . . . 7_655 ? O10 C53 O11 Pb3 9(2) . . . 7_655 ? C50 C53 O11 Pb3 -163.3(15) . . . 7_655 ? O14 C31 O13 Pb1 -5.1(14) . . . . ? C19 C31 O13 Pb1 174.9(11) . . . . ? O13 C31 O14 Pb1 5.4(15) . . . . ? C19 C31 O14 Pb1 -174.6(10) . . . . ? O13 C31 O14 Pb3 -112.4(13) . . . . ? C19 C31 O14 Pb3 67.6(15) . . . . ? C31 O14 Pb1 O4 95.2(8) . . . 2_655 ? Pb3 O14 Pb1 O4 -126.5(4) . . . 2_655 ? C31 O14 Pb1 O8 178.1(8) . . . 3_545 ? Pb3 O14 Pb1 O8 -43.7(3) . . . 3_545 ? C31 O14 Pb1 O13 -2.7(7) . . . . ? Pb3 O14 Pb1 O13 135.6(5) . . . . ? C31 O13 Pb1 O4 -68.8(9) . . . 2_655 ? C31 O13 Pb1 O8 3.9(10) . . . 3_545 ? C31 O13 Pb1 O14 2.9(8) . . . . ? C31 O14 Pb3 O1 -6.1(10) . . . 5_665 ? Pb1 O14 Pb3 O1 -120.2(4) . . . 5_665 ? C31 O14 Pb3 O2 -56.6(11) . . . 5_665 ? Pb1 O14 Pb3 O2 -170.7(5) . . . 5_665 ? C31 O14 Pb3 O11 -178(2) . . . 7_655 ? Pb1 O14 Pb3 O11 68(2) . . . 7_655 ? C31 O14 Pb3 O12 -135.2(10) . . . . ? Pb1 O14 Pb3 O12 110.7(4) . . . . ? C31 O14 Pb3 O10 117.8(10) . . . 7_655 ? Pb1 O14 Pb3 O10 3.7(5) . . . 7_655 ? C31 O14 Pb3 C41 -31.1(11) . . . 5_665 ? Pb1 O14 Pb3 C41 -145.2(6) . . . 5_665 ? C79 O9 Pb2 O6 127.9(7) . . . 1_565 ? C79 O9 Pb2 O3 -146.2(6) . . . 3 ? C79 O9 Pb2 O7 -122(3) . . . . ? C79 O9 Pb2 O10 15.2(6) . . . 5_665 ? C79 O9 Pb2 C67 111.3(7) . . . 1_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.716 _refine_diff_density_min -1.842 _refine_diff_density_rms 0.195 _database_code_depnum_ccdc_archive 'CCDC 896049' ####################################################################### # # 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_Zn #TrackingRef 'Zn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H N O Zn' _chemical_formula_weight 108.40 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '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' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' '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' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-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' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-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' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 19.850(3) _cell_length_b 19.850(3) _cell_length_c 83.91(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 28632(11) _cell_formula_units_Z 357 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18564 _exptl_absorpt_coefficient_mu 7.387 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42358 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -99 _diffrn_reflns_limit_l_max 98 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5581 _reflns_number_gt 3781 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5581 _refine_ls_number_parameters 274 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.1155 _refine_ls_wR_factor_ref 0.3580 _refine_ls_wR_factor_gt 0.3348 _refine_ls_goodness_of_fit_ref 1.384 _refine_ls_restrained_S_all 1.400 _refine_ls_shift/su_max 7.170 _refine_ls_shift/su_mean 0.062 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 C1 C 0.6988(4) 1.1695(4) -0.01632(8) 0.0473(17) Uani 1 1 d . . . H1 H 0.7170 1.2031 -0.0250 0.09(3) Uiso 1 1 calc R . . C2 C 0.6364(4) 1.1350(4) 0.00899(8) 0.0469(17) Uani 1 1 d . . . H2 H 0.6156 1.1468 0.0178 0.049(19) Uiso 1 1 calc R . . C3 C 0.6688(4) 1.1889(4) -0.00337(8) 0.0411(15) Uani 1 1 d . . . C4 C 0.5915(4) 1.0055(4) 0.02085(8) 0.0479(17) Uani 1 1 d . . . C5 C 0.5051(4) 0.8896(4) 0.04320(8) 0.0476(17) Uani 1 1 d . . . C6 C 0.6344(4) 1.0647(4) 0.00853(8) 0.0465(17) Uani 1 1 d . . . C7 C 0.7029(4) 1.1027(4) -0.01687(8) 0.0493(18) Uani 1 1 d . . . C8 C 0.4555(5) 0.8255(4) 0.05429(9) 0.0510(18) Uani 1 1 d . . . C9 C 0.7440(5) 1.0886(5) -0.02986(9) 0.060(2) Uani 1 1 d . . . C10 C 0.5208(5) 0.9940(5) 0.02651(9) 0.057(2) Uani 1 1 d . . . H10 H 0.5016 1.0252 0.0227 1.0(3) Uiso 1 1 calc R . . C11 C 0.6177(5) 0.9570(5) 0.02677(8) 0.0543(19) Uani 1 1 d . . . H11 H 0.6645 0.9629 0.0231 0.07(2) Uiso 1 1 calc R . . C12 C 0.7425(5) 1.1090(5) -0.04552(8) 0.057(2) Uani 1 1 d . . . H12 H 0.7137 1.1326 -0.0482 0.05(2) Uiso 1 1 calc R . . C13 C 0.4798(5) 0.9389(4) 0.03725(9) 0.0545(19) Uani 1 1 d . . . H13 H 0.4329 0.9332 0.0409 0.06(2) Uiso 1 1 calc R . . C14 C 0.5756(5) 0.9008(5) 0.03791(9) 0.0541(18) Uani 1 1 d . . . H14 H 0.5948 0.8700 0.0419 0.06(2) Uiso 1 1 calc R . . C15 C 0.6696(4) 1.0495(4) -0.00444(8) 0.0522(18) Uani 1 1 d . . . H15 H 0.6708 1.0032 -0.0047 0.07(2) Uiso 1 1 calc R . . C16 C 0.7823(6) 1.0953(5) -0.05727(10) 0.069(2) Uani 1 1 d . . . H16 H 0.7800 1.1099 -0.0677 0.09(3) Uiso 1 1 calc R . . C17 C 0.8261(7) 1.0601(7) -0.05381(12) 0.091(3) Uani 1 1 d . . . C18 C 0.7879(8) 1.0516(8) -0.02657(12) 0.104(4) Uani 1 1 d U . . H18 H 0.7910 1.0376 -0.0161 2(3) Uiso 1 1 calc R . . C19 C 0.8246(8) 1.0366(9) -0.03804(14) 0.113(4) Uani 1 1 d U . . H19 H 0.8502 1.0095 -0.0355 0.17(6) Uiso 1 1 calc R . . C21 C 0.5219(4) 1.1871(4) -0.00206(11) 0.055(2) Uani 1 1 d . . . H21A H 0.5137 1.1673 0.0086 0.10(4) Uiso 1 1 calc R . . H21B H 0.5243 1.1504 -0.0092 0.14(5) Uiso 1 1 calc R . . H21C H 0.4797 1.1949 -0.0051 0.06(2) Uiso 1 1 calc R . . C22 C 0.5103(8) 0.7100(9) 0.10050(17) 0.120(5) Uani 1 1 d . . . C23 C 0.5961(4) 1.2622(4) -0.00285(8) 0.0416(16) Uani 1 1 d . . . C24 C 0.6677(4) 1.2643(4) -0.00286(7) 0.0404(15) Uani 1 1 d . . . O1 O 0.3333 0.6667 0.07937(8) 0.0363(17) Uani 1 3 d S . . O2 O 0.4786(3) 0.7789(4) 0.05791(7) 0.0632(15) Uani 1 1 d . . . O3 O 0.5253(4) 0.7190(4) 0.08657(9) 0.092(2) Uani 1 1 d . . . O4 O 0.4391(9) 0.6772(11) 0.1043(2) 0.250(8) Uani 1 1 d U . . O5 O 0.3943(3) 0.8218(3) 0.05915(7) 0.0635(15) Uani 1 1 d . . . Zn1 Zn 0.43718(4) 0.69057(5) 0.072663(8) 0.0413(4) Uani 1 1 d . . . Zn2 Zn 0.3333 0.6667 0.10347(3) 0.1159(10) Uani 1 3 d S . . 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 C1 0.049(4) 0.051(4) 0.041(4) 0.006(3) 0.011(3) 0.025(4) C2 0.053(4) 0.051(4) 0.041(4) 0.001(3) 0.012(3) 0.029(4) C3 0.042(4) 0.039(4) 0.047(4) 0.005(3) 0.007(3) 0.024(3) C4 0.052(4) 0.044(4) 0.046(4) 0.002(3) 0.010(3) 0.023(3) C5 0.052(4) 0.052(4) 0.043(4) 0.005(3) 0.006(3) 0.029(4) C6 0.051(4) 0.043(4) 0.045(4) 0.007(3) 0.012(3) 0.023(3) C7 0.056(4) 0.052(4) 0.045(4) 0.005(3) 0.016(3) 0.031(4) C8 0.058(5) 0.048(4) 0.047(4) 0.009(3) 0.009(3) 0.027(4) C9 0.074(6) 0.065(5) 0.057(4) 0.012(4) 0.024(4) 0.048(5) C10 0.061(5) 0.058(5) 0.059(4) 0.010(4) 0.016(4) 0.035(4) C11 0.057(5) 0.060(5) 0.056(4) 0.012(4) 0.012(4) 0.037(4) C12 0.070(5) 0.061(5) 0.047(4) 0.007(4) 0.020(4) 0.038(4) C13 0.055(5) 0.055(5) 0.056(4) 0.017(4) 0.025(4) 0.030(4) C14 0.053(4) 0.055(5) 0.059(4) 0.012(4) 0.009(4) 0.031(4) C15 0.062(5) 0.047(4) 0.054(4) 0.006(3) 0.014(4) 0.032(4) C16 0.087(7) 0.064(6) 0.054(5) 0.002(4) 0.021(4) 0.036(5) C17 0.116(9) 0.103(8) 0.079(6) 0.020(6) 0.050(6) 0.075(7) C18 0.146(9) 0.152(9) 0.074(6) 0.041(6) 0.050(6) 0.120(8) C19 0.148(10) 0.161(11) 0.094(7) 0.032(7) 0.048(7) 0.126(9) C21 0.038(4) 0.044(4) 0.078(6) -0.006(4) 0.003(4) 0.018(4) C22 0.081(9) 0.139(12) 0.101(9) 0.030(8) -0.041(7) 0.024(8) C23 0.046(4) 0.045(4) 0.036(3) -0.007(3) 0.001(3) 0.025(3) C24 0.045(4) 0.043(4) 0.035(3) 0.002(3) 0.006(3) 0.023(3) O1 0.041(3) 0.041(3) 0.027(3) 0.000 0.000 0.0204(13) O2 0.059(4) 0.068(4) 0.067(3) 0.026(3) 0.017(3) 0.035(3) O3 0.095(6) 0.088(5) 0.085(5) -0.012(4) -0.049(4) 0.041(4) O4 0.154(10) 0.323(16) 0.195(11) 0.037(11) -0.115(9) 0.061(10) O5 0.064(4) 0.063(4) 0.071(4) 0.025(3) 0.027(3) 0.037(3) Zn1 0.0432(6) 0.0441(6) 0.0363(5) -0.0021(3) -0.0036(3) 0.0216(4) Zn2 0.1396(15) 0.1396(15) 0.0684(14) 0.000 0.000 0.0698(8) _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 C1 C7 1.367(10) . ? C1 C3 1.383(9) . ? C2 C6 1.376(10) . ? C2 C3 1.395(9) . ? C3 C24 1.508(9) . ? C4 C11 1.393(10) . ? C4 C10 1.389(10) . ? C4 C6 1.474(9) . ? C5 C14 1.377(10) . ? C5 C13 1.396(10) . ? C5 C8 1.484(10) . ? C6 C15 1.406(9) . ? C7 C15 1.394(9) . ? C7 C9 1.470(9) . ? C8 O2 1.260(9) . ? C8 O5 1.249(9) . ? C9 C12 1.380(11) . ? C9 C18 1.420(13) . ? C10 C13 1.334(10) . ? C11 C14 1.373(10) . ? C12 C16 1.373(10) . ? C16 C17 1.392(14) . ? C17 C19 1.398(15) . ? C17 C22 1.445(14) 29 ? C18 C19 1.328(13) . ? C21 C23 1.484(10) . ? C22 O3 1.197(15) . ? C22 O4 1.27(2) . ? C22 C17 1.445(14) 35_545 ? C23 C24 1.386(9) 3_575 ? C23 C24 1.402(9) . ? C24 C23 1.386(9) 2_775 ? O1 Zn1 1.953(2) . ? O1 Zn1 1.953(2) 3_565 ? O1 Zn1 1.953(2) 2_665 ? O1 Zn2 2.022(7) . ? O2 Zn1 1.959(5) . ? O3 Zn1 1.936(6) . ? O4 Zn2 2.003(17) . ? O5 Zn1 1.959(5) 2_665 ? Zn1 O5 1.958(5) 3_565 ? Zn2 O4 2.003(18) 3_565 ? Zn2 O4 2.003(17) 2_665 ? 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 C7 C1 C3 122.6(6) . . ? C6 C2 C3 121.7(6) . . ? C1 C3 C2 117.9(6) . . ? C1 C3 C24 121.4(6) . . ? C2 C3 C24 120.7(6) . . ? C11 C4 C10 117.3(7) . . ? C11 C4 C6 122.4(7) . . ? C10 C4 C6 120.3(7) . . ? C14 C5 C13 117.7(7) . . ? C14 C5 C8 121.6(7) . . ? C13 C5 C8 120.6(7) . . ? C2 C6 C15 118.3(6) . . ? C2 C6 C4 120.1(6) . . ? C15 C6 C4 121.5(6) . . ? C1 C7 C15 118.3(6) . . ? C1 C7 C9 121.1(6) . . ? C15 C7 C9 120.5(7) . . ? O2 C8 O5 125.5(7) . . ? O2 C8 C5 116.9(7) . . ? O5 C8 C5 117.6(7) . . ? C12 C9 C18 116.5(7) . . ? C12 C9 C7 123.7(7) . . ? C18 C9 C7 119.8(7) . . ? C13 C10 C4 121.3(8) . . ? C14 C11 C4 121.3(7) . . ? C16 C12 C9 121.8(8) . . ? C10 C13 C5 122.0(7) . . ? C11 C14 C5 120.4(7) . . ? C7 C15 C6 120.9(7) . . ? C12 C16 C17 121.1(8) . . ? C19 C17 C16 116.8(8) . . ? C19 C17 C22 121.6(11) . 29 ? C16 C17 C22 121.5(11) . 29 ? C19 C18 C9 121.5(10) . . ? C18 C19 C17 122.2(11) . . ? O3 C22 O4 116.8(12) . . ? O3 C22 C17 124.0(14) . 35_545 ? O4 C22 C17 118.9(13) . 35_545 ? C24 C23 C24 118.3(7) 3_575 . ? C24 C23 C21 120.9(7) 3_575 . ? C24 C23 C21 120.8(7) . . ? C23 C24 C23 121.7(7) 2_775 . ? C23 C24 C3 119.0(6) 2_775 . ? C23 C24 C3 119.3(6) . . ? Zn1 O1 Zn1 112.06(17) . 3_565 ? Zn1 O1 Zn1 112.05(17) . 2_665 ? Zn1 O1 Zn1 112.05(17) 3_565 2_665 ? Zn1 O1 Zn2 106.75(19) . . ? Zn1 O1 Zn2 106.75(19) 3_565 . ? Zn1 O1 Zn2 106.75(19) 2_665 . ? C8 O2 Zn1 131.7(5) . . ? C22 O3 Zn1 115.1(9) . . ? C22 O4 Zn2 152.6(14) . . ? C8 O5 Zn1 132.4(5) . 2_665 ? O3 Zn1 O1 125.9(3) . . ? O3 Zn1 O5 106.6(3) . 3_565 ? O1 Zn1 O5 108.71(19) . 3_565 ? O3 Zn1 O2 101.9(3) . . ? O1 Zn1 O2 108.6(2) . . ? O5 Zn1 O2 102.7(3) 3_565 . ? O1 Zn2 O4 92.0(5) . 3_565 ? O1 Zn2 O4 92.0(5) . 2_665 ? O4 Zn2 O4 119.88(6) 3_565 2_665 ? O1 Zn2 O4 92.0(5) . . ? O4 Zn2 O4 119.88(6) 3_565 . ? O4 Zn2 O4 119.89(6) 2_665 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.582 _refine_diff_density_min -3.059 _refine_diff_density_rms 0.254 _database_code_depnum_ccdc_archive 'CCDC 896050'