# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Bryan Eichhorn' 'James C. Fettinger' 'Emren Nalbant Esenturk' _publ_contact_author_name 'Prof Bryan Eichhorn' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Maryland College Park Maryland 20742 UNITED STATES OF AMERICA ; _publ_contact_author_email EICHHORN@UMD.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; The closo-Pb102- Zintl Ion in the [Ni@Pb10]2- cluster ; data_1027atwin560st _database_code_depnum_ccdc_archive 'CCDC 245966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 K2 N4 Ni O12 Pb10' _chemical_formula_weight 2961.79 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 24.843(3) _cell_length_b 11.9405(16) _cell_length_c 21.403(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.907(2) _cell_angle_gamma 90.00 _cell_volume 6302.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7526 _cell_measurement_theta_min 2.625 _cell_measurement_theta_max 25.002 _exptl_crystal_description Plate _exptl_crystal_colour Black _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5192 _exptl_absorpt_coefficient_mu 27.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0322 _exptl_absorpt_correction_T_max 0.3124 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% 0 _diffrn_reflns_number 5757 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5758 _reflns_number_gt 4234 _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^)+(0.1203P)^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 5758 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 0.0000 0.56703(18) 0.2500 0.0252(5) Uani 1 2 d S . . Pb1 Pb 0.02670(3) 0.56607(6) 0.10695(3) 0.05538(19) Uani 1 1 d . . . Pb2 Pb 0.09925(2) 0.64160(5) 0.22777(3) 0.04600(16) Uani 1 1 d . . . Pb3 Pb -0.02688(3) 0.75289(5) 0.17962(3) 0.04498(17) Uani 1 1 d . . . Pb4 Pb -0.07638(2) 0.48723(5) 0.15954(3) 0.04260(16) Uani 1 1 d . . . Pb5 Pb 0.04732(2) 0.37976(5) 0.20750(3) 0.04066(15) Uani 1 1 d . . . K11 K 0.32550(12) 0.5046(2) 0.52648(12) 0.0284(6) Uani 1 1 d . . . N11 N 0.2683(5) 0.5178(9) 0.6422(5) 0.036(3) Uani 1 1 d . . . N12 N 0.3804(5) 0.4885(9) 0.4097(5) 0.035(3) Uani 1 1 d . . . C11 C 0.2823(7) 0.6287(12) 0.6736(6) 0.043(4) Uani 1 1 d . . . H11A H 0.2579 0.6413 0.7062 0.052 Uiso 1 1 calc R . . H11B H 0.3199 0.6249 0.6951 0.052 Uiso 1 1 calc R . . C12 C 0.2779(7) 0.7251(13) 0.6300(7) 0.045(4) Uani 1 1 d . . . H12A H 0.2401 0.7325 0.6098 0.054 Uiso 1 1 calc R . . H12B H 0.2879 0.7949 0.6536 0.054 Uiso 1 1 calc R . . O12 O 0.3130(4) 0.7089(7) 0.5834(4) 0.034(2) Uani 1 1 d . . . C13 C 0.3208(6) 0.8090(11) 0.5477(6) 0.041(4) Uani 1 1 d . . . H13A H 0.3299 0.8724 0.5768 0.049 Uiso 1 1 calc R . . H13B H 0.2868 0.8275 0.5206 0.049 Uiso 1 1 calc R . . C14 C 0.3641(6) 0.7929(11) 0.5088(6) 0.040(4) Uani 1 1 d . . . H14A H 0.3703 0.8634 0.4864 0.048 Uiso 1 1 calc R . . H14B H 0.3981 0.7734 0.5357 0.048 Uiso 1 1 calc R . . O14 O 0.3504(4) 0.7054(7) 0.4641(4) 0.030(2) Uani 1 1 d . . . C15 C 0.3904(6) 0.6949(12) 0.4221(7) 0.046(4) Uani 1 1 d . . . H15A H 0.4264 0.6839 0.4467 0.055 Uiso 1 1 calc R . . H15B H 0.3917 0.7648 0.3974 0.055 Uiso 1 1 calc R . . C16 C 0.3784(7) 0.5997(12) 0.3790(6) 0.042(4) Uani 1 1 d . . . H16A H 0.4047 0.6003 0.3477 0.051 Uiso 1 1 calc R . . H16B H 0.3418 0.6105 0.3558 0.051 Uiso 1 1 calc R . . C17 C 0.4383(6) 0.4584(13) 0.4272(7) 0.043(4) Uani 1 1 d . . . H17A H 0.4585 0.5250 0.4448 0.052 Uiso 1 1 calc R . . H17B H 0.4542 0.4349 0.3890 0.052 Uiso 1 1 calc R . . C18 C 0.4446(6) 0.3637(12) 0.4755(6) 0.040(4) Uani 1 1 d . . . H18A H 0.4210 0.2999 0.4607 0.048 Uiso 1 1 calc R . . H18B H 0.4826 0.3373 0.4818 0.048 Uiso 1 1 calc R . . O18 O 0.4292(4) 0.4073(8) 0.5332(4) 0.038(2) Uani 1 1 d . . . C19 C 0.4416(6) 0.3284(11) 0.5836(6) 0.037(4) Uani 1 1 d . . . H19A H 0.4811 0.3140 0.5904 0.045 Uiso 1 1 calc R . . H19B H 0.4228 0.2566 0.5730 0.045 Uiso 1 1 calc R . . C20 C 0.4234(7) 0.3763(12) 0.6410(6) 0.044(4) Uani 1 1 d . . . H20A H 0.4361 0.3285 0.6776 0.053 Uiso 1 1 calc R . . H20B H 0.4393 0.4519 0.6487 0.053 Uiso 1 1 calc R . . O20 O 0.3665(4) 0.3837(8) 0.6344(4) 0.038(2) Uani 1 1 d . . . C21 C 0.3474(7) 0.4122(14) 0.6938(7) 0.052(4) Uani 1 1 d . . . H21A H 0.3646 0.4827 0.7104 0.062 Uiso 1 1 calc R . . H21B H 0.3571 0.3521 0.7250 0.062 Uiso 1 1 calc R . . C22 C 0.2865(7) 0.4260(13) 0.6829(7) 0.050(4) Uani 1 1 d . . . H22A H 0.2703 0.3559 0.6645 0.060 Uiso 1 1 calc R . . H22B H 0.2728 0.4372 0.7240 0.060 Uiso 1 1 calc R . . C23 C 0.2096(6) 0.5152(12) 0.6225(6) 0.040(4) Uani 1 1 d . . . H23A H 0.1982 0.5879 0.6029 0.048 Uiso 1 1 calc R . . H23B H 0.1905 0.5055 0.6601 0.048 Uiso 1 1 calc R . . C24 C 0.1929(6) 0.4219(14) 0.5762(7) 0.055(4) Uani 1 1 d . . . H24A H 0.2049 0.3491 0.5951 0.065 Uiso 1 1 calc R . . H24B H 0.1529 0.4204 0.5670 0.065 Uiso 1 1 calc R . . O24 O 0.2160(4) 0.4371(8) 0.5190(4) 0.037(2) Uani 1 1 d . . . C25 C 0.1950(6) 0.3555(11) 0.4723(7) 0.040(4) Uani 1 1 d . . . H25A H 0.1548 0.3570 0.4668 0.048 Uiso 1 1 calc R . . H25B H 0.2070 0.2793 0.4859 0.048 Uiso 1 1 calc R . . C26 C 0.2159(6) 0.3843(12) 0.4112(7) 0.044(4) Uani 1 1 d . . . H26A H 0.2013 0.3304 0.3784 0.053 Uiso 1 1 calc R . . H26B H 0.2032 0.4600 0.3977 0.053 Uiso 1 1 calc R . . O26 O 0.2733(4) 0.3814(7) 0.4175(4) 0.031(2) Uani 1 1 d . . . C27 C 0.2931(6) 0.4101(11) 0.3595(6) 0.039(4) Uani 1 1 d . . . H27A H 0.2812 0.4868 0.3470 0.047 Uiso 1 1 calc R . . H27B H 0.2778 0.3579 0.3261 0.047 Uiso 1 1 calc R . . C28 C 0.3523(6) 0.4043(12) 0.3661(6) 0.039(4) Uani 1 1 d . . . H28A H 0.3644 0.4143 0.3240 0.046 Uiso 1 1 calc R . . H28B H 0.3637 0.3285 0.3812 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0199(11) 0.0161(11) 0.0410(12) 0.000 0.0100(10) 0.000 Pb1 0.0643(4) 0.0547(4) 0.0518(3) 0.0076(3) 0.0262(3) -0.0012(3) Pb2 0.0291(3) 0.0412(3) 0.0716(4) 0.0012(3) 0.0224(3) -0.0073(2) Pb3 0.0472(4) 0.0278(3) 0.0602(3) 0.0143(2) 0.0079(3) 0.0018(3) Pb4 0.0375(3) 0.0361(3) 0.0518(3) -0.0019(2) -0.0046(3) -0.0056(3) Pb5 0.0459(3) 0.0268(3) 0.0524(3) -0.0060(2) 0.0183(3) 0.0092(2) K11 0.0294(15) 0.0203(13) 0.0367(14) 0.0011(10) 0.0088(12) 0.0026(12) N11 0.043(7) 0.036(7) 0.035(5) 0.003(5) 0.022(5) 0.003(6) N12 0.045(7) 0.035(6) 0.028(5) 0.001(4) 0.016(5) 0.005(6) C11 0.050(10) 0.048(9) 0.034(7) -0.008(6) 0.012(7) 0.001(8) C12 0.045(9) 0.039(9) 0.054(8) -0.007(7) 0.020(7) 0.013(7) O12 0.040(6) 0.013(4) 0.053(5) 0.003(4) 0.015(4) -0.002(4) C13 0.053(10) 0.016(7) 0.051(8) -0.010(5) -0.003(7) 0.004(7) C14 0.050(9) 0.018(7) 0.048(7) 0.005(5) -0.009(7) -0.011(7) O14 0.026(5) 0.022(5) 0.044(5) 0.002(4) 0.008(4) -0.005(4) C15 0.045(8) 0.028(8) 0.072(9) 0.021(6) 0.039(7) -0.003(7) C16 0.051(9) 0.038(8) 0.042(7) 0.005(6) 0.026(7) 0.003(7) C17 0.033(8) 0.050(9) 0.049(8) -0.001(7) 0.012(7) -0.001(7) C18 0.035(8) 0.038(9) 0.047(8) -0.009(6) 0.005(7) 0.013(7) O18 0.045(6) 0.026(5) 0.046(5) 0.005(4) 0.012(5) 0.001(4) C19 0.029(7) 0.012(6) 0.074(9) 0.009(6) 0.017(7) 0.004(6) C20 0.059(10) 0.026(7) 0.045(8) 0.005(6) -0.002(7) 0.010(7) O20 0.034(5) 0.040(6) 0.041(5) 0.008(4) 0.013(4) 0.019(4) C21 0.068(12) 0.048(9) 0.043(8) 0.015(7) 0.023(8) 0.009(9) C22 0.071(11) 0.041(9) 0.045(7) 0.015(6) 0.034(8) 0.013(8) C23 0.036(8) 0.047(9) 0.042(7) -0.005(6) 0.022(7) 0.006(7) C24 0.038(8) 0.056(10) 0.080(10) 0.019(8) 0.047(8) 0.009(8) O24 0.029(5) 0.039(6) 0.042(5) -0.003(4) 0.002(4) -0.012(5) C25 0.034(8) 0.019(7) 0.065(9) -0.004(6) -0.002(7) -0.006(6) C26 0.037(8) 0.025(7) 0.071(10) -0.013(7) 0.005(8) 0.010(7) O26 0.026(5) 0.031(5) 0.038(5) -0.007(4) 0.009(4) 0.009(4) C27 0.050(9) 0.024(7) 0.041(7) -0.007(6) -0.002(7) -0.002(7) C28 0.052(9) 0.027(7) 0.042(7) -0.008(5) 0.026(7) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 Pb4 2.7155(9) . ? Ni1 Pb4 2.7155(9) 2 ? Ni1 Pb2 2.7168(9) . ? Ni1 Pb2 2.7168(9) 2 ? Ni1 Pb3 2.7200(18) 2 ? Ni1 Pb3 2.7200(18) . ? Ni1 Pb5 2.7325(18) 2 ? Ni1 Pb5 2.7325(18) . ? Ni1 Pb1 3.2097(7) . ? Ni1 Pb1 3.2097(7) 2 ? Pb1 Pb4 3.0666(10) . ? Pb1 Pb5 3.0948(9) . ? Pb1 Pb2 3.1028(9) . ? Pb1 Pb3 3.1089(9) . ? Pb2 Pb3 3.1280(9) 2 ? Pb2 Pb4 3.1414(9) 2 ? Pb2 Pb5 3.3901(9) . ? Pb2 Pb3 3.4452(9) . ? Pb3 Pb2 3.1280(9) 2 ? Pb3 Pb3 3.1452(12) 2 ? Pb3 Pb4 3.4106(9) . ? Pb4 Pb5 3.1261(8) 2 ? Pb4 Pb2 3.1414(9) 2 ? Pb4 Pb5 3.3743(9) . ? Pb5 Pb4 3.1261(8) 2 ? Pb5 Pb5 3.1410(12) 2 ? K11 O12 2.762(9) . ? K11 O20 2.809(9) . ? K11 O18 2.814(10) . ? K11 O24 2.823(10) . ? K11 O14 2.848(9) . ? K11 O26 2.925(9) . ? K11 N12 2.994(11) . ? K11 N11 3.003(11) . ? N11 C22 1.439(18) . ? N11 C23 1.468(19) . ? N11 C11 1.507(18) . ? N12 C16 1.480(17) . ? N12 C17 1.487(19) . ? N12 C28 1.488(17) . ? C11 C12 1.48(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.413(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O12 C13 1.444(16) . ? C13 C14 1.45(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O14 1.430(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O14 C15 1.424(16) . ? C15 C16 1.47(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.53(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O18 1.434(15) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O18 C19 1.437(15) . ? C19 C20 1.47(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O20 1.408(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O20 C21 1.450(17) . ? C21 C22 1.51(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.52(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O24 1.424(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O24 C25 1.448(16) . ? C25 C26 1.50(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O26 1.416(18) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O26 C27 1.431(16) . ? C27 C28 1.46(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 Pb4 Ni1 Pb4 138.92(9) . 2 ? Pb4 Ni1 Pb2 124.14(2) . . ? Pb4 Ni1 Pb2 70.66(2) 2 . ? Pb4 Ni1 Pb2 70.66(2) . 2 ? Pb4 Ni1 Pb2 124.14(2) 2 2 ? Pb2 Ni1 Pb2 141.74(9) . 2 ? Pb4 Ni1 Pb3 141.73(6) . 2 ? Pb4 Ni1 Pb3 77.73(3) 2 2 ? Pb2 Ni1 Pb3 70.25(4) . 2 ? Pb2 Ni1 Pb3 78.65(5) 2 2 ? Pb4 Ni1 Pb3 77.73(3) . . ? Pb4 Ni1 Pb3 141.73(6) 2 . ? Pb2 Ni1 Pb3 78.65(5) . . ? Pb2 Ni1 Pb3 70.25(4) 2 . ? Pb3 Ni1 Pb3 70.64(6) 2 . ? Pb4 Ni1 Pb5 70.03(4) . 2 ? Pb4 Ni1 Pb5 76.54(5) 2 2 ? Pb2 Ni1 Pb5 139.67(6) . 2 ? Pb2 Ni1 Pb5 76.94(3) 2 2 ? Pb3 Ni1 Pb5 124.761(19) 2 2 ? Pb3 Ni1 Pb5 139.929(19) . 2 ? Pb4 Ni1 Pb5 76.54(5) . . ? Pb4 Ni1 Pb5 70.03(4) 2 . ? Pb2 Ni1 Pb5 76.94(3) . . ? Pb2 Ni1 Pb5 139.67(6) 2 . ? Pb3 Ni1 Pb5 139.929(19) 2 . ? Pb3 Ni1 Pb5 124.762(19) . . ? Pb5 Ni1 Pb5 70.16(6) 2 . ? Pb4 Ni1 Pb1 61.67(2) . . ? Pb4 Ni1 Pb1 118.17(3) 2 . ? Pb2 Ni1 Pb1 62.488(19) . . ? Pb2 Ni1 Pb1 117.66(3) 2 . ? Pb3 Ni1 Pb1 117.78(6) 2 . ? Pb3 Ni1 Pb1 62.60(2) . . ? Pb5 Ni1 Pb1 117.46(6) 2 . ? Pb5 Ni1 Pb1 62.16(2) . . ? Pb4 Ni1 Pb1 118.17(3) . 2 ? Pb4 Ni1 Pb1 61.67(2) 2 2 ? Pb2 Ni1 Pb1 117.66(3) . 2 ? Pb2 Ni1 Pb1 62.488(19) 2 2 ? Pb3 Ni1 Pb1 62.60(2) 2 2 ? Pb3 Ni1 Pb1 117.78(6) . 2 ? Pb5 Ni1 Pb1 62.16(2) 2 2 ? Pb5 Ni1 Pb1 117.46(6) . 2 ? Pb1 Ni1 Pb1 179.59(8) . 2 ? Pb4 Pb1 Pb5 66.41(2) . . ? Pb4 Pb1 Pb2 102.15(2) . . ? Pb5 Pb1 Pb2 66.32(2) . . ? Pb4 Pb1 Pb3 67.04(2) . . ? Pb5 Pb1 Pb3 102.29(2) . . ? Pb2 Pb1 Pb3 67.37(2) . . ? Pb4 Pb1 Ni1 51.21(2) . . ? Pb5 Pb1 Ni1 51.33(4) . . ? Pb2 Pb1 Ni1 50.95(2) . . ? Pb3 Pb1 Ni1 50.96(4) . . ? Ni1 Pb2 Pb1 66.56(2) . . ? Ni1 Pb2 Pb3 54.92(4) . 2 ? Pb1 Pb2 Pb3 109.33(3) . 2 ? Ni1 Pb2 Pb4 54.65(3) . 2 ? Pb1 Pb2 Pb4 109.20(2) . 2 ? Pb3 Pb2 Pb4 65.91(2) 2 2 ? Ni1 Pb2 Pb5 51.74(4) . . ? Pb1 Pb2 Pb5 56.726(19) . . ? Pb3 Pb2 Pb5 103.53(2) 2 . ? Pb4 Pb2 Pb5 57.037(18) 2 . ? Ni1 Pb2 Pb3 50.72(4) . . ? Pb1 Pb2 Pb3 56.40(2) . . ? Pb3 Pb2 Pb3 56.93(2) 2 . ? Pb4 Pb2 Pb3 102.36(2) 2 . ? Pb5 Pb2 Pb3 89.95(2) . . ? Ni1 Pb3 Pb1 66.44(3) . . ? Ni1 Pb3 Pb2 54.828(16) . 2 ? Pb1 Pb3 Pb2 109.00(2) . 2 ? Ni1 Pb3 Pb3 54.68(3) . 2 ? Pb1 Pb3 Pb3 108.73(2) . 2 ? Pb2 Pb3 Pb3 66.62(2) 2 2 ? Ni1 Pb3 Pb4 51.08(3) . . ? Pb1 Pb3 Pb4 55.89(2) . . ? Pb2 Pb3 Pb4 57.231(18) 2 . ? Pb3 Pb3 Pb4 103.054(15) 2 . ? Ni1 Pb3 Pb2 50.636(16) . . ? Pb1 Pb3 Pb2 56.23(2) . . ? Pb2 Pb3 Pb2 102.59(2) 2 . ? Pb3 Pb3 Pb2 56.45(2) 2 . ? Pb4 Pb3 Pb2 88.86(2) . . ? Ni1 Pb4 Pb1 67.12(2) . . ? Ni1 Pb4 Pb5 55.24(4) . 2 ? Pb1 Pb4 Pb5 110.40(2) . 2 ? Ni1 Pb4 Pb2 54.69(3) . 2 ? Pb1 Pb4 Pb2 109.74(2) . 2 ? Pb5 Pb4 Pb2 65.49(2) 2 2 ? Ni1 Pb4 Pb5 51.96(4) . . ? Pb1 Pb4 Pb5 57.20(2) . . ? Pb5 Pb4 Pb5 57.64(2) 2 . ? Pb2 Pb4 Pb5 103.40(2) 2 . ? Ni1 Pb4 Pb3 51.19(4) . . ? Pb1 Pb4 Pb3 57.07(2) . . ? Pb5 Pb4 Pb3 103.11(2) 2 . ? Pb2 Pb4 Pb3 56.855(19) 2 . ? Pb5 Pb4 Pb3 90.80(2) . . ? Ni1 Pb5 Pb1 66.51(3) . . ? Ni1 Pb5 Pb4 54.728(15) . 2 ? Pb1 Pb5 Pb4 109.80(2) . 2 ? Ni1 Pb5 Pb5 54.92(3) . 2 ? Pb1 Pb5 Pb5 109.26(2) . 2 ? Pb4 Pb5 Pb5 65.15(2) 2 2 ? Ni1 Pb5 Pb4 51.503(16) . . ? Pb1 Pb5 Pb4 56.394(19) . . ? Pb4 Pb5 Pb4 102.89(2) 2 . ? Pb5 Pb5 Pb4 57.21(2) 2 . ? Ni1 Pb5 Pb2 51.32(3) . . ? Pb1 Pb5 Pb2 56.95(2) . . ? Pb4 Pb5 Pb2 57.472(18) 2 . ? Pb5 Pb5 Pb2 103.047(16) 2 . ? Pb4 Pb5 Pb2 90.39(2) . . ? O12 K11 O20 98.1(3) . . ? O12 K11 O18 119.6(3) . . ? O20 K11 O18 60.4(3) . . ? O12 K11 O24 96.8(3) . . ? O20 K11 O24 98.7(3) . . ? O18 K11 O24 139.0(3) . . ? O12 K11 O14 60.4(3) . . ? O20 K11 O14 137.8(3) . . ? O18 K11 O14 97.0(3) . . ? O24 K11 O14 118.4(3) . . ? O12 K11 O26 137.2(3) . . ? O20 K11 O26 118.6(3) . . ? O18 K11 O26 98.5(3) . . ? O24 K11 O26 58.6(3) . . ? O14 K11 O26 98.6(3) . . ? O12 K11 N12 120.8(3) . . ? O20 K11 N12 119.8(3) . . ? O18 K11 N12 60.7(3) . . ? O24 K11 N12 117.8(3) . . ? O14 K11 N12 61.1(3) . . ? O26 K11 N12 60.3(3) . . ? O12 K11 N11 60.0(3) . . ? O20 K11 N11 60.6(3) . . ? O18 K11 N11 120.0(3) . . ? O24 K11 N11 60.9(3) . . ? O14 K11 N11 119.6(3) . . ? O26 K11 N11 118.4(3) . . ? N12 K11 N11 178.7(3) . . ? C22 N11 C23 112.7(12) . . ? C22 N11 C11 111.1(11) . . ? C23 N11 C11 108.3(11) . . ? C22 N11 K11 108.3(8) . . ? C23 N11 K11 108.3(7) . . ? C11 N11 K11 107.9(8) . . ? C16 N12 C17 107.9(12) . . ? C16 N12 C28 109.8(10) . . ? C17 N12 C28 111.2(11) . . ? C16 N12 K11 108.6(8) . . ? C17 N12 K11 109.3(7) . . ? C28 N12 K11 109.9(8) . . ? C12 C11 N11 114.0(11) . . ? C12 C11 H11A 108.8 . . ? N11 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? N11 C11 H11B 108.8 . . ? H11A C11 H11B 107.6 . . ? O12 C12 C11 109.5(12) . . ? O12 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O12 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C12 O12 C13 113.3(10) . . ? C12 O12 K11 122.9(8) . . ? C13 O12 K11 117.8(7) . . ? O12 C13 C14 110.6(11) . . ? O12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? O12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O14 C14 C13 110.3(12) . . ? O14 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? O14 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C15 O14 C14 110.9(11) . . ? C15 O14 K11 115.4(7) . . ? C14 O14 K11 110.4(7) . . ? O14 C15 C16 111.1(12) . . ? O14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? O14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 N12 114.8(11) . . ? C15 C16 H16A 108.6 . . ? N12 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? N12 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? N12 C17 C18 111.4(12) . . ? N12 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N12 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? O18 C18 C17 107.4(11) . . ? O18 C18 H18A 110.2 . . ? C17 C18 H18A 110.2 . . ? O18 C18 H18B 110.2 . . ? C17 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 O18 C19 110.7(10) . . ? C18 O18 K11 116.3(7) . . ? C19 O18 K11 114.9(8) . . ? O18 C19 C20 108.1(11) . . ? O18 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O18 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O20 C20 C19 110.2(11) . . ? O20 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? O20 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 O20 C21 110.9(11) . . ? C20 O20 K11 112.0(8) . . ? C21 O20 K11 118.5(8) . . ? O20 C21 C22 108.4(12) . . ? O20 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O20 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? N11 C22 C21 114.4(13) . . ? N11 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? N11 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N11 C23 C24 112.8(12) . . ? N11 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? N11 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O24 C24 C23 111.2(12) . . ? O24 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? O24 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 O24 C25 111.0(11) . . ? C24 O24 K11 118.2(8) . . ? C25 O24 K11 119.8(8) . . ? O24 C25 C26 108.2(11) . . ? O24 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? O24 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O26 C26 C25 111.2(12) . . ? O26 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? O26 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 O26 C27 111.0(10) . . ? C26 O26 K11 114.1(7) . . ? C27 O26 K11 113.9(7) . . ? O26 C27 C28 110.6(11) . . ? O26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 N12 114.8(12) . . ? C27 C28 H28A 108.6 . . ? N12 C28 H28A 108.6 . . ? C27 C28 H28B 108.6 . . ? N12 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.059 _refine_diff_density_min -2.698 _refine_diff_density_rms 0.409