# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2307 data_[Li(NH~3~)~4~]~4~Sn~9~(NH~3~) _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_contact_author ; Prof. Dr. Nikolaus Korber Institut f. Anorganische Chemie, Universit\"at Regensburg 93040 Regensburg Germany ; _publ_contact_author_phone '+49 941 9434448' _publ_contact_author_fax '+49 941 9431812' _publ_contact_author_email nikolaus.korber@chemie.uni-regensburg.de loop_ _publ_author_name _publ_author_address 'Korber, Nikolaus, Prof. Dr.' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; 'Fleischmann, Andrea, Dipl.-Chem.' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; _publ_section_title ; Synthesis and Crystal Structure of [Li(NH~3~)~4~]~4~Sn~9~ · NH~3~ and [Li(NH~3~)~4~]~4~Pb~9~ · NH~3~ ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(tetraamminelithium)nonastannide-ammonia(1/1) ; _chemical_formula_moiety '4 (H12 Li N4 +), (Sn9 4-), (H3 N)' _chemical_formula_sum 'H51 Li4 N17 Sn9' _chemical_formula_weight 1385.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Sn' 'Sn' -0.6537 1.4246 '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' 'Li' 'Li' -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5292(7) _cell_length_b 17.6999(9) _cell_length_c 21.1898(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.930(8) _cell_angle_gamma 90.00 _cell_volume 3901.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 499 _cell_measurement_theta_min 9.04 _cell_measurement_theta_max 21.36 _exptl_crystal_description prism _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 5.677 _exptl_absorpt_correction_type refdelf _exptl_special_details ; crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) ; _diffrn_ambient_temperature 123(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 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method Phi _diffrn_reflns_number 25889 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6728 _reflns_number_gt 4147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 1998)' _computing_cell_refinement 'IPDS' _computing_data_reduction 'IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CIFTAB in SHELXL97' _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^)+(0.0278P)^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 6728 _refine_ls_number_parameters 296 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 0.673 _refine_ls_restrained_S_all 0.672 _refine_ls_shift/su_max 0.003 _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 Sn1 Sn 0.01312(5) 0.29482(3) 0.43163(3) 0.02460(13) Uani 1 1 d . . . Sn2 Sn 0.43790(5) 0.20382(3) 0.46990(2) 0.02080(12) Uani 1 1 d . . . Sn3 Sn 0.22858(6) 0.10378(3) 0.40863(3) 0.02262(13) Uani 1 1 d . . . Sn4 Sn 0.26972(5) 0.35210(3) 0.48671(2) 0.02040(13) Uani 1 1 d . . . Sn5 Sn 0.16777(6) 0.35555(3) 0.33684(2) 0.02148(13) Uani 1 1 d . . . Sn6 Sn 0.19157(6) 0.19870(3) 0.51986(2) 0.02280(13) Uani 1 1 d . . . Sn7 Sn 0.33675(5) 0.20657(3) 0.32002(2) 0.02017(12) Uani 1 1 d . . . Sn8 Sn 0.05536(5) 0.20145(3) 0.32140(2) 0.02051(12) Uani 1 1 d . . . Sn9 Sn 0.44187(6) 0.34037(3) 0.39076(3) 0.02323(14) Uani 1 1 d . . . N1 N 0.1711(8) 0.1370(4) 0.1568(3) 0.0312(18) Uani 1 1 d . . . H1A H 0.0841 0.1372 0.1548 0.037 Uiso 1 1 calc R . . H1B H 0.1916 0.1509 0.1183 0.037 Uiso 1 1 calc R . . H1C H 0.2070 0.1700 0.1873 0.037 Uiso 1 1 calc R . . N2 N 0.2396(7) -0.0353(4) 0.0988(3) 0.0252(16) Uani 1 1 d . . . H2A H 0.3153 -0.0608 0.1013 0.030 Uiso 1 1 calc R . . H2B H 0.2295 -0.0047 0.0638 0.030 Uiso 1 1 calc R . . H2C H 0.1734 -0.0688 0.0954 0.030 Uiso 1 1 calc R . . N3 N 0.4253(8) 0.0272(5) 0.2268(4) 0.049(2) Uani 1 1 d . . . H3A H 0.4379 0.0670 0.2543 0.059 Uiso 1 1 calc R . . H3B H 0.4811 0.0305 0.1981 0.059 Uiso 1 1 calc R . . H3C H 0.4392 -0.0167 0.2491 0.059 Uiso 1 1 calc R . . N4 N 0.1261(7) -0.0107(4) 0.2442(3) 0.0291(17) Uani 1 1 d . . . H4A H 0.0603 -0.0386 0.2230 0.035 Uiso 1 1 calc R . . H4B H 0.0937 0.0291 0.2637 0.035 Uiso 1 1 calc R . . H4C H 0.1743 -0.0401 0.2741 0.035 Uiso 1 1 calc R . . N5 N -0.3968(7) 0.4453(4) 0.5607(3) 0.0295(17) Uani 1 1 d . . . H5A H -0.4353 0.4176 0.5269 0.035 Uiso 1 1 calc R . . H5B H -0.3830 0.4932 0.5476 0.035 Uiso 1 1 calc R . . H5C H -0.4485 0.4468 0.5913 0.035 Uiso 1 1 calc R . . N6 N -0.2240(7) 0.2914(4) 0.5590(3) 0.0304(17) Uani 1 1 d . . . H6A H -0.3053 0.2785 0.5410 0.036 Uiso 1 1 calc R . . H6B H -0.1944 0.2576 0.5902 0.036 Uiso 1 1 calc R . . H6C H -0.1719 0.2909 0.5285 0.036 Uiso 1 1 calc R . . N7 N -0.2022(8) 0.4155(4) 0.6970(3) 0.0354(19) Uani 1 1 d . . . H7A H -0.2763 0.4031 0.7117 0.042 Uiso 1 1 calc R . . H7B H -0.1839 0.4651 0.7054 0.042 Uiso 1 1 calc R . . H7C H -0.1368 0.3864 0.7169 0.042 Uiso 1 1 calc R . . N8 N -0.0735(7) 0.4548(4) 0.5680(3) 0.0300(17) Uani 1 1 d . . . H8A H -0.0451 0.4288 0.5358 0.036 Uiso 1 1 calc R . . H8B H -0.0084 0.4595 0.6014 0.036 Uiso 1 1 calc R . . H8C H -0.1006 0.5015 0.5538 0.036 Uiso 1 1 calc R . . N9 N 0.2910(7) -0.1562(4) 0.6366(4) 0.039(2) Uani 1 1 d . . . H9A H 0.3180 -0.1893 0.6086 0.047 Uiso 1 1 calc R . . H9B H 0.2201 -0.1750 0.6507 0.047 Uiso 1 1 calc R . . H9C H 0.3547 -0.1492 0.6704 0.047 Uiso 1 1 calc R . . N10 N 0.4028(7) -0.0018(4) 0.5698(3) 0.0300(18) Uani 1 1 d . . . H10A H 0.4758 -0.0223 0.5917 0.036 Uiso 1 1 calc R . . H10B H 0.3983 0.0479 0.5804 0.036 Uiso 1 1 calc R . . H10C H 0.4040 -0.0060 0.5271 0.036 Uiso 1 1 calc R . . N11 N 0.1236(7) 0.0108(4) 0.6379(4) 0.0349(19) Uani 1 1 d . . . H11A H 0.1625 0.0223 0.6781 0.042 Uiso 1 1 calc R . . H11B H 0.0493 -0.0148 0.6399 0.042 Uiso 1 1 calc R . . H11C H 0.1055 0.0541 0.6151 0.042 Uiso 1 1 calc R . . N12 N 0.1313(8) -0.0805(5) 0.5072(4) 0.045(2) Uani 1 1 d . . . H12A H 0.1483 -0.0472 0.4770 0.054 Uiso 1 1 calc R . . H12B H 0.0473 -0.0764 0.5124 0.054 Uiso 1 1 calc R . . H12C H 0.1469 -0.1284 0.4947 0.054 Uiso 1 1 calc R . . N13 N 0.6988(7) 0.1704(4) 0.7743(3) 0.0282(17) Uani 1 1 d . . . H13A H 0.7174 0.1226 0.7888 0.034 Uiso 1 1 calc R . . H13B H 0.6594 0.1960 0.8030 0.034 Uiso 1 1 calc R . . H13C H 0.7728 0.1946 0.7692 0.034 Uiso 1 1 calc R . . N14 N 0.5305(7) 0.2745(4) 0.6585(3) 0.0331(18) Uani 1 1 d . . . H14A H 0.6028 0.2993 0.6516 0.040 Uiso 1 1 calc R . . H14B H 0.4954 0.2985 0.6895 0.040 Uiso 1 1 calc R . . H14C H 0.4729 0.2738 0.6217 0.040 Uiso 1 1 calc R . . N15 N 0.3927(7) 0.1278(4) 0.6911(3) 0.0294(18) Uani 1 1 d . . . H15A H 0.3367 0.1495 0.6592 0.035 Uiso 1 1 calc R . . H15B H 0.3705 0.1405 0.7295 0.035 Uiso 1 1 calc R . . H15C H 0.3898 0.0767 0.6865 0.035 Uiso 1 1 calc R . . N16 N 0.6729(6) 0.1131(4) 0.6203(3) 0.0236(15) Uani 1 1 d . . . H16A H 0.6713 0.0622 0.6260 0.028 Uiso 1 1 calc R . . H16B H 0.7559 0.1293 0.6257 0.028 Uiso 1 1 calc R . . H16C H 0.6336 0.1248 0.5802 0.028 Uiso 1 1 calc R . . N17 N -0.0419(8) 0.3162(4) 0.1566(3) 0.033(2) Uani 1 1 d D . . H17A H -0.001(8) 0.352(3) 0.177(3) 0.040 Uiso 1 1 d D . . H17B H -0.024(9) 0.282(3) 0.184(3) 0.040 Uiso 1 1 d D . . H17C H 0.014(7) 0.305(4) 0.134(4) 0.040 Uiso 1 1 d D . . Li1 Li 0.2409(13) 0.0292(7) 0.1795(6) 0.025(3) Uani 1 1 d . . . Li2 Li -0.2250(13) 0.3968(7) 0.5974(6) 0.022(3) Uani 1 1 d . . . Li3 Li 0.2475(13) -0.0572(7) 0.5927(6) 0.021(3) Uani 1 1 d . . . Li4 Li 0.5767(14) 0.1656(8) 0.6866(8) 0.033(4) 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 Sn1 0.0165(3) 0.0331(3) 0.0252(3) -0.0028(3) 0.0063(3) 0.0041(3) Sn2 0.0166(3) 0.0252(3) 0.0189(3) -0.0001(2) -0.0027(2) 0.0020(3) Sn3 0.0303(3) 0.0137(3) 0.0220(3) -0.0003(2) -0.0017(3) -0.0025(2) Sn4 0.0270(3) 0.0170(3) 0.0180(3) -0.0049(2) 0.0061(3) -0.0044(2) Sn5 0.0273(3) 0.0173(3) 0.0190(3) 0.0044(2) 0.0008(3) 0.0019(2) Sn6 0.0292(3) 0.0212(3) 0.0198(3) 0.0035(2) 0.0096(3) -0.0021(3) Sn7 0.0183(3) 0.0262(3) 0.0170(3) -0.0056(2) 0.0055(2) -0.0015(3) Sn8 0.0148(3) 0.0226(3) 0.0225(3) -0.0034(2) -0.0023(2) -0.0014(2) Sn9 0.0227(3) 0.0256(3) 0.0227(3) -0.0045(2) 0.0076(3) -0.0105(3) N1 0.042(5) 0.025(4) 0.025(4) -0.001(3) 0.001(4) 0.001(3) N2 0.024(4) 0.025(4) 0.027(4) 0.005(3) 0.008(3) 0.002(3) N3 0.036(5) 0.038(5) 0.067(6) -0.005(4) -0.009(5) 0.004(4) N4 0.035(5) 0.032(4) 0.020(4) -0.004(3) 0.002(4) -0.003(3) N5 0.023(4) 0.025(4) 0.037(4) 0.002(3) -0.009(4) -0.003(3) N6 0.029(4) 0.027(4) 0.035(4) -0.003(3) 0.008(4) 0.000(3) N7 0.033(5) 0.042(5) 0.029(4) 0.005(3) -0.001(4) 0.006(4) N8 0.035(5) 0.028(4) 0.029(4) 0.000(3) 0.010(4) -0.001(3) N9 0.027(4) 0.039(5) 0.054(5) 0.013(4) 0.017(4) 0.000(4) N10 0.029(5) 0.026(4) 0.037(4) 0.004(3) 0.011(4) -0.003(3) N11 0.032(5) 0.039(4) 0.034(4) 0.004(3) 0.005(4) 0.001(4) N12 0.051(6) 0.043(5) 0.045(5) -0.007(4) 0.018(5) -0.013(4) N13 0.033(4) 0.023(4) 0.030(4) -0.010(3) 0.012(4) 0.000(3) N14 0.035(5) 0.031(4) 0.035(4) 0.000(3) 0.009(4) 0.003(3) N15 0.036(5) 0.030(4) 0.024(4) 0.003(3) 0.010(4) 0.001(3) N16 0.019(4) 0.030(4) 0.020(4) 0.001(3) -0.001(3) -0.005(3) N17 0.039(5) 0.034(5) 0.028(4) 0.000(3) 0.006(4) 0.000(3) Li1 0.022(8) 0.023(7) 0.029(8) -0.001(6) 0.003(7) 0.008(6) Li2 0.023(7) 0.018(6) 0.025(7) -0.004(6) 0.000(6) 0.005(6) Li3 0.020(8) 0.012(6) 0.029(8) 0.000(5) 0.000(7) -0.002(5) Li4 0.021(8) 0.030(8) 0.049(9) -0.010(7) 0.005(8) -0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Sn8 2.9508(7) . ? Sn1 Sn4 2.9514(8) . ? Sn1 Sn6 2.9715(9) . ? Sn1 Sn5 2.9759(7) . ? Sn2 Sn9 2.9456(8) . ? Sn2 Sn6 2.9510(7) . ? Sn2 Sn3 2.9649(8) . ? Sn2 Sn7 3.1895(8) . ? Sn2 Sn4 3.2165(8) . ? Sn3 Sn8 2.9470(9) . ? Sn3 Sn7 2.9660(7) . ? Sn3 Sn6 2.9691(7) . ? Sn4 Sn9 2.9336(7) . ? Sn4 Sn6 2.9532(8) . ? Sn4 Sn5 3.1910(8) . ? Sn5 Sn9 2.9468(9) . ? Sn5 Sn8 2.9710(8) . ? Sn5 Sn7 3.2315(8) . ? Sn7 Sn9 2.9267(8) . ? Sn7 Sn8 2.9689(7) . ? N1 Li1 2.074(15) . ? N2 Li1 2.056(15) . ? N3 Li1 2.043(17) . ? N4 Li1 2.086(14) . ? N5 Li2 2.044(15) . ? N6 Li2 2.037(14) . ? N7 Li2 2.113(14) . ? N8 Li2 2.072(15) . ? N9 Li3 2.004(15) . ? N10 Li3 2.029(14) . ? N11 Li3 2.110(14) . ? N12 Li3 2.064(16) . ? N13 Li4 2.090(18) . ? N14 Li4 2.053(17) . ? N15 Li4 2.066(16) . ? N16 Li4 2.074(15) . ? 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 Sn8 Sn1 Sn4 105.32(2) . . ? Sn8 Sn1 Sn6 91.09(2) . . ? Sn4 Sn1 Sn6 59.81(2) . . ? Sn8 Sn1 Sn5 60.170(18) . . ? Sn4 Sn1 Sn5 65.143(19) . . ? Sn6 Sn1 Sn5 105.82(2) . . ? Sn9 Sn2 Sn6 108.68(2) . . ? Sn9 Sn2 Sn3 108.42(2) . . ? Sn6 Sn2 Sn3 60.249(19) . . ? Sn9 Sn2 Sn7 56.816(18) . . ? Sn6 Sn2 Sn7 100.45(2) . . ? Sn3 Sn2 Sn7 57.483(18) . . ? Sn9 Sn2 Sn4 56.653(17) . . ? Sn6 Sn2 Sn4 57.022(17) . . ? Sn3 Sn2 Sn4 98.70(2) . . ? Sn7 Sn2 Sn4 89.62(2) . . ? Sn8 Sn3 Sn2 105.66(2) . . ? Sn8 Sn3 Sn7 60.277(18) . . ? Sn2 Sn3 Sn7 65.066(19) . . ? Sn8 Sn3 Sn6 91.21(2) . . ? Sn2 Sn3 Sn6 59.644(18) . . ? Sn7 Sn3 Sn6 105.43(2) . . ? Sn9 Sn4 Sn1 109.13(2) . . ? Sn9 Sn4 Sn6 108.95(2) . . ? Sn1 Sn4 Sn6 60.43(2) . . ? Sn9 Sn4 Sn5 57.333(19) . . ? Sn1 Sn4 Sn5 57.800(19) . . ? Sn6 Sn4 Sn5 101.02(2) . . ? Sn9 Sn4 Sn2 57.011(17) . . ? Sn1 Sn4 Sn2 99.32(2) . . ? Sn6 Sn4 Sn2 56.958(17) . . ? Sn5 Sn4 Sn2 90.650(19) . . ? Sn9 Sn5 Sn8 107.97(2) . . ? Sn9 Sn5 Sn1 108.12(2) . . ? Sn8 Sn5 Sn1 59.496(18) . . ? Sn9 Sn5 Sn4 56.938(19) . . ? Sn8 Sn5 Sn4 99.13(2) . . ? Sn1 Sn5 Sn4 57.058(18) . . ? Sn9 Sn5 Sn7 56.323(18) . . ? Sn8 Sn5 Sn7 57.010(17) . . ? Sn1 Sn5 Sn7 98.51(2) . . ? Sn4 Sn5 Sn7 89.33(2) . . ? Sn2 Sn6 Sn4 66.020(19) . . ? Sn2 Sn6 Sn3 60.107(19) . . ? Sn4 Sn6 Sn3 104.81(2) . . ? Sn2 Sn6 Sn1 105.18(2) . . ? Sn4 Sn6 Sn1 59.76(2) . . ? Sn3 Sn6 Sn1 88.43(2) . . ? Sn9 Sn7 Sn3 108.91(2) . . ? Sn9 Sn7 Sn8 108.56(2) . . ? Sn3 Sn7 Sn8 59.546(19) . . ? Sn9 Sn7 Sn2 57.388(19) . . ? Sn3 Sn7 Sn2 57.451(18) . . ? Sn8 Sn7 Sn2 99.74(2) . . ? Sn9 Sn7 Sn5 56.918(19) . . ? Sn3 Sn7 Sn5 99.128(19) . . ? Sn8 Sn7 Sn5 57.074(18) . . ? Sn2 Sn7 Sn5 90.41(2) . . ? Sn3 Sn8 Sn1 89.24(2) . . ? Sn3 Sn8 Sn7 60.177(19) . . ? Sn1 Sn8 Sn7 105.30(2) . . ? Sn3 Sn8 Sn5 105.80(2) . . ? Sn1 Sn8 Sn5 60.334(18) . . ? Sn7 Sn8 Sn5 65.916(19) . . ? Sn7 Sn9 Sn4 100.78(2) . . ? Sn7 Sn9 Sn2 65.796(19) . . ? Sn4 Sn9 Sn2 66.336(18) . . ? Sn7 Sn9 Sn5 66.76(2) . . ? Sn4 Sn9 Sn5 65.73(2) . . ? Sn2 Sn9 Sn5 101.30(2) . . ? N3 Li1 N2 106.4(6) . . ? N3 Li1 N1 113.9(7) . . ? N2 Li1 N1 111.1(7) . . ? N3 Li1 N4 106.0(7) . . ? N2 Li1 N4 115.4(7) . . ? N1 Li1 N4 104.1(6) . . ? N6 Li2 N5 106.9(7) . . ? N6 Li2 N8 106.3(6) . . ? N5 Li2 N8 110.8(7) . . ? N6 Li2 N7 122.4(7) . . ? N5 Li2 N7 105.7(6) . . ? N8 Li2 N7 104.5(7) . . ? N9 Li3 N10 113.5(7) . . ? N9 Li3 N12 107.1(7) . . ? N10 Li3 N12 106.1(6) . . ? N9 Li3 N11 113.6(6) . . ? N10 Li3 N11 114.3(6) . . ? N12 Li3 N11 100.8(7) . . ? N14 Li4 N15 97.8(7) . . ? N14 Li4 N16 110.0(7) . . ? N15 Li4 N16 116.5(7) . . ? N14 Li4 N13 107.8(7) . . ? N15 Li4 N13 115.1(7) . . ? N16 Li4 N13 108.8(7) . . ? 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 Sn6 Sn3 Sn8 Sn1 -1.06(2) . . . . ? Sn4 Sn1 Sn5 Sn9 26.37(2) . . . . ? Sn2 Sn9 Sn7 Sn3 26.58(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.556 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.155 #===END data_[Li(NH~3~)~4~]~4~Pb~9~(NH~3~) _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_contact_author ; Prof. Dr. Nikolaus Korber Institut f. Anorganische Chemie, Universit\"at Regensburg 93040 Regensburg Germany ; _publ_contact_author_phone '+49 941 9434448' _publ_contact_author_fax '+49 941 9431812' _publ_contact_author_email nikolaus.korber@chemie.uni-regensburg.de loop_ _publ_author_name _publ_author_address 'Korber, Nikolaus, Prof. Dr.' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; 'Fleischmann, Andrea, Dipl.-Chem.' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; _publ_section_title ; Synthesis and Crystal Structure of [Li(NH~3~)~4~]~4~Sn~9~ · NH~3~ and [Li(NH~3~)~4~]~4~Pb~9~ · NH~3~ ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(tetraamminelithium)nonaplumbide-ammonia(1/1) ; _chemical_formula_moiety '4 (H12 Li N4 +), (Pb9 4-), (H3 N)' _chemical_formula_sum 'H51 Li4 N17 Pb9' _chemical_formula_weight 2182.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 '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' 'Li' 'Li' -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6109(8) _cell_length_b 17.8636(9) _cell_length_c 21.4144(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.046(9) _cell_angle_gamma 90.00 _cell_volume 4008.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 499 _cell_measurement_theta_min 11.91 _cell_measurement_theta_max 23.19 _exptl_crystal_description prism _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 37.667 _exptl_absorpt_correction_type refdelf _exptl_special_details ; crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) ; _diffrn_ambient_temperature 123(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 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method Phi _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19948 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.79 _reflns_number_total 7491 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 1998)' _computing_cell_refinement 'IPDS' _computing_data_reduction 'IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CIFTAB in SHELXL97' _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^)+(0.0278P)^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 7491 _refine_ls_number_parameters 296 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.00614(5) 0.29551(4) 0.43218(3) 0.02839(15) Uani 1 1 d . . . Pb2 Pb 0.44533(5) 0.20105(4) 0.47242(3) 0.02415(14) Uani 1 1 d . . . Pb3 Pb 0.22677(6) 0.09835(4) 0.40897(3) 0.02619(14) Uani 1 1 d . . . Pb4 Pb 0.27200(6) 0.35520(4) 0.49019(3) 0.02247(14) Uani 1 1 d . . . Pb5 Pb 0.16646(6) 0.35924(4) 0.33437(3) 0.02518(14) Uani 1 1 d . . . Pb6 Pb 0.18977(6) 0.19645(4) 0.52375(3) 0.02555(14) Uani 1 1 d . . . Pb7 Pb 0.34150(5) 0.20360(4) 0.31736(2) 0.02266(13) Uani 1 1 d . . . Pb8 Pb 0.05004(5) 0.19984(4) 0.31844(3) 0.02310(14) Uani 1 1 d . . . Pb9 Pb 0.44870(6) 0.34199(4) 0.39083(3) 0.02601(15) Uani 1 1 d . . . N1 N 0.1716(16) 0.1374(9) 0.1577(6) 0.040(4) Uani 1 1 d . . . H1A H 0.0848 0.1374 0.1505 0.048 Uiso 1 1 calc R . . H1B H 0.2014 0.1530 0.1223 0.048 Uiso 1 1 calc R . . H1C H 0.2001 0.1689 0.1903 0.048 Uiso 1 1 calc R . . N2 N 0.2352(12) -0.0350(8) 0.1002(6) 0.027(3) Uani 1 1 d . . . H2A H 0.3012 -0.0681 0.1063 0.032 Uiso 1 1 calc R . . H2B H 0.2432 -0.0047 0.0669 0.032 Uiso 1 1 calc R . . H2C H 0.1601 -0.0604 0.0920 0.032 Uiso 1 1 calc R . . N3 N 0.4298(16) 0.0268(11) 0.2224(10) 0.069(7) Uani 1 1 d . . . H3A H 0.4512 0.0715 0.2418 0.083 Uiso 1 1 calc R . . H3B H 0.4794 0.0187 0.1921 0.083 Uiso 1 1 calc R . . H3C H 0.4422 -0.0106 0.2516 0.083 Uiso 1 1 calc R . . N4 N 0.1301(16) -0.0107(9) 0.2438(7) 0.042(4) Uani 1 1 d . . . H4A H 0.0671 -0.0405 0.2235 0.051 Uiso 1 1 calc R . . H4B H 0.0948 0.0282 0.2623 0.051 Uiso 1 1 calc R . . H4C H 0.1803 -0.0378 0.2741 0.051 Uiso 1 1 calc R . . N5 N -0.3948(13) 0.4449(8) 0.5605(7) 0.035(4) Uani 1 1 d . . . H5A H -0.4081 0.4422 0.5175 0.042 Uiso 1 1 calc R . . H5B H -0.3922 0.4937 0.5727 0.042 Uiso 1 1 calc R . . H5C H -0.4595 0.4211 0.5758 0.042 Uiso 1 1 calc R . . N6 N -0.2219(14) 0.2913(9) 0.5604(6) 0.035(3) Uani 1 1 d . . . H6A H -0.3011 0.2705 0.5559 0.042 Uiso 1 1 calc R . . H6B H -0.1666 0.2632 0.5875 0.042 Uiso 1 1 calc R . . H6C H -0.1952 0.2931 0.5220 0.042 Uiso 1 1 calc R . . N7 N -0.2018(15) 0.4157(10) 0.6944(6) 0.042(4) Uani 1 1 d . . . H7A H -0.2743 0.4034 0.7098 0.050 Uiso 1 1 calc R . . H7B H -0.1840 0.4650 0.7020 0.050 Uiso 1 1 calc R . . H7C H -0.1358 0.3874 0.7139 0.050 Uiso 1 1 calc R . . N8 N -0.0745(13) 0.4537(8) 0.5681(7) 0.032(3) Uani 1 1 d . . . H8A H -0.0502 0.4314 0.5337 0.038 Uiso 1 1 calc R . . H8B H -0.0080 0.4534 0.6007 0.038 Uiso 1 1 calc R . . H8C H -0.0983 0.5018 0.5585 0.038 Uiso 1 1 calc R . . N9 N 0.2941(16) -0.1567(9) 0.6381(8) 0.047(4) Uani 1 1 d . . . H9A H 0.3377 -0.1860 0.6141 0.056 Uiso 1 1 calc R . . H9B H 0.2208 -0.1803 0.6440 0.056 Uiso 1 1 calc R . . H9C H 0.3432 -0.1482 0.6763 0.056 Uiso 1 1 calc R . . N10 N 0.4038(12) 0.0001(8) 0.5712(7) 0.030(3) Uani 1 1 d . . . H10A H 0.4650 -0.0330 0.5639 0.036 Uiso 1 1 calc R . . H10B H 0.4355 0.0306 0.6040 0.036 Uiso 1 1 calc R . . H10C H 0.3793 0.0281 0.5359 0.036 Uiso 1 1 calc R . . N11 N 0.1282(13) 0.0098(9) 0.6392(7) 0.039(4) Uani 1 1 d . . . H11A H 0.1714 0.0264 0.6767 0.047 Uiso 1 1 calc R . . H11B H 0.0599 -0.0179 0.6462 0.047 Uiso 1 1 calc R . . H11C H 0.1006 0.0497 0.6143 0.047 Uiso 1 1 calc R . . N12 N 0.1366(14) -0.0817(9) 0.5106(7) 0.040(4) Uani 1 1 d . . . H12A H 0.1428 -0.0448 0.4819 0.048 Uiso 1 1 calc R . . H12B H 0.0542 -0.0855 0.5173 0.048 Uiso 1 1 calc R . . H12C H 0.1617 -0.1260 0.4955 0.048 Uiso 1 1 calc R . . N13 N 0.7013(13) 0.1713(9) 0.7733(6) 0.037(4) Uani 1 1 d . . . H13A H 0.7082 0.1265 0.7937 0.044 Uiso 1 1 calc R . . H13B H 0.6693 0.2060 0.7977 0.044 Uiso 1 1 calc R . . H13C H 0.7797 0.1862 0.7661 0.044 Uiso 1 1 calc R . . N14 N 0.5290(14) 0.2743(10) 0.6589(7) 0.044(4) Uani 1 1 d . . . H14A H 0.6001 0.2992 0.6518 0.053 Uiso 1 1 calc R . . H14B H 0.4951 0.2977 0.6902 0.053 Uiso 1 1 calc R . . H14C H 0.4707 0.2738 0.6229 0.053 Uiso 1 1 calc R . . N15 N 0.3954(14) 0.1269(9) 0.6937(7) 0.038(4) Uani 1 1 d . . . H15A H 0.3410 0.1446 0.6598 0.046 Uiso 1 1 calc R . . H15B H 0.3725 0.1453 0.7299 0.046 Uiso 1 1 calc R . . H15C H 0.3917 0.0760 0.6942 0.046 Uiso 1 1 calc R . . N16 N 0.6714(13) 0.1127(8) 0.6217(6) 0.028(3) Uani 1 1 d . . . H16A H 0.6668 0.0620 0.6247 0.034 Uiso 1 1 calc R . . H16B H 0.7547 0.1271 0.6285 0.034 Uiso 1 1 calc R . . H16C H 0.6343 0.1274 0.5824 0.034 Uiso 1 1 calc R . . N17 N -0.0422(14) 0.3177(9) 0.1568(7) 0.031(4) Uani 1 1 d D . . H17A H 0.038(10) 0.312(9) 0.177(7) 0.037 Uiso 1 1 d D . . H17B H -0.035(16) 0.274(6) 0.177(7) 0.037 Uiso 1 1 d D . . H17C H -0.001(14) 0.286(8) 0.135(6) 0.037 Uiso 1 1 d D . . Li1 Li 0.238(3) 0.0292(17) 0.1807(13) 0.030(7) Uani 1 1 d . . . Li2 Li -0.228(3) 0.3952(17) 0.5947(12) 0.030(6) Uani 1 1 d . . . Li3 Li 0.250(2) -0.0569(16) 0.5932(13) 0.029(6) Uani 1 1 d . . . Li4 Li 0.579(2) 0.1604(15) 0.6873(11) 0.020(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0178(3) 0.0375(4) 0.0312(3) -0.0044(3) 0.0082(2) 0.0059(3) Pb2 0.0175(3) 0.0286(4) 0.0241(3) -0.0004(3) -0.0036(2) 0.0028(3) Pb3 0.0346(3) 0.0147(3) 0.0268(3) -0.0003(3) -0.0025(2) -0.0027(3) Pb4 0.0300(3) 0.0186(3) 0.0205(3) -0.0066(2) 0.0091(2) -0.0061(3) Pb5 0.0318(3) 0.0189(3) 0.0240(3) 0.0055(3) 0.0016(2) 0.0015(3) Pb6 0.0328(3) 0.0230(3) 0.0230(3) 0.0039(3) 0.0111(2) -0.0035(3) Pb7 0.0193(3) 0.0300(4) 0.0202(3) -0.0090(3) 0.0077(2) -0.0029(3) Pb8 0.0153(2) 0.0250(3) 0.0270(3) -0.0055(3) -0.0029(2) -0.0010(3) Pb9 0.0246(3) 0.0295(4) 0.0260(3) -0.0052(3) 0.0104(2) -0.0126(3) N1 0.061(10) 0.039(10) 0.020(7) -0.002(7) 0.002(6) 0.014(8) N2 0.021(7) 0.036(9) 0.024(7) 0.001(6) 0.006(5) 0.002(6) N3 0.032(9) 0.061(14) 0.103(15) -0.033(12) -0.028(10) 0.021(9) N4 0.066(11) 0.036(10) 0.027(8) 0.003(7) 0.015(7) 0.002(9) N5 0.029(8) 0.023(8) 0.049(9) -0.001(7) -0.010(6) -0.013(7) N6 0.037(8) 0.033(9) 0.036(8) 0.006(7) 0.009(6) -0.004(7) N7 0.044(9) 0.049(11) 0.035(8) -0.004(7) 0.014(7) -0.005(8) N8 0.034(8) 0.017(8) 0.042(8) 0.002(6) 0.000(6) 0.000(6) N9 0.045(9) 0.031(10) 0.066(11) 0.006(8) 0.012(8) 0.004(8) N10 0.020(7) 0.029(9) 0.043(8) 0.001(7) 0.008(6) 0.003(6) N11 0.019(7) 0.046(10) 0.052(9) -0.007(8) 0.007(6) -0.003(7) N12 0.042(9) 0.040(10) 0.045(9) -0.010(7) 0.026(7) -0.023(8) N13 0.026(7) 0.045(10) 0.037(8) -0.006(7) 0.001(6) 0.000(7) N14 0.038(9) 0.053(12) 0.050(9) -0.007(8) 0.029(7) -0.009(8) N15 0.043(9) 0.038(10) 0.038(8) -0.005(7) 0.024(7) -0.011(8) N16 0.028(7) 0.032(9) 0.026(7) 0.002(6) 0.007(5) 0.000(7) N17 0.027(7) 0.037(10) 0.033(8) 0.005(7) 0.017(6) 0.006(7) Li1 0.026(14) 0.030(17) 0.035(15) -0.008(13) 0.006(11) 0.014(12) Li2 0.029(14) 0.034(17) 0.028(13) -0.012(13) 0.011(11) 0.001(13) Li3 0.021(13) 0.022(16) 0.041(16) 0.005(12) -0.002(11) 0.005(12) Li4 0.005(10) 0.030(16) 0.022(12) 0.001(11) -0.006(8) -0.012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Pb8 3.0703(9) . ? Pb1 Pb4 3.0881(8) . ? Pb1 Pb6 3.0937(9) . ? Pb1 Pb5 3.1142(9) . ? Pb2 Pb9 3.0680(9) . ? Pb2 Pb6 3.0832(9) . ? Pb2 Pb3 3.0982(9) . ? Pb2 Pb7 3.3303(8) . ? Pb2 Pb4 3.3660(9) . ? Pb3 Pb8 3.0690(9) . ? Pb3 Pb6 3.0937(9) . ? Pb3 Pb7 3.1009(9) . ? Pb4 Pb9 3.0582(9) . ? Pb4 Pb6 3.0849(9) . ? Pb4 Pb5 3.3493(8) . ? Pb5 Pb9 3.0638(9) . ? Pb5 Pb8 3.1013(9) . ? Pb5 Pb7 3.3949(9) . ? Pb7 Pb9 3.0526(9) . ? Pb7 Pb8 3.0971(8) . ? N1 Li1 2.09(3) . ? N2 Li1 2.07(3) . ? N3 Li1 2.09(3) . ? N4 Li1 2.03(3) . ? N5 Li2 2.01(3) . ? N6 Li2 2.00(3) . ? N7 Li2 2.14(3) . ? N8 Li2 2.09(3) . ? N9 Li3 2.04(3) . ? N10 Li3 2.04(3) . ? N11 Li3 2.11(3) . ? N12 Li3 2.03(3) . ? N13 Li4 2.09(2) . ? N14 Li4 2.17(3) . ? N15 Li4 2.07(3) . ? N16 Li4 2.02(3) . ? 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 Pb8 Pb1 Pb4 105.57(2) . . ? Pb8 Pb1 Pb6 91.46(2) . . ? Pb4 Pb1 Pb6 59.87(2) . . ? Pb8 Pb1 Pb5 60.19(2) . . ? Pb4 Pb1 Pb5 65.37(2) . . ? Pb6 Pb1 Pb5 106.21(2) . . ? Pb9 Pb2 Pb6 108.33(2) . . ? Pb9 Pb2 Pb3 108.13(2) . . ? Pb6 Pb2 Pb3 60.06(2) . . ? Pb9 Pb2 Pb7 56.814(19) . . ? Pb6 Pb2 Pb7 100.62(2) . . ? Pb3 Pb2 Pb7 57.545(19) . . ? Pb9 Pb2 Pb4 56.533(19) . . ? Pb6 Pb2 Pb4 56.951(19) . . ? Pb3 Pb2 Pb4 98.59(2) . . ? Pb7 Pb2 Pb4 90.03(2) . . ? Pb8 Pb3 Pb6 91.49(2) . . ? Pb8 Pb3 Pb2 105.55(3) . . ? Pb6 Pb3 Pb2 59.73(2) . . ? Pb8 Pb3 Pb7 60.258(19) . . ? Pb6 Pb3 Pb7 105.71(2) . . ? Pb2 Pb3 Pb7 64.99(2) . . ? Pb9 Pb4 Pb6 108.54(2) . . ? Pb9 Pb4 Pb1 108.35(2) . . ? Pb6 Pb4 Pb1 60.16(2) . . ? Pb9 Pb4 Pb5 56.913(19) . . ? Pb6 Pb4 Pb5 100.92(2) . . ? Pb1 Pb4 Pb5 57.69(2) . . ? Pb9 Pb4 Pb2 56.81(2) . . ? Pb6 Pb4 Pb2 56.903(19) . . ? Pb1 Pb4 Pb2 98.79(2) . . ? Pb5 Pb4 Pb2 90.46(2) . . ? Pb9 Pb5 Pb8 107.39(2) . . ? Pb9 Pb5 Pb1 107.53(2) . . ? Pb8 Pb5 Pb1 59.21(2) . . ? Pb9 Pb5 Pb4 56.753(19) . . ? Pb8 Pb5 Pb4 98.91(2) . . ? Pb1 Pb5 Pb4 56.941(18) . . ? Pb9 Pb5 Pb7 56.128(18) . . ? Pb8 Pb5 Pb7 56.731(18) . . ? Pb1 Pb5 Pb7 97.97(2) . . ? Pb4 Pb5 Pb7 89.22(2) . . ? Pb2 Pb6 Pb4 66.15(2) . . ? Pb2 Pb6 Pb3 60.21(2) . . ? Pb4 Pb6 Pb3 105.05(2) . . ? Pb2 Pb6 Pb1 105.09(2) . . ? Pb4 Pb6 Pb1 59.97(2) . . ? Pb3 Pb6 Pb1 88.07(2) . . ? Pb9 Pb7 Pb8 107.78(2) . . ? Pb9 Pb7 Pb3 108.45(2) . . ? Pb8 Pb7 Pb3 59.36(2) . . ? Pb9 Pb7 Pb2 57.258(19) . . ? Pb8 Pb7 Pb2 99.58(2) . . ? Pb3 Pb7 Pb2 57.466(19) . . ? Pb9 Pb7 Pb5 56.44(2) . . ? Pb8 Pb7 Pb5 56.849(19) . . ? Pb3 Pb7 Pb5 98.79(2) . . ? Pb2 Pb7 Pb5 90.29(2) . . ? Pb3 Pb8 Pb1 88.94(2) . . ? Pb3 Pb8 Pb7 60.38(2) . . ? Pb1 Pb8 Pb7 105.67(2) . . ? Pb3 Pb8 Pb5 106.24(2) . . ? Pb1 Pb8 Pb5 60.61(2) . . ? Pb7 Pb8 Pb5 66.42(2) . . ? Pb7 Pb9 Pb4 101.62(2) . . ? Pb7 Pb9 Pb5 67.43(2) . . ? Pb4 Pb9 Pb5 66.33(2) . . ? Pb7 Pb9 Pb2 65.93(2) . . ? Pb4 Pb9 Pb2 66.66(2) . . ? Pb5 Pb9 Pb2 102.07(2) . . ? N4 Li1 N2 115.2(16) . . ? N4 Li1 N1 106.3(14) . . ? N2 Li1 N1 110.9(14) . . ? N4 Li1 N3 108.7(15) . . ? N2 Li1 N3 103.2(13) . . ? N1 Li1 N3 112.7(16) . . ? N6 Li2 N5 110.7(14) . . ? N6 Li2 N8 106.9(13) . . ? N5 Li2 N8 111.1(16) . . ? N6 Li2 N7 121.2(16) . . ? N5 Li2 N7 104.9(13) . . ? N8 Li2 N7 101.6(13) . . ? N12 Li3 N10 107.2(14) . . ? N12 Li3 N9 106.2(15) . . ? N10 Li3 N9 114.5(13) . . ? N12 Li3 N11 101.8(12) . . ? N10 Li3 N11 113.4(15) . . ? N9 Li3 N11 112.5(15) . . ? N16 Li4 N15 119.3(13) . . ? N16 Li4 N13 110.6(12) . . ? N15 Li4 N13 115.5(13) . . ? N16 Li4 N14 109.0(12) . . ? N15 Li4 N14 95.6(11) . . ? N13 Li4 N14 104.5(13) . . ? 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 Pb6 Pb3 Pb8 Pb1 -1.46(2) . . . . ? Pb4 Pb1 Pb5 Pb9 26.91(2) . . . . ? Pb2 Pb9 Pb7 Pb3 27.30(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.79 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.288 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.324