data_jfe64 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Ge8 N8 Pb8' _chemical_formula_weight 2674.85 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' 'Ge' 'Ge' 0.1547 1.8001 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 18.2282(14) _cell_length_b 18.2282(14) _cell_length_c 18.2282(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6056.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4592 _exptl_absorpt_coefficient_mu 26.067 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0367 _exptl_absorpt_correction_T_max 0.1474 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 36464 _diffrn_reflns_av_R_equivalents 0.2330 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.68 _reflns_number_total 2561 _reflns_number_gt 1359 _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^)+(0.0999P)^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 SHELXL _refine_ls_extinction_coef 0.00010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 2561 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.006 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 -0.06725(4) -0.06725(4) -1.06725(4) 0.0355(4) Uani 1 3 d S . . Pb2 Pb -0.06738(4) -0.18229(4) -0.56655(4) 0.0335(2) Uani 1 1 d . . . Ge1 Ge -0.11625(19) -0.11625(19) -0.88375(19) 0.050(2) Uani 1 3 d S . . Ge2 Ge 0.11789(15) -0.13777(15) -0.61886(17) 0.0446(8) Uani 1 1 d . . . N1 N -0.0585(9) -0.0585(9) -0.9415(9) 0.048(9) Uani 1 3 d S . . N2 N 0.0552(8) -0.1928(9) -0.5581(8) 0.030(3) Uani 1 1 d . . . C1 C -0.1172(15) -0.0861(17) -0.7802(16) 0.103(13) Uani 1 1 d . . . H1A H -0.1323 -0.1263 -0.7505 0.154 Uiso 1 1 calc R . . H1B H -0.1504 -0.0464 -0.7739 0.154 Uiso 1 1 calc R . . H1C H -0.0693 -0.0711 -0.7660 0.154 Uiso 1 1 calc R . . C2 C 0.173(6) -0.213(6) -0.713(6) 0.05(3) Uiso 0.20 1 d P . . C2A C 0.1031(19) -0.1682(19) -0.7198(19) 0.064(9) Uiso 0.80 1 d P . . C3 C 0.2128(18) -0.1867(19) -0.6205(17) 0.063(10) Uiso 0.80 1 d P . . C3A C 0.177(8) -0.263(8) -0.652(9) 0.09(5) Uiso 0.20 1 d P . . C4 C 0.123(3) -0.036(3) -0.588(3) 0.048(12) Uiso 0.50 1 d P . . C4A C 0.077(3) -0.034(3) -0.619(2) 0.050(12) Uiso 0.50 1 d P . . 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 0.0355(4) 0.0355(4) 0.0355(4) -0.0035(3) -0.0035(3) -0.0035(3) Pb2 0.0351(4) 0.0299(4) 0.0355(4) 0.0027(3) -0.0060(3) 0.0032(3) Ge1 0.050(2) 0.050(2) 0.050(2) 0.0102(13) 0.0102(13) -0.0102(13) Ge2 0.0448(14) 0.0443(11) 0.045(2) 0.0165(15) 0.0061(13) -0.0116(13) N1 0.048(9) 0.048(9) 0.048(9) 0.009(9) 0.009(9) -0.009(9) N2 0.029(8) 0.029(8) 0.032(9) -0.006(7) -0.011(7) 0.013(6) C1 0.08(2) 0.14(3) 0.09(3) 0.06(2) 0.029(18) 0.00(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N1 2.303(14) 4_553 ? Pb1 N1 2.303(14) . ? Pb1 N1 2.303(14) 3_553 ? Pb1 Pb1 3.467(2) 2 ? Pb1 Pb1 3.467(2) 4_553 ? Pb1 Pb1 3.467(2) 3_553 ? Pb2 N2 2.247(15) . ? Pb2 N2 2.291(15) 3_554 ? Pb2 N2 2.293(16) 22_544 ? Pb2 C3A 2.73(15) 22_544 ? Pb2 Pb2 3.4525(15) 3_554 ? Pb2 Pb2 3.4719(13) 24_444 ? Pb2 Pb2 3.4719(13) 22_544 ? Ge1 N1 1.82(3) . ? Ge1 C1 1.97(3) 8_454 ? Ge1 C1 1.97(3) . ? Ge1 C1 1.97(3) 11_544 ? Ge2 N2 1.88(2) . ? Ge2 C2A 1.94(3) . ? Ge2 C4 1.95(5) . ? Ge2 C3 1.95(3) . ? Ge2 C4A 2.04(5) . ? Ge2 C2 2.41(10) . ? N1 Pb1 2.303(14) 4_553 ? N1 Pb1 2.303(14) 3_553 ? N2 Pb2 2.291(15) 3_554 ? N2 Pb2 2.293(16) 24_444 ? C2 C3A 1.45(16) . ? C2 C2A 1.51(10) . ? C2 C3 1.91(12) . ? C3 C3A 1.64(16) . ? C3A Pb2 2.73(15) 24_444 ? C4 C4A 1.02(6) . ? 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 N1 Pb1 N1 81.8(9) 4_553 . ? N1 Pb1 N1 81.8(9) 4_553 3_553 ? N1 Pb1 N1 81.8(9) . 3_553 ? N1 Pb1 Pb1 41.2(4) 4_553 2 ? N1 Pb1 Pb1 84.4(6) . 2 ? N1 Pb1 Pb1 41.2(4) 3_553 2 ? N1 Pb1 Pb1 41.2(4) 4_553 4_553 ? N1 Pb1 Pb1 41.2(4) . 4_553 ? N1 Pb1 Pb1 84.4(6) 3_553 4_553 ? Pb1 Pb1 Pb1 60.0 2 4_553 ? N1 Pb1 Pb1 84.4(6) 4_553 3_553 ? N1 Pb1 Pb1 41.2(4) . 3_553 ? N1 Pb1 Pb1 41.2(4) 3_553 3_553 ? Pb1 Pb1 Pb1 60.0 2 3_553 ? Pb1 Pb1 Pb1 60.0 4_553 3_553 ? N2 Pb2 N2 80.1(7) . 3_554 ? N2 Pb2 N2 80.5(7) . 22_544 ? N2 Pb2 N2 79.6(7) 3_554 22_544 ? N2 Pb2 C3A 126(3) . 22_544 ? N2 Pb2 C3A 139(3) 3_554 22_544 ? N2 Pb2 C3A 75(3) 22_544 22_544 ? N2 Pb2 Pb2 40.9(4) . 3_554 ? N2 Pb2 Pb2 40.0(4) 3_554 3_554 ? N2 Pb2 Pb2 83.3(4) 22_544 3_554 ? C3A Pb2 Pb2 157(3) 22_544 3_554 ? N2 Pb2 Pb2 40.6(4) . 24_444 ? N2 Pb2 Pb2 82.9(5) 3_554 24_444 ? N2 Pb2 Pb2 40.7(4) 22_544 24_444 ? C3A Pb2 Pb2 98(3) 22_544 24_444 ? Pb2 Pb2 Pb2 60.185(12) 3_554 24_444 ? N2 Pb2 Pb2 83.5(5) . 22_544 ? N2 Pb2 Pb2 40.8(4) 3_554 22_544 ? N2 Pb2 Pb2 39.6(4) 22_544 22_544 ? C3A Pb2 Pb2 105(3) 22_544 22_544 ? Pb2 Pb2 Pb2 60.185(12) 3_554 22_544 ? Pb2 Pb2 Pb2 59.63(2) 24_444 22_544 ? N1 Ge1 C1 113.5(9) . 8_454 ? N1 Ge1 C1 113.5(9) . . ? C1 Ge1 C1 105.2(10) 8_454 . ? N1 Ge1 C1 113.5(9) . 11_544 ? C1 Ge1 C1 105.2(10) 8_454 11_544 ? C1 Ge1 C1 105.2(10) . 11_544 ? N2 Ge2 C2A 108.7(12) . . ? N2 Ge2 C4 111.6(15) . . ? C2A Ge2 C4 123.8(18) . . ? N2 Ge2 C3 107.8(10) . . ? C2A Ge2 C3 88.8(13) . . ? C4 Ge2 C3 113.4(17) . . ? N2 Ge2 C4A 105.9(14) . . ? C2A Ge2 C4A 102.2(15) . . ? C4 Ge2 C4A 29.7(17) . . ? C3 Ge2 C4A 138.8(19) . . ? N2 Ge2 C2 112(3) . . ? C2A Ge2 C2 39(3) . . ? C4 Ge2 C2 137(3) . . ? C3 Ge2 C2 50(3) . . ? C4A Ge2 C2 132(3) . . ? Ge1 N1 Pb1 119.6(6) . 4_553 ? Ge1 N1 Pb1 119.6(6) . . ? Pb1 N1 Pb1 97.7(8) 4_553 . ? Ge1 N1 Pb1 119.6(6) . 3_553 ? Pb1 N1 Pb1 97.7(8) 4_553 3_553 ? Pb1 N1 Pb1 97.7(8) . 3_553 ? Ge2 N2 Pb2 121.2(7) . . ? Ge2 N2 Pb2 118.7(8) . 3_554 ? Pb2 N2 Pb2 99.1(6) . 3_554 ? Ge2 N2 Pb2 115.5(7) . 24_444 ? Pb2 N2 Pb2 99.8(7) . 24_444 ? Pb2 N2 Pb2 98.5(6) 3_554 24_444 ? C3A C2 C2A 117(10) . . ? C3A C2 C3 57(8) . . ? C2A C2 C3 105(6) . . ? C3A C2 Ge2 80(8) . . ? C2A C2 Ge2 53(3) . . ? C3 C2 Ge2 52(3) . . ? C2 C2A Ge2 88(5) . . ? C3A C3 C2 47(6) . . ? C3A C3 Ge2 92(6) . . ? C2 C3 Ge2 78(3) . . ? C2 C3A C3 76(8) . . ? C2 C3A Pb2 129(10) . 24_444 ? C3 C3A Pb2 114(8) . 24_444 ? C4A C4 Ge2 80(5) . . ? C4 C4A Ge2 70(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.859 _refine_diff_density_min -2.406 _refine_diff_density_rms 0.368