# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andreas Schnepf' _publ_contact_author_email SCHNEPF@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; [Si(SiMe3)3]6Ge18M (M = Zn, Cd, Hg): Neutral metalloid cluster compounds of germanium as highly soluble building blocks for a supramolecular chemistry. ; loop_ _publ_author_name 'Andreas Schnepf' 'Florian Henke' 'Christian Schenk' # Attachment 'Hg_Ge18.cif' data_fhp25mon _database_code_depnum_ccdc_archive 'CCDC 725133' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H186 Ge18 Hg Si24' _chemical_formula_weight 3137.50 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' Si Si 0.0817 0.0704 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.953(3) _cell_length_b 19.069(4) _cell_length_c 23.622(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.29(3) _cell_angle_gamma 90.00 _cell_volume 6730(2) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 38706 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 26.09 _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3124 _exptl_absorpt_coefficient_mu 5.329 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1353 _exptl_absorpt_correction_T_max 0.7165 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(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 45929 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.66 _reflns_number_total 12651 _reflns_number_gt 9654 _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^)+(0.0486P)^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 12651 _refine_ls_number_parameters 529 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Hg1 Hg 0.0000 0.5000 0.0000 0.03178(8) Uani 1 2 d S . . Ge1 Ge 0.04889(4) 0.60328(3) -0.16100(3) 0.03266(14) Uani 1 1 d . . . Ge2 Ge -0.15072(4) 0.66739(3) -0.08932(3) 0.03502(15) Uani 1 1 d . . . Ge3 Ge 0.07246(4) 0.71812(3) -0.03654(3) 0.03306(14) Uani 1 1 d . . . Ge4 Ge -0.05160(4) 0.64261(3) -0.00390(3) 0.03024(14) Uani 1 1 d . . . Ge5 Ge 0.10943(4) 0.59451(3) -0.06111(2) 0.02936(13) Uani 1 1 d . . . Ge6 Ge -0.07580(4) 0.55262(3) -0.10652(3) 0.03096(14) Uani 1 1 d . . . Ge7 Ge -0.05437(4) 0.77863(3) -0.09465(3) 0.03426(15) Uani 1 1 d . . . Ge8 Ge 0.08747(4) 0.73292(3) -0.14399(3) 0.03277(14) Uani 1 1 d . . . Ge9 Ge -0.07439(4) 0.69398(3) -0.18238(3) 0.03345(14) Uani 1 1 d . . . Si1 Si 0.11598(10) 0.54639(8) -0.23848(6) 0.0277(3) Uani 1 1 d . . . Si2 Si -0.30619(11) 0.68857(8) -0.07868(7) 0.0312(3) Uani 1 1 d . A . Si3 Si 0.15510(11) 0.79012(8) 0.02913(6) 0.0289(3) Uani 1 1 d . . . Si10 Si 0.02410(14) 0.57017(10) -0.31967(7) 0.0451(4) Uani 1 1 d . . . Si11 Si 0.26132(13) 0.59238(10) -0.24277(9) 0.0444(5) Uani 1 1 d . . . Si12 Si 0.11773(12) 0.42546(8) -0.22035(7) 0.0350(4) Uani 1 1 d . . . Si20 Si -0.36936(12) 0.58601(10) -0.04269(8) 0.0407(4) Uani 1 1 d . . . Si21 Si -0.36989(12) 0.71550(10) -0.16821(8) 0.0414(4) Uani 1 1 d . . . Si22 Si -0.31804(12) 0.78458(10) -0.01649(8) 0.0426(4) Uani 1 1 d . . . Si30 Si 0.05307(13) 0.85553(9) 0.08094(8) 0.0405(4) Uani 1 1 d . . . Si31 Si 0.24807(12) 0.86111(9) -0.02480(8) 0.0382(4) Uani 1 1 d . . . Si32 Si 0.24095(12) 0.71798(9) 0.09055(7) 0.0357(4) Uani 1 1 d . . . C10C C -0.0951(6) 0.5455(5) -0.3070(4) 0.067(2) Uani 1 1 d . . . H10A H -0.1325 0.5557 -0.3411 0.101 Uiso 1 1 calc R . . H10B H -0.1167 0.5727 -0.2751 0.101 Uiso 1 1 calc R . . H10C H -0.0984 0.4954 -0.2983 0.101 Uiso 1 1 calc R . . C10B C 0.0294(6) 0.6656(4) -0.3380(3) 0.063(2) Uani 1 1 d . . . H10D H -0.0091 0.6748 -0.3718 0.094 Uiso 1 1 calc R . . H10E H 0.0913 0.6784 -0.3457 0.094 Uiso 1 1 calc R . . H10F H 0.0088 0.6935 -0.3062 0.094 Uiso 1 1 calc R . . C10A C 0.0643(8) 0.5190(6) -0.3812(4) 0.093(4) Uani 1 1 d . . . H10G H 0.0260 0.5289 -0.4148 0.140 Uiso 1 1 calc R . . H10H H 0.0620 0.4688 -0.3725 0.140 Uiso 1 1 calc R . . H10I H 0.1261 0.5325 -0.3884 0.140 Uiso 1 1 calc R . . C11C C 0.2609(6) 0.6879(4) -0.2615(4) 0.072(3) Uani 1 1 d . . . H11A H 0.3227 0.7048 -0.2628 0.107 Uiso 1 1 calc R . . H11B H 0.2294 0.7143 -0.2328 0.107 Uiso 1 1 calc R . . H11C H 0.2306 0.6945 -0.2986 0.107 Uiso 1 1 calc R . . C11B C 0.3249(6) 0.5474(5) -0.2992(5) 0.088(4) Uani 1 1 d . . . H11D H 0.3852 0.5673 -0.3003 0.133 Uiso 1 1 calc R . . H11E H 0.2936 0.5542 -0.3361 0.133 Uiso 1 1 calc R . . H11F H 0.3290 0.4971 -0.2909 0.133 Uiso 1 1 calc R . . C11A C 0.3203(6) 0.5800(7) -0.1731(4) 0.096(4) Uani 1 1 d . . . H11G H 0.3811 0.5990 -0.1744 0.143 Uiso 1 1 calc R . . H11H H 0.3233 0.5299 -0.1640 0.143 Uiso 1 1 calc R . . H11I H 0.2877 0.6047 -0.1439 0.143 Uiso 1 1 calc R . . C12C C 0.1875(6) 0.3802(4) -0.2731(3) 0.063(2) Uani 1 1 d . . . H12A H 0.1881 0.3297 -0.2655 0.094 Uiso 1 1 calc R . . H12B H 0.2487 0.3985 -0.2701 0.094 Uiso 1 1 calc R . . H12C H 0.1622 0.3888 -0.3114 0.094 Uiso 1 1 calc R . . C12B C 0.0008(5) 0.3904(4) -0.2277(4) 0.060(2) Uani 1 1 d . . . H12D H 0.0013 0.3399 -0.2202 0.090 Uiso 1 1 calc R . . H12E H -0.0233 0.3990 -0.2663 0.090 Uiso 1 1 calc R . . H12F H -0.0368 0.4140 -0.2005 0.090 Uiso 1 1 calc R . . C12A C 0.1634(7) 0.4069(4) -0.1480(3) 0.070(2) Uani 1 1 d . . . H12G H 0.1635 0.3562 -0.1414 0.104 Uiso 1 1 calc R . . H12H H 0.1262 0.4299 -0.1203 0.104 Uiso 1 1 calc R . . H12I H 0.2248 0.4248 -0.1439 0.104 Uiso 1 1 calc R . . C20A C -0.3697(19) 0.5119(16) -0.0965(11) 0.081(9) Uani 0.50 1 d PU A 1 H20A H -0.3967 0.4700 -0.0802 0.122 Uiso 0.50 1 calc PR A 1 H20B H -0.3081 0.5014 -0.1064 0.122 Uiso 0.50 1 calc PR A 1 H20C H -0.4046 0.5260 -0.1307 0.122 Uiso 0.50 1 calc PR A 1 C20B C -0.308(2) 0.5522(19) 0.0198(18) 0.074(8) Uani 0.50 1 d PU A 1 H20D H -0.3368 0.5095 0.0330 0.110 Uiso 0.50 1 calc PR A 1 H20E H -0.3070 0.5876 0.0499 0.110 Uiso 0.50 1 calc PR A 1 H20F H -0.2461 0.5414 0.0101 0.110 Uiso 0.50 1 calc PR A 1 C20C C -0.485(3) 0.603(3) -0.0235(17) 0.097(16) Uani 0.50 1 d PU A 1 H20G H -0.5108 0.5595 -0.0085 0.145 Uiso 0.50 1 calc PR A 1 H20H H -0.5204 0.6178 -0.0571 0.145 Uiso 0.50 1 calc PR A 1 H20I H -0.4858 0.6394 0.0055 0.145 Uiso 0.50 1 calc PR A 1 C20F C -0.490(2) 0.591(3) -0.0488(16) 0.077(13) Uani 0.50 1 d PU A 2 H20J H -0.5162 0.5484 -0.0336 0.116 Uiso 0.50 1 calc PR A 2 H20K H -0.5093 0.5967 -0.0887 0.116 Uiso 0.50 1 calc PR A 2 H20L H -0.5106 0.6318 -0.0272 0.116 Uiso 0.50 1 calc PR A 2 C20E C -0.325(4) 0.576(2) 0.033(2) 0.17(2) Uani 0.50 1 d PU A 2 H20M H -0.3495 0.5340 0.0494 0.250 Uiso 0.50 1 calc PR A 2 H20N H -0.3417 0.6174 0.0548 0.250 Uiso 0.50 1 calc PR A 2 H20O H -0.2591 0.5727 0.0331 0.250 Uiso 0.50 1 calc PR A 2 C20D C -0.330(2) 0.5142(17) -0.084(2) 0.135(16) Uani 0.50 1 d PU A 2 H20P H -0.3546 0.4702 -0.0708 0.203 Uiso 0.50 1 calc PR A 2 H20Q H -0.2641 0.5123 -0.0808 0.203 Uiso 0.50 1 calc PR A 2 H20R H -0.3482 0.5213 -0.1242 0.203 Uiso 0.50 1 calc PR A 2 C21C C -0.3109(5) 0.7898(4) -0.2009(3) 0.0543(19) Uani 1 1 d . A . H21A H -0.3388 0.8000 -0.2382 0.082 Uiso 1 1 calc R . . H21B H -0.2479 0.7774 -0.2051 0.082 Uiso 1 1 calc R . . H21C H -0.3147 0.8313 -0.1766 0.082 Uiso 1 1 calc R . . C21B C -0.3656(9) 0.6377(5) -0.2158(4) 0.091(4) Uani 1 1 d . A . H21D H -0.3924 0.6497 -0.2530 0.137 Uiso 1 1 calc R . . H21E H -0.3989 0.5989 -0.1994 0.137 Uiso 1 1 calc R . . H21F H -0.3031 0.6237 -0.2198 0.137 Uiso 1 1 calc R . . C21A C -0.4888(5) 0.7429(5) -0.1604(4) 0.072(3) Uani 1 1 d . A . H21G H -0.5159 0.7543 -0.1977 0.108 Uiso 1 1 calc R . . H21H H -0.4906 0.7843 -0.1358 0.108 Uiso 1 1 calc R . . H21I H -0.5221 0.7045 -0.1435 0.108 Uiso 1 1 calc R . . C22C C -0.2481(6) 0.7688(5) 0.0499(3) 0.062(2) Uani 1 1 d . A . H22A H -0.2535 0.8090 0.0754 0.093 Uiso 1 1 calc R . . H22B H -0.1854 0.7630 0.0404 0.093 Uiso 1 1 calc R . . H22C H -0.2689 0.7263 0.0686 0.093 Uiso 1 1 calc R . . C22B C -0.2833(6) 0.8691(4) -0.0490(4) 0.068(2) Uani 1 1 d . A . H22D H -0.2894 0.9072 -0.0216 0.101 Uiso 1 1 calc R . . H22E H -0.3215 0.8787 -0.0828 0.101 Uiso 1 1 calc R . . H22F H -0.2208 0.8657 -0.0597 0.101 Uiso 1 1 calc R . . C22A C -0.4382(5) 0.7958(5) 0.0027(4) 0.078(3) Uani 1 1 d . A . H22G H -0.4431 0.8357 0.0285 0.117 Uiso 1 1 calc R . . H22H H -0.4588 0.7531 0.0212 0.117 Uiso 1 1 calc R . . H22I H -0.4753 0.8044 -0.0318 0.117 Uiso 1 1 calc R . . C30C C -0.0355(5) 0.8965(4) 0.0346(3) 0.059(2) Uani 1 1 d . . . H30A H -0.0763 0.9232 0.0579 0.088 Uiso 1 1 calc R . . H30B H -0.0690 0.8599 0.0138 0.088 Uiso 1 1 calc R . . H30C H -0.0079 0.9282 0.0077 0.088 Uiso 1 1 calc R . . C30B C -0.0003(5) 0.7958(4) 0.1332(3) 0.0535(19) Uani 1 1 d . . . H30D H -0.0430 0.8225 0.1550 0.080 Uiso 1 1 calc R . . H30E H 0.0460 0.7759 0.1589 0.080 Uiso 1 1 calc R . . H30F H -0.0318 0.7578 0.1128 0.080 Uiso 1 1 calc R . . C30A C 0.1134(6) 0.9278(4) 0.1194(4) 0.064(2) Uani 1 1 d . . . H30G H 0.0708 0.9550 0.1410 0.097 Uiso 1 1 calc R . . H30H H 0.1416 0.9585 0.0920 0.097 Uiso 1 1 calc R . . H30I H 0.1594 0.9079 0.1454 0.097 Uiso 1 1 calc R . . C31C C 0.3133(5) 0.8064(4) -0.0738(3) 0.0504(18) Uani 1 1 d . . . H31A H 0.3517 0.8367 -0.0959 0.076 Uiso 1 1 calc R . . H31B H 0.2720 0.7807 -0.0995 0.076 Uiso 1 1 calc R . . H31C H 0.3504 0.7731 -0.0518 0.076 Uiso 1 1 calc R . . C31B C 0.1787(6) 0.9251(4) -0.0674(4) 0.063(2) Uani 1 1 d . . . H31D H 0.2178 0.9545 -0.0898 0.094 Uiso 1 1 calc R . . H31E H 0.1450 0.9548 -0.0419 0.094 Uiso 1 1 calc R . . H31F H 0.1369 0.8996 -0.0929 0.094 Uiso 1 1 calc R . . C31A C 0.3291(6) 0.9093(4) 0.0239(3) 0.061(2) Uani 1 1 d . . . H31G H 0.3679 0.9389 0.0015 0.092 Uiso 1 1 calc R . . H31H H 0.3656 0.8754 0.0458 0.092 Uiso 1 1 calc R . . H31I H 0.2959 0.9387 0.0498 0.092 Uiso 1 1 calc R . . C32C C 0.1738(5) 0.6408(4) 0.1126(3) 0.0509(17) Uani 1 1 d . . . H32A H 0.2105 0.6112 0.1382 0.076 Uiso 1 1 calc R . . H32B H 0.1547 0.6137 0.0790 0.076 Uiso 1 1 calc R . . H32C H 0.1211 0.6571 0.1321 0.076 Uiso 1 1 calc R . . C32B C 0.3419(5) 0.6867(4) 0.0550(3) 0.0551(19) Uani 1 1 d . . . H32D H 0.3773 0.6566 0.0810 0.083 Uiso 1 1 calc R . . H32E H 0.3781 0.7270 0.0442 0.083 Uiso 1 1 calc R . . H32F H 0.3237 0.6599 0.0211 0.083 Uiso 1 1 calc R . . C32A C 0.2771(6) 0.7699(4) 0.1544(3) 0.0588(19) Uani 1 1 d . . . H32G H 0.3131 0.7402 0.1803 0.088 Uiso 1 1 calc R . . H32H H 0.2243 0.7867 0.1735 0.088 Uiso 1 1 calc R . . H32I H 0.3130 0.8100 0.1428 0.088 Uiso 1 1 calc R . . C100 C -0.1883(9) 0.9455(6) -0.2363(6) 0.113(4) Uani 1 1 d . . . H10J H -0.2153 0.9525 -0.1996 0.169 Uiso 1 1 calc R B 1 H10K H -0.2254 0.9132 -0.2594 0.169 Uiso 1 1 calc R B 1 H10L H -0.1844 0.9907 -0.2559 0.169 Uiso 1 1 calc R B 1 C104 C 0.0673(11) 0.8675(9) -0.3344(8) 0.154(7) Uani 1 1 d . . . H10S H 0.1091 0.8282 -0.3375 0.231 Uiso 1 1 calc R . . H10T H 0.0975 0.9113 -0.3442 0.231 Uiso 1 1 calc R . . H10U H 0.0155 0.8602 -0.3604 0.231 Uiso 1 1 calc R . . C103 C 0.0373(13) 0.8719(9) -0.2758(9) 0.148(6) Uani 1 1 d . . . H10M H 0.0334 0.8247 -0.2586 0.178 Uiso 1 1 calc R C 1 H10N H 0.0785 0.9012 -0.2520 0.178 Uiso 1 1 calc R C 1 C101 C -0.099(2) 0.9162(15) -0.2275(13) 0.100(9) Uani 0.50 1 d P D 1 H10O H -0.1038 0.8709 -0.2074 0.121 Uiso 0.50 1 calc PR D 1 H10P H -0.0630 0.9483 -0.2030 0.121 Uiso 0.50 1 calc PR D 1 C102 C -0.051(2) 0.9045(18) -0.2820(14) 0.110(10) Uani 0.50 1 d P D 1 H10Q H -0.0896 0.8746 -0.3072 0.132 Uiso 0.50 1 calc PR D 1 H10R H -0.0448 0.9503 -0.3011 0.132 Uiso 0.50 1 calc PR D 1 C112 C -0.026(2) 0.9200(16) -0.2445(18) 0.112(10) Uani 0.50 1 d P D 2 H11J H -0.0176 0.9136 -0.2031 0.134 Uiso 0.50 1 calc PR D 2 H11K H -0.0140 0.9697 -0.2538 0.134 Uiso 0.50 1 calc PR D 2 C111 C -0.1185(18) 0.8993(13) -0.2643(16) 0.102(8) Uani 0.50 1 d P D 2 H11L H -0.1290 0.8496 -0.2547 0.122 Uiso 0.50 1 calc PR D 2 H11M H -0.1248 0.9043 -0.3060 0.122 Uiso 0.50 1 calc PR D 2 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 Hg1 0.03770(18) 0.02646(14) 0.03112(16) 0.00624(13) 0.00079(14) 0.00137(13) Ge1 0.0396(3) 0.0296(3) 0.0290(3) -0.0010(2) 0.0041(3) 0.0048(3) Ge2 0.0304(3) 0.0371(3) 0.0376(3) 0.0053(3) 0.0024(3) 0.0053(3) Ge3 0.0392(3) 0.0283(3) 0.0314(3) -0.0002(2) -0.0021(3) -0.0020(3) Ge4 0.0324(3) 0.0302(3) 0.0283(3) 0.0015(2) 0.0027(3) 0.0023(2) Ge5 0.0323(3) 0.0271(3) 0.0287(3) 0.0009(2) 0.0013(3) 0.0034(2) Ge6 0.0338(3) 0.0283(3) 0.0307(3) 0.0007(2) 0.0005(3) -0.0004(2) Ge7 0.0388(3) 0.0270(3) 0.0370(3) -0.0006(2) 0.0016(3) 0.0070(3) Ge8 0.0370(3) 0.0306(3) 0.0311(3) 0.0010(2) 0.0062(3) -0.0023(3) Ge9 0.0360(3) 0.0367(3) 0.0275(3) 0.0027(2) -0.0010(3) 0.0063(3) Si1 0.0330(8) 0.0251(7) 0.0251(7) -0.0002(6) 0.0013(7) -0.0002(6) Si2 0.0287(8) 0.0343(8) 0.0304(8) 0.0026(6) 0.0001(7) 0.0038(7) Si3 0.0319(8) 0.0265(7) 0.0282(7) -0.0021(6) 0.0021(7) -0.0013(6) Si10 0.0574(12) 0.0487(10) 0.0288(8) -0.0005(8) -0.0049(9) 0.0145(9) Si11 0.0410(10) 0.0397(9) 0.0533(11) -0.0090(8) 0.0127(9) -0.0085(8) Si12 0.0462(10) 0.0273(8) 0.0315(8) 0.0007(6) 0.0009(8) 0.0013(7) Si20 0.0335(9) 0.0419(9) 0.0464(10) 0.0120(8) -0.0021(8) -0.0013(7) Si21 0.0414(10) 0.0449(10) 0.0374(9) 0.0085(8) -0.0054(8) 0.0033(8) Si22 0.0348(9) 0.0472(10) 0.0458(10) -0.0117(8) 0.0021(8) 0.0072(8) Si30 0.0481(10) 0.0349(8) 0.0391(9) -0.0100(7) 0.0064(9) 0.0029(8) Si31 0.0409(9) 0.0350(8) 0.0388(9) 0.0075(7) 0.0039(8) -0.0059(7) Si32 0.0363(9) 0.0367(9) 0.0339(8) 0.0064(7) -0.0015(8) -0.0043(7) C10C 0.063(5) 0.059(5) 0.076(6) 0.005(4) -0.037(5) 0.000(4) C10B 0.074(5) 0.070(5) 0.044(4) 0.022(4) 0.002(4) 0.010(4) C10A 0.126(9) 0.109(8) 0.043(4) -0.016(5) -0.019(5) 0.062(7) C11C 0.065(5) 0.042(4) 0.110(7) -0.014(4) 0.033(5) -0.025(4) C11B 0.077(6) 0.065(5) 0.128(9) -0.039(6) 0.059(7) -0.024(5) C11A 0.055(5) 0.147(10) 0.083(7) 0.017(7) -0.025(5) -0.042(6) C12C 0.093(6) 0.031(3) 0.066(5) -0.003(3) 0.030(5) 0.010(4) C12B 0.059(5) 0.042(4) 0.079(6) 0.005(4) 0.000(4) -0.015(3) C12A 0.101(7) 0.051(4) 0.056(5) 0.007(4) -0.011(5) 0.020(5) C20A 0.11(2) 0.056(12) 0.086(14) -0.028(10) 0.044(15) -0.056(16) C20B 0.070(12) 0.071(17) 0.076(17) 0.022(12) -0.042(11) -0.029(11) C20C 0.07(2) 0.08(2) 0.15(4) 0.05(3) 0.06(3) 0.021(18) C20F 0.028(11) 0.08(2) 0.13(3) 0.06(2) -0.020(18) -0.015(13) C20E 0.26(5) 0.14(4) 0.10(3) 0.08(3) -0.09(3) -0.13(3) C20D 0.08(2) 0.042(12) 0.29(4) 0.004(18) 0.08(2) -0.038(14) C21C 0.049(4) 0.061(5) 0.054(4) 0.024(4) 0.008(4) 0.009(4) C21B 0.169(11) 0.057(5) 0.045(4) -0.009(4) -0.026(6) 0.001(6) C21A 0.037(4) 0.097(7) 0.082(6) 0.043(5) -0.005(4) -0.003(4) C22C 0.064(5) 0.073(5) 0.048(4) -0.020(4) -0.007(4) 0.003(4) C22B 0.083(6) 0.050(4) 0.071(5) -0.010(4) 0.008(5) 0.011(4) C22A 0.046(4) 0.103(7) 0.086(6) -0.045(6) 0.011(5) 0.014(5) C30C 0.068(5) 0.045(4) 0.065(5) -0.015(4) 0.004(4) 0.024(4) C30B 0.059(4) 0.054(4) 0.049(4) -0.007(3) 0.020(4) 0.002(4) C30A 0.083(6) 0.054(4) 0.056(5) -0.024(4) 0.002(5) -0.003(4) C31C 0.042(4) 0.063(4) 0.047(4) 0.008(3) 0.012(3) 0.000(3) C31B 0.070(5) 0.049(4) 0.071(5) 0.033(4) 0.012(5) 0.003(4) C31A 0.062(5) 0.061(5) 0.061(5) -0.003(4) 0.002(4) -0.029(4) C32C 0.054(4) 0.043(4) 0.055(4) 0.014(3) -0.003(4) -0.004(3) C32B 0.049(4) 0.056(4) 0.061(5) 0.018(4) 0.009(4) 0.010(3) C32A 0.062(5) 0.062(5) 0.051(4) 0.005(4) -0.016(4) -0.009(4) C100 0.136(11) 0.066(7) 0.137(11) -0.010(7) 0.012(10) -0.033(7) C104 0.139(14) 0.150(15) 0.170(17) 0.034(13) -0.029(13) -0.063(11) C103 0.157(16) 0.111(12) 0.175(18) 0.046(12) -0.020(15) 0.007(11) C101 0.12(2) 0.075(15) 0.11(2) -0.031(14) -0.05(2) 0.026(16) C102 0.073(17) 0.14(2) 0.12(2) 0.05(2) -0.036(18) -0.048(17) C112 0.10(2) 0.097(19) 0.13(3) -0.002(18) -0.06(2) -0.016(18) C111 0.10(2) 0.079(15) 0.12(2) 0.003(15) -0.026(19) -0.055(15) _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 Hg1 Ge4 2.8273(8) 3_565 ? Hg1 Ge4 2.8273(8) . ? Hg1 Ge5 2.8633(8) 3_565 ? Hg1 Ge5 2.8633(8) . ? Hg1 Ge6 2.8974(9) 3_565 ? Hg1 Ge6 2.8974(9) . ? Ge1 Si1 2.3834(16) . ? Ge1 Ge5 2.4988(11) . ? Ge1 Ge6 2.5016(10) . ? Ge1 Ge9 2.5633(10) . ? Ge1 Ge8 2.5666(10) . ? Ge2 Si2 2.3827(17) . ? Ge2 Ge6 2.4993(9) . ? Ge2 Ge4 2.5005(12) . ? Ge2 Ge9 2.5676(10) . ? Ge2 Ge7 2.5700(10) . ? Ge3 Si3 2.3802(18) . ? Ge3 Ge4 2.4947(9) . ? Ge3 Ge5 2.4949(9) . ? Ge3 Ge7 2.5698(11) . ? Ge3 Ge8 2.5725(10) . ? Ge7 Ge8 2.6105(10) . ? Ge7 Ge9 2.6344(10) . ? Ge8 Ge9 2.6564(11) . ? Si1 Si12 2.345(2) . ? Si1 Si11 2.350(2) . ? Si1 Si10 2.358(3) . ? Si2 Si21 2.342(3) . ? Si2 Si20 2.346(2) . ? Si2 Si22 2.358(2) . ? Si3 Si32 2.345(2) . ? Si3 Si30 2.352(2) . ? Si3 Si31 2.352(2) . ? Si10 C10A 1.870(8) . ? Si10 C10B 1.873(8) . ? Si10 C10C 1.879(9) . ? Si11 C11A 1.851(10) . ? Si11 C11C 1.874(8) . ? Si11 C11B 1.876(8) . ? Si12 C12A 1.850(9) . ? Si12 C12C 1.867(7) . ? Si12 C12B 1.873(8) . ? Si20 C20D 1.80(4) . ? Si20 C20F 1.81(4) . ? Si20 C20B 1.83(4) . ? Si20 C20C 1.83(4) . ? Si20 C20E 1.89(5) . ? Si20 C20A 1.90(2) . ? Si21 C21C 1.854(7) . ? Si21 C21B 1.863(9) . ? Si21 C21A 1.869(8) . ? Si22 C22B 1.868(9) . ? Si22 C22C 1.873(9) . ? Si22 C22A 1.883(7) . ? Si30 C30C 1.856(8) . ? Si30 C30A 1.863(8) . ? Si30 C30B 1.881(7) . ? Si31 C31C 1.862(7) . ? Si31 C31B 1.870(8) . ? Si31 C31A 1.877(8) . ? Si32 C32B 1.855(7) . ? Si32 C32A 1.865(8) . ? Si32 C32C 1.867(7) . ? C100 C101 1.45(3) . ? C100 C111 1.54(4) . ? C104 C103 1.48(2) . ? C103 C102 1.47(3) . ? C103 C112 1.53(4) . ? C101 C102 1.51(4) . ? C112 C111 1.50(4) . ? 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 Ge4 Hg1 Ge4 180.0 3_565 . ? Ge4 Hg1 Ge5 62.54(2) 3_565 3_565 ? Ge4 Hg1 Ge5 117.46(2) . 3_565 ? Ge4 Hg1 Ge5 117.46(2) 3_565 . ? Ge4 Hg1 Ge5 62.54(2) . . ? Ge5 Hg1 Ge5 180.000(18) 3_565 . ? Ge4 Hg1 Ge6 62.731(18) 3_565 3_565 ? Ge4 Hg1 Ge6 117.269(18) . 3_565 ? Ge5 Hg1 Ge6 63.63(2) 3_565 3_565 ? Ge5 Hg1 Ge6 116.37(2) . 3_565 ? Ge4 Hg1 Ge6 117.269(18) 3_565 . ? Ge4 Hg1 Ge6 62.731(18) . . ? Ge5 Hg1 Ge6 116.37(2) 3_565 . ? Ge5 Hg1 Ge6 63.63(2) . . ? Ge6 Hg1 Ge6 180.0 3_565 . ? Si1 Ge1 Ge5 123.16(5) . . ? Si1 Ge1 Ge6 124.38(5) . . ? Ge5 Ge1 Ge6 74.79(3) . . ? Si1 Ge1 Ge9 118.51(5) . . ? Ge5 Ge1 Ge9 117.50(3) . . ? Ge6 Ge1 Ge9 79.45(3) . . ? Si1 Ge1 Ge8 117.37(4) . . ? Ge5 Ge1 Ge8 81.14(3) . . ? Ge6 Ge1 Ge8 117.32(3) . . ? Ge9 Ge1 Ge8 62.37(3) . . ? Si2 Ge2 Ge6 127.67(5) . . ? Si2 Ge2 Ge4 119.75(5) . . ? Ge6 Ge2 Ge4 73.18(3) . . ? Si2 Ge2 Ge9 121.72(5) . . ? Ge6 Ge2 Ge9 79.41(3) . . ? Ge4 Ge2 Ge9 117.31(3) . . ? Si2 Ge2 Ge7 114.61(5) . . ? Ge6 Ge2 Ge7 117.32(3) . . ? Ge4 Ge2 Ge7 83.12(3) . . ? Ge9 Ge2 Ge7 61.70(3) . . ? Si3 Ge3 Ge4 120.30(5) . . ? Si3 Ge3 Ge5 125.63(5) . . ? Ge4 Ge3 Ge5 72.60(3) . . ? Si3 Ge3 Ge7 116.23(5) . . ? Ge4 Ge3 Ge7 83.23(3) . . ? Ge5 Ge3 Ge7 117.75(3) . . ? Si3 Ge3 Ge8 121.08(5) . . ? Ge4 Ge3 Ge8 117.62(4) . . ? Ge5 Ge3 Ge8 81.10(3) . . ? Ge7 Ge3 Ge8 61.01(3) . . ? Ge3 Ge4 Ge2 93.76(3) . . ? Ge3 Ge4 Hg1 111.10(3) . . ? Ge2 Ge4 Hg1 111.12(3) . . ? Ge3 Ge5 Ge1 94.66(3) . . ? Ge3 Ge5 Hg1 109.94(3) . . ? Ge1 Ge5 Hg1 108.99(3) . . ? Ge2 Ge6 Ge1 95.37(3) . . ? Ge2 Ge6 Hg1 108.93(3) . . ? Ge1 Ge6 Hg1 107.86(3) . . ? Ge3 Ge7 Ge2 90.37(3) . . ? Ge3 Ge7 Ge8 59.54(3) . . ? Ge2 Ge7 Ge8 102.32(3) . . ? Ge3 Ge7 Ge9 101.73(3) . . ? Ge2 Ge7 Ge9 59.11(3) . . ? Ge8 Ge7 Ge9 60.86(3) . . ? Ge1 Ge8 Ge3 91.20(3) . . ? Ge1 Ge8 Ge7 102.12(3) . . ? Ge3 Ge8 Ge7 59.44(3) . . ? Ge1 Ge8 Ge9 58.75(2) . . ? Ge3 Ge8 Ge9 101.06(4) . . ? Ge7 Ge8 Ge9 60.02(3) . . ? Ge1 Ge9 Ge2 92.23(3) . . ? Ge1 Ge9 Ge7 101.55(4) . . ? Ge2 Ge9 Ge7 59.20(3) . . ? Ge1 Ge9 Ge8 58.87(3) . . ? Ge2 Ge9 Ge8 101.13(4) . . ? Ge7 Ge9 Ge8 59.13(3) . . ? Si12 Si1 Si11 111.79(9) . . ? Si12 Si1 Si10 109.85(9) . . ? Si11 Si1 Si10 113.76(10) . . ? Si12 Si1 Ge1 108.01(7) . . ? Si11 Si1 Ge1 106.36(8) . . ? Si10 Si1 Ge1 106.72(8) . . ? Si21 Si2 Si20 110.79(10) . . ? Si21 Si2 Si22 110.75(9) . . ? Si20 Si2 Si22 112.34(9) . . ? Si21 Si2 Ge2 107.78(8) . . ? Si20 Si2 Ge2 107.79(8) . . ? Si22 Si2 Ge2 107.17(8) . . ? Si32 Si3 Si30 109.86(9) . . ? Si32 Si3 Si31 110.62(9) . . ? Si30 Si3 Si31 112.74(9) . . ? Si32 Si3 Ge3 108.79(8) . . ? Si30 Si3 Ge3 108.32(8) . . ? Si31 Si3 Ge3 106.36(8) . . ? C10A Si10 C10B 108.0(4) . . ? C10A Si10 C10C 109.3(5) . . ? C10B Si10 C10C 109.2(4) . . ? C10A Si10 Si1 109.7(3) . . ? C10B Si10 Si1 110.3(3) . . ? C10C Si10 Si1 110.4(3) . . ? C11A Si11 C11C 109.3(5) . . ? C11A Si11 C11B 109.7(6) . . ? C11C Si11 C11B 105.9(4) . . ? C11A Si11 Si1 108.8(3) . . ? C11C Si11 Si1 112.3(3) . . ? C11B Si11 Si1 110.8(3) . . ? C12A Si12 C12C 109.4(4) . . ? C12A Si12 C12B 109.0(4) . . ? C12C Si12 C12B 108.5(4) . . ? C12A Si12 Si1 111.0(3) . . ? C12C Si12 Si1 109.6(2) . . ? C12B Si12 Si1 109.3(3) . . ? C20D Si20 C20F 110.5(18) . . ? C20D Si20 C20B 90.4(19) . . ? C20F Si20 C20B 123.6(17) . . ? C20D Si20 C20C 127.0(19) . . ? C20F Si20 C20C 20(2) . . ? C20B Si20 C20C 108.2(18) . . ? C20D Si20 C20E 109(2) . . ? C20F Si20 C20E 113(2) . . ? C20B Si20 C20E 19(2) . . ? C20C Si20 C20E 95(2) . . ? C20D Si20 C20A 20.2(16) . . ? C20F Si20 C20A 90.7(17) . . ? C20B Si20 C20A 105.4(16) . . ? C20C Si20 C20A 108.4(18) . . ? C20E Si20 C20A 123.4(19) . . ? C20D Si20 Si2 106.8(10) . . ? C20F Si20 Si2 109.9(15) . . ? C20B Si20 Si2 112.9(11) . . ? C20C Si20 Si2 110.1(17) . . ? C20E Si20 Si2 106.9(14) . . ? C20A Si20 Si2 111.6(8) . . ? C21C Si21 C21B 109.2(4) . . ? C21C Si21 C21A 107.4(4) . . ? C21B Si21 C21A 109.8(5) . . ? C21C Si21 Si2 111.1(3) . . ? C21B Si21 Si2 110.3(3) . . ? C21A Si21 Si2 109.0(3) . . ? C22B Si22 C22C 109.1(4) . . ? C22B Si22 C22A 106.6(5) . . ? C22C Si22 C22A 108.8(4) . . ? C22B Si22 Si2 112.6(3) . . ? C22C Si22 Si2 110.1(3) . . ? C22A Si22 Si2 109.5(3) . . ? C30C Si30 C30A 107.2(4) . . ? C30C Si30 C30B 109.3(4) . . ? C30A Si30 C30B 109.8(4) . . ? C30C Si30 Si3 112.3(2) . . ? C30A Si30 Si3 109.5(3) . . ? C30B Si30 Si3 108.7(2) . . ? C31C Si31 C31B 108.9(4) . . ? C31C Si31 C31A 108.3(4) . . ? C31B Si31 C31A 109.9(4) . . ? C31C Si31 Si3 110.5(2) . . ? C31B Si31 Si3 109.9(2) . . ? C31A Si31 Si3 109.3(2) . . ? C32B Si32 C32A 108.8(4) . . ? C32B Si32 C32C 109.2(3) . . ? C32A Si32 C32C 109.6(4) . . ? C32B Si32 Si3 110.1(3) . . ? C32A Si32 Si3 108.8(3) . . ? C32C Si32 Si3 110.4(3) . . ? C101 C100 C111 37.4(13) . . ? C102 C103 C104 104(2) . . ? C102 C103 C112 38.8(15) . . ? C104 C103 C112 135(2) . . ? C100 C101 C102 113(3) . . ? C103 C102 C101 116(3) . . ? C111 C112 C103 106(3) . . ? C112 C111 C100 111(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.026 _refine_diff_density_min -1.542 _refine_diff_density_rms 0.119 # Attachment 'Cd_Ge18.cif' data_p361 _database_code_depnum_ccdc_archive 'CCDC 725134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H186 Cd Ge18 Si24' _chemical_formula_weight 3049.31 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' Si Si 0.0817 0.0704 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.956(3) _cell_length_b 19.083(4) _cell_length_c 23.622(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.23(3) _cell_angle_gamma 90.00 _cell_volume 6737(2) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 17856 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 26.12 _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 4.344 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3165 _exptl_absorpt_correction_T_max 0.7873 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(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 45713 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.70 _reflns_number_total 12718 _reflns_number_gt 10171 _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^)+(0.0401P)^2^+5.5437P] 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 12718 _refine_ls_number_parameters 583 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cd1 Cd 0.5000 0.0000 0.0000 0.03320(11) Uani 1 2 d S . . Ge2 Ge 0.39323(3) 0.09620(2) 0.062025(19) 0.02964(10) Uani 1 1 d . . . Ge3 Ge 0.55468(3) 0.27983(3) 0.09528(2) 0.03506(11) Uani 1 1 d . . . Ge4 Ge 0.57396(3) 0.05514(2) 0.10624(2) 0.03138(11) Uani 1 1 d . . . Ge5 Ge 0.55135(3) 0.14397(2) 0.006222(19) 0.03050(10) Uani 1 1 d . . . Ge6 Ge 0.57423(3) 0.19575(3) 0.183465(19) 0.03423(11) Uani 1 1 d . . . Ge7 Ge 0.42706(3) 0.22019(3) 0.03770(2) 0.03607(11) Uani 1 1 d . . . Ge8 Ge 0.45089(3) 0.10540(3) 0.16232(2) 0.03550(11) Uani 1 1 d . . . Ge9 Ge 0.41229(3) 0.23458(3) 0.14490(2) 0.03344(11) Uani 1 1 d . . . Ge10 Ge 0.65136(3) 0.16921(3) 0.09097(2) 0.03802(12) Uani 1 1 d . . . Si1 Si 0.38369(7) 0.04743(6) 0.23907(5) 0.0283(2) Uani 1 1 d . . . Si32 Si 0.25949(8) 0.21775(7) -0.08950(6) 0.0369(3) Uani 1 1 d . . . Si3 Si 0.34479(7) 0.29083(6) -0.02856(5) 0.0293(2) Uani 1 1 d . . . Si31 Si 0.25175(9) 0.36218(7) 0.02486(6) 0.0385(3) Uani 1 1 d . . . Si2 Si 0.80668(7) 0.18964(7) 0.07958(5) 0.0318(3) Uani 1 1 d . . . Si22 Si 0.87092(9) 0.21675(8) 0.16901(6) 0.0422(3) Uani 1 1 d . . . Si21 Si 0.81856(9) 0.28505(8) 0.01715(6) 0.0441(3) Uani 1 1 d . . . Si12 Si 0.38202(9) -0.07297(7) 0.21997(5) 0.0357(3) Uani 1 1 d . . . Si11 Si 0.23799(9) 0.09329(8) 0.24327(7) 0.0450(3) Uani 1 1 d . . . Si33 Si 0.44729(9) 0.35556(7) -0.08080(6) 0.0416(3) Uani 1 1 d . . . Si23 Si 0.86891(9) 0.08660(8) 0.04369(6) 0.0428(3) Uani 1 1 d . . . C21B C 0.7488(4) 0.2701(4) -0.0490(3) 0.0649(17) Uani 1 1 d . . . H21A H 0.7663 0.2258 -0.0665 0.10(3) Uiso 1 1 calc R . . H21B H 0.7579 0.3087 -0.0756 0.13(3) Uiso 1 1 calc R . . H21C H 0.6855 0.2679 -0.0398 0.08(2) Uiso 1 1 calc R . . C32A C 0.3270(4) 0.1408(3) -0.1114(2) 0.0509(13) Uani 1 1 d . . . H32A H 0.3799 0.1572 -0.1307 0.069(19) Uiso 1 1 calc R . . H32B H 0.2906 0.1111 -0.1371 0.08(2) Uiso 1 1 calc R . . H32C H 0.3459 0.1137 -0.0778 0.10(3) Uiso 1 1 calc R . . C33A C 0.5368(4) 0.3970(3) -0.0348(3) 0.0610(16) Uani 1 1 d . . . H33A H 0.5699 0.3606 -0.0136 0.070(19) Uiso 1 1 calc R . . H33B H 0.5095 0.4293 -0.0082 0.08(2) Uiso 1 1 calc R . . H33C H 0.5778 0.4229 -0.0585 0.10(2) Uiso 1 1 calc R . . C33B C 0.5010(4) 0.2953(3) -0.1322(3) 0.0562(15) Uani 1 1 d . . . H33D H 0.5328 0.2579 -0.1114 0.09(2) Uiso 1 1 calc R . . H33E H 0.5434 0.3218 -0.1545 0.12(3) Uiso 1 1 calc R . . H33F H 0.4548 0.2747 -0.1576 0.058(17) Uiso 1 1 calc R . . C23C C 0.8140(8) 0.0629(7) -0.0237(5) 0.158(6) Uani 1 1 d . . . H23A H 0.7496 0.0576 -0.0188 0.30(10) Uiso 1 1 calc R . . H23B H 0.8388 0.0186 -0.0371 0.10(2) Uiso 1 1 calc R . . H23C H 0.8242 0.0999 -0.0516 0.40(15) Uiso 1 1 calc R . . Si13 Si 0.47542(10) 0.07080(8) 0.32009(6) 0.0460(3) Uani 1 1 d . . . C31B C 0.1860(3) 0.3079(3) 0.0741(2) 0.0526(14) Uani 1 1 d . . . H31A H 0.1495 0.2740 0.0522 0.08(2) Uiso 1 1 calc R . . H31B H 0.1468 0.3383 0.0956 0.12(3) Uiso 1 1 calc R . . H31C H 0.2270 0.2828 0.1004 0.09(2) Uiso 1 1 calc R . . C12A C 0.4985(4) -0.1079(3) 0.2262(3) 0.0658(17) Uani 1 1 d . . . H12A H 0.5237 -0.0987 0.2644 0.12(3) Uiso 1 1 calc R . . H12B H 0.5353 -0.0847 0.1983 0.10(3) Uiso 1 1 calc R . . H12C H 0.4977 -0.1585 0.2191 0.10(3) Uiso 1 1 calc R . . C33C C 0.3866(4) 0.4272(3) -0.1202(3) 0.0644(17) Uani 1 1 d . . . H33G H 0.3391 0.4070 -0.1448 0.08(2) Uiso 1 1 calc R . . H33H H 0.4287 0.4529 -0.1433 0.09(2) Uiso 1 1 calc R . . H33I H 0.3603 0.4594 -0.0932 0.07(2) Uiso 1 1 calc R . . C12B C 0.3121(5) -0.1182(3) 0.2722(3) 0.0643(18) Uani 1 1 d . . . H12D H 0.3361 -0.1087 0.3106 0.10(3) Uiso 1 1 calc R . . H12E H 0.3128 -0.1688 0.2651 0.10(3) Uiso 1 1 calc R . . H12F H 0.2504 -0.1009 0.2684 0.10(3) Uiso 1 1 calc R . . C31A C 0.1705(4) 0.4097(3) -0.0241(3) 0.0613(16) Uani 1 1 d . . . H31D H 0.1344 0.3756 -0.0460 0.08(2) Uiso 1 1 calc R . . H31E H 0.2035 0.4392 -0.0501 0.08(2) Uiso 1 1 calc R . . H31F H 0.1312 0.4391 -0.0019 0.12(3) Uiso 1 1 calc R . . C31C C 0.3204(4) 0.4267(3) 0.0663(3) 0.0672(18) Uani 1 1 d . . . H31G H 0.3547 0.4554 0.0405 0.065(18) Uiso 1 1 calc R . . H31H H 0.3616 0.4018 0.0926 0.07(2) Uiso 1 1 calc R . . H31I H 0.2811 0.4569 0.0878 0.08(2) Uiso 1 1 calc R . . C32B C 0.1589(3) 0.1862(3) -0.0530(3) 0.0570(15) Uani 1 1 d . . . H32D H 0.1234 0.2264 -0.0414 0.08(2) Uiso 1 1 calc R . . H32E H 0.1778 0.1588 -0.0196 0.060(18) Uiso 1 1 calc R . . H32F H 0.1227 0.1567 -0.0790 0.08(2) Uiso 1 1 calc R . . C22A C 0.8110(4) 0.2908(3) 0.2019(3) 0.0582(16) Uani 1 1 d . . . H22A H 0.8126 0.3319 0.1771 0.11(3) Uiso 1 1 calc R . . H22B H 0.8401 0.3022 0.2387 0.10(2) Uiso 1 1 calc R . . H22C H 0.7486 0.2774 0.2074 0.09(2) Uiso 1 1 calc R . . C11C C 0.2383(5) 0.1873(3) 0.2620(4) 0.074(2) Uani 1 1 d . . . H11A H 0.2695 0.1939 0.2988 0.13(4) Uiso 1 1 calc R . . H11B H 0.1765 0.2040 0.2639 0.09(2) Uiso 1 1 calc R . . H11C H 0.2690 0.2140 0.2330 0.09(2) Uiso 1 1 calc R . . C13C C 0.4361(6) 0.0181(5) 0.3814(3) 0.089(3) Uani 1 1 d . . . H13A H 0.4382 -0.0318 0.3721 0.08(2) Uiso 1 1 calc R . . H13B H 0.3745 0.0314 0.3893 0.062(19) Uiso 1 1 calc R . . H13C H 0.4750 0.0274 0.4149 0.09(2) Uiso 1 1 calc R . . C32C C 0.2222(4) 0.2693(4) -0.1536(2) 0.0600(15) Uani 1 1 d . . . H32G H 0.1869 0.3097 -0.1420 0.09(2) Uiso 1 1 calc R . . H32H H 0.1855 0.2395 -0.1791 0.11(3) Uiso 1 1 calc R . . H32I H 0.2748 0.2857 -0.1734 0.10(3) Uiso 1 1 calc R . . C22B C 0.8674(7) 0.1396(4) 0.2165(3) 0.092(3) Uani 1 1 d . . . H22D H 0.8988 0.1003 0.1995 0.11(3) Uiso 1 1 calc R . . H22E H 0.8050 0.1265 0.2221 0.11(3) Uiso 1 1 calc R . . H22F H 0.8966 0.1512 0.2532 0.13(3) Uiso 1 1 calc R . . C12C C 0.3370(5) -0.0915(4) 0.1470(3) 0.0708(18) Uani 1 1 d . . . H12G H 0.3738 -0.0677 0.1195 0.12(3) Uiso 1 1 calc R . . H12H H 0.2752 -0.0744 0.1429 0.056(17) Uiso 1 1 calc R . . H12I H 0.3380 -0.1421 0.1401 0.10(2) Uiso 1 1 calc R . . C11A C 0.1748(5) 0.0483(4) 0.2996(4) 0.090(3) Uani 1 1 d . . . H11D H 0.1722 -0.0021 0.2917 0.14(4) Uiso 1 1 calc R . . H11E H 0.1140 0.0672 0.3000 0.15(4) Uiso 1 1 calc R . . H11F H 0.2053 0.0561 0.3365 0.12(4) Uiso 1 1 calc R . . C13A C 0.4710(4) 0.1659(3) 0.3387(3) 0.0633(17) Uani 1 1 d . . . H13D H 0.4918 0.1938 0.3069 0.09(2) Uiso 1 1 calc R . . H13E H 0.5097 0.1747 0.3723 0.08(2) Uiso 1 1 calc R . . H13F H 0.4094 0.1790 0.3465 0.08(2) Uiso 1 1 calc R . . C13B C 0.5950(4) 0.0471(4) 0.3072(3) 0.0660(17) Uani 1 1 d . . . H13G H 0.5986 -0.0028 0.2974 0.11(3) Uiso 1 1 calc R . . H13H H 0.6320 0.0562 0.3415 0.10(3) Uiso 1 1 calc R . . H13I H 0.6166 0.0753 0.2759 0.18(5) Uiso 1 1 calc R . . C21A C 0.7850(5) 0.3690(3) 0.0497(3) 0.0712(18) Uani 1 1 d . . . H21D H 0.8214 0.3771 0.0845 0.10(3) Uiso 1 1 calc R . . H21E H 0.7217 0.3668 0.0588 0.10(3) Uiso 1 1 calc R . . H21F H 0.7941 0.4075 0.0231 0.16(4) Uiso 1 1 calc R . . C21C C 0.9386(4) 0.2949(5) -0.0027(3) 0.079(2) Uani 1 1 d . . . H21G H 0.9587 0.2516 -0.0204 0.08(2) Uiso 1 1 calc R . . H21H H 0.9760 0.3045 0.0314 0.08(2) Uiso 1 1 calc R . . H21I H 0.9435 0.3339 -0.0294 0.10(3) Uiso 1 1 calc R . . C22C C 0.9905(3) 0.2443(5) 0.1605(3) 0.073(2) Uani 1 1 d . . . H22G H 1.0235 0.2060 0.1432 0.08(2) Uiso 1 1 calc R . . H22H H 1.0181 0.2553 0.1978 0.13(3) Uiso 1 1 calc R . . H22I H 0.9921 0.2858 0.1362 0.16(5) Uiso 1 1 calc R . . C11B C 0.1788(5) 0.0812(6) 0.1733(4) 0.100(3) Uani 1 1 d . . . H11G H 0.1782 0.0314 0.1633 0.16(5) Uiso 1 1 calc R . . H11H H 0.2098 0.1077 0.1444 0.11(3) Uiso 1 1 calc R . . H11I H 0.1172 0.0983 0.1753 0.073(19) Uiso 1 1 calc R . . C23A C 0.8496(11) 0.0131(5) 0.0935(6) 0.148(5) Uani 1 1 d . . . H23D H 0.8787 0.0237 0.1304 0.47(19) Uiso 1 1 calc R . . H23E H 0.8746 -0.0301 0.0784 0.20(5) Uiso 1 1 calc R . . H23F H 0.7851 0.0072 0.0980 0.45(17) Uiso 1 1 calc R . . C23B C 0.9908(4) 0.0978(5) 0.0380(6) 0.113(4) Uani 1 1 d . . . H23G H 1.0174 0.1112 0.0749 0.17(5) Uiso 1 1 calc R . . H23H H 1.0024 0.1345 0.0102 0.21(7) Uiso 1 1 calc R . . H23I H 1.0172 0.0536 0.0257 0.11(3) Uiso 1 1 calc R . . C5 C 0.6888(7) 0.4470(5) 0.2387(5) 0.110(3) Uani 1 1 d D . . H5A H 0.7482 0.4291 0.2502 0.164 Uiso 1 1 calc R A 1 H5B H 0.6819 0.4948 0.2530 0.164 Uiso 1 1 calc R A 1 H5C H 0.6822 0.4472 0.1972 0.164 Uiso 1 1 calc R A 1 C1 C 0.4347(9) 0.3673(8) 0.3375(6) 0.162(5) Uani 1 1 d D C . H1A H 0.3872 0.3323 0.3404 0.243 Uiso 1 1 calc R . . H1B H 0.4132 0.4128 0.3507 0.243 Uiso 1 1 calc R . . H1C H 0.4870 0.3529 0.3609 0.243 Uiso 1 1 calc R . . C2 C 0.4598(9) 0.3734(7) 0.2782(6) 0.146(4) Uani 1 1 d D . . H2A H 0.4018 0.3807 0.2573 0.175 Uiso 1 1 calc R B 1 H2B H 0.4785 0.3253 0.2683 0.175 Uiso 1 1 calc R B 1 C3 C 0.5233(11) 0.4191(10) 0.2474(11) 0.123(9) Uani 0.50 1 d PD C 1 H3A H 0.5122 0.4136 0.2060 0.147 Uiso 0.50 1 calc PR C 1 H3B H 0.5124 0.4687 0.2571 0.147 Uiso 0.50 1 calc PR C 1 C4 C 0.6188(10) 0.4010(8) 0.2623(10) 0.103(6) Uani 0.50 1 d PD C 1 H4A H 0.6268 0.4014 0.3041 0.124 Uiso 0.50 1 calc PR C 1 H4B H 0.6297 0.3524 0.2495 0.124 Uiso 0.50 1 calc PR C 1 C4A C 0.5938(12) 0.4215(14) 0.2292(9) 0.135(11) Uani 0.50 1 d PD C 2 H4A1 H 0.5577 0.4587 0.2101 0.162 Uiso 0.50 1 calc PR C 2 H4A2 H 0.5935 0.3802 0.2038 0.162 Uiso 0.50 1 calc PR C 2 C3A C 0.5516(10) 0.4018(11) 0.2838(8) 0.106(7) Uani 0.50 1 d PD C 2 H3A1 H 0.5902 0.3666 0.3034 0.127 Uiso 0.50 1 calc PR C 2 H3A2 H 0.5505 0.4439 0.3082 0.127 Uiso 0.50 1 calc PR C 2 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 Cd1 0.0385(2) 0.0300(2) 0.0313(2) -0.0072(2) 0.00315(18) -0.00144(18) Ge2 0.0303(2) 0.0308(2) 0.0279(2) -0.00121(19) 0.00288(17) -0.00330(18) Ge3 0.0379(2) 0.0311(2) 0.0363(3) 0.0010(2) 0.00329(19) -0.00706(19) Ge4 0.0327(2) 0.0318(2) 0.0297(2) -0.0003(2) 0.00203(18) 0.00071(18) Ge5 0.0313(2) 0.0334(2) 0.0272(2) -0.0015(2) 0.00481(17) -0.00240(18) Ge6 0.0349(2) 0.0411(3) 0.0266(2) -0.0024(2) 0.00030(18) -0.0069(2) Ge7 0.0413(2) 0.0339(3) 0.0329(3) 0.0006(2) -0.00002(19) 0.0024(2) Ge8 0.0415(2) 0.0356(3) 0.0299(2) 0.0007(2) 0.0071(2) -0.0047(2) Ge9 0.0361(2) 0.0345(3) 0.0303(2) -0.0008(2) 0.00805(18) 0.00238(19) Ge10 0.0308(2) 0.0439(3) 0.0397(3) -0.0063(2) 0.00484(19) -0.0055(2) Si1 0.0319(6) 0.0289(6) 0.0244(6) 0.0022(5) 0.0035(4) -0.0002(5) Si32 0.0359(6) 0.0403(7) 0.0343(7) -0.0062(6) 0.0001(5) 0.0032(5) Si3 0.0318(5) 0.0291(6) 0.0271(6) 0.0004(5) 0.0041(4) 0.0016(5) Si31 0.0395(6) 0.0384(7) 0.0379(7) -0.0072(6) 0.0061(5) 0.0058(5) Si2 0.0259(5) 0.0394(7) 0.0302(6) -0.0028(5) 0.0022(4) -0.0038(5) Si22 0.0412(7) 0.0494(8) 0.0357(7) -0.0073(6) -0.0036(5) -0.0042(6) Si21 0.0344(6) 0.0517(8) 0.0463(8) 0.0126(7) 0.0050(6) -0.0067(6) Si12 0.0463(7) 0.0294(6) 0.0317(7) -0.0001(5) 0.0032(5) 0.0005(5) Si11 0.0387(7) 0.0433(8) 0.0542(9) 0.0088(7) 0.0155(6) 0.0083(6) Si33 0.0473(7) 0.0392(7) 0.0389(7) 0.0103(6) 0.0099(6) -0.0023(6) Si23 0.0338(6) 0.0481(8) 0.0462(8) -0.0131(7) 0.0005(6) 0.0022(6) C21B 0.062(4) 0.079(5) 0.054(4) 0.019(4) -0.002(3) -0.006(3) C32A 0.054(3) 0.048(3) 0.051(3) -0.015(3) 0.004(3) 0.006(2) C33A 0.063(3) 0.055(4) 0.066(4) 0.013(3) 0.013(3) -0.021(3) C33B 0.054(3) 0.066(4) 0.050(3) 0.000(3) 0.018(3) -0.006(3) C23C 0.166(10) 0.173(11) 0.129(9) -0.119(9) -0.087(7) 0.112(8) Si13 0.0560(8) 0.0536(9) 0.0280(7) 0.0010(6) -0.0037(6) -0.0148(7) C31B 0.040(3) 0.073(4) 0.045(3) -0.010(3) 0.009(2) 0.003(3) C12A 0.070(4) 0.040(3) 0.088(5) -0.001(3) 0.015(4) 0.011(3) C33C 0.073(4) 0.061(4) 0.059(4) 0.026(3) 0.006(3) 0.001(3) C12B 0.088(5) 0.038(3) 0.069(4) 0.004(3) 0.032(4) -0.009(3) C31A 0.065(4) 0.056(4) 0.062(4) -0.002(3) 0.006(3) 0.025(3) C31C 0.070(4) 0.060(4) 0.072(4) -0.029(4) 0.014(4) -0.006(3) C32B 0.045(3) 0.063(4) 0.064(4) -0.021(3) 0.008(3) -0.012(3) C22A 0.048(3) 0.072(4) 0.056(3) -0.030(3) 0.008(3) -0.011(3) C11C 0.067(4) 0.049(4) 0.110(6) 0.014(4) 0.043(4) 0.020(3) C13C 0.117(7) 0.105(7) 0.044(4) 0.014(4) -0.016(4) -0.055(5) C32C 0.067(4) 0.067(4) 0.045(3) -0.001(3) -0.016(3) 0.010(3) C22B 0.156(9) 0.073(5) 0.045(4) 0.004(4) -0.024(4) -0.009(5) C12C 0.102(5) 0.057(4) 0.052(4) -0.012(3) -0.016(4) -0.004(4) C11A 0.077(5) 0.070(5) 0.128(8) 0.035(5) 0.066(5) 0.021(4) C13A 0.069(4) 0.071(4) 0.050(4) -0.022(3) 0.010(3) -0.017(3) C13B 0.060(3) 0.074(5) 0.062(4) -0.002(4) -0.028(3) 0.000(3) C21A 0.080(4) 0.049(4) 0.085(5) 0.008(4) 0.008(4) -0.015(3) C21C 0.043(3) 0.120(7) 0.076(5) 0.044(5) 0.011(3) -0.009(4) C22C 0.036(3) 0.108(6) 0.076(4) -0.042(5) -0.003(3) 0.002(3) C11B 0.048(4) 0.155(9) 0.095(6) -0.018(6) -0.016(4) 0.037(5) C23A 0.223(13) 0.056(5) 0.171(12) 0.022(6) 0.106(10) 0.050(7) C23B 0.049(4) 0.091(6) 0.202(11) -0.072(8) 0.027(5) 0.002(4) C5 0.128(8) 0.075(6) 0.127(8) 0.007(6) 0.018(6) 0.027(5) C1 0.160(11) 0.165(13) 0.160(13) -0.037(11) 0.001(10) 0.054(10) C2 0.137(10) 0.125(10) 0.174(14) -0.024(10) -0.007(9) -0.008(8) C3 0.125(18) 0.068(12) 0.17(3) 0.004(14) -0.062(18) -0.007(13) C4 0.115(15) 0.047(9) 0.15(2) 0.000(11) 0.017(14) 0.031(9) C4A 0.19(3) 0.099(17) 0.115(19) 0.060(14) -0.061(19) -0.044(19) C3A 0.104(14) 0.123(17) 0.090(13) -0.011(12) -0.016(11) 0.059(13) _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 Cd1 Ge5 2.8548(7) . ? Cd1 Ge5 2.8548(7) 3_655 ? Cd1 Ge2 2.8720(7) . ? Cd1 Ge2 2.8720(7) 3_655 ? Cd1 Ge4 2.9006(8) . ? Cd1 Ge4 2.9006(8) 3_655 ? Ge2 Ge7 2.4914(8) . ? Ge2 Ge8 2.4957(9) . ? Ge2 Ge5 2.8988(9) . ? Ge3 Ge10 2.5629(8) . ? Ge3 Ge7 2.5664(9) . ? Ge3 Ge9 2.6170(9) . ? Ge3 Ge6 2.6367(8) . ? Ge4 Ge10 2.4983(8) . ? Ge4 Ge8 2.5003(9) . ? Ge4 Ge5 2.9168(8) . ? Ge5 Ge7 2.4963(8) . ? Ge5 Ge10 2.4990(10) . ? Ge6 Ge8 2.5600(8) . ? Ge6 Ge10 2.5606(9) . ? Ge6 Ge9 2.6596(9) . ? Ge7 Si3 2.3730(14) . ? Ge7 Ge9 2.5652(8) . ? Ge8 Si1 2.3796(13) . ? Ge8 Ge9 2.5614(9) . ? Ge10 Si2 2.3810(13) . ? Si1 Si12 2.3413(18) . ? Si1 Si13 2.3537(19) . ? Si1 Si11 2.3540(17) . ? Si32 C32B 1.862(5) . ? Si32 C32A 1.866(5) . ? Si32 C32C 1.873(6) . ? Si32 Si3 2.3457(19) . ? Si3 Si31 2.3492(17) . ? Si3 Si33 2.3549(17) . ? Si31 C31C 1.858(6) . ? Si31 C31B 1.866(6) . ? Si31 C31A 1.878(6) . ? Si2 Si22 2.3443(19) . ? Si2 Si23 2.3478(19) . ? Si2 Si21 2.3540(19) . ? Si22 C22B 1.854(8) . ? Si22 C22A 1.860(6) . ? Si22 C22C 1.882(6) . ? Si21 C21A 1.856(7) . ? Si21 C21B 1.868(6) . ? Si21 C21C 1.882(6) . ? Si12 C12C 1.860(6) . ? Si12 C12B 1.861(5) . ? Si12 C12A 1.866(6) . ? Si11 C11C 1.848(7) . ? Si11 C11B 1.859(8) . ? Si11 C11A 1.870(6) . ? Si33 C33A 1.866(6) . ? Si33 C33C 1.869(6) . ? Si33 C33B 1.875(6) . ? Si23 C23C 1.820(8) . ? Si23 C23B 1.845(7) . ? Si23 C23A 1.861(10) . ? Si13 C13A 1.868(6) . ? Si13 C13C 1.876(7) . ? Si13 C13B 1.881(6) . ? C5 C4 1.491(13) . ? C5 C4A 1.511(14) . ? C1 C2 1.470(12) . ? C2 C3A 1.478(13) . ? C2 C3 1.499(14) . ? C3 C4 1.498(14) . ? C4A C3A 1.505(14) . ? 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 Ge5 Cd1 Ge5 180.000(19) . 3_655 ? Ge5 Cd1 Ge2 60.819(18) . . ? Ge5 Cd1 Ge2 119.181(18) 3_655 . ? Ge5 Cd1 Ge2 119.181(18) . 3_655 ? Ge5 Cd1 Ge2 60.819(18) 3_655 3_655 ? Ge2 Cd1 Ge2 180.00(2) . 3_655 ? Ge5 Cd1 Ge4 60.896(14) . . ? Ge5 Cd1 Ge4 119.104(14) 3_655 . ? Ge2 Cd1 Ge4 61.812(19) . . ? Ge2 Cd1 Ge4 118.19(2) 3_655 . ? Ge5 Cd1 Ge4 119.104(14) . 3_655 ? Ge5 Cd1 Ge4 60.896(14) 3_655 3_655 ? Ge2 Cd1 Ge4 118.189(19) . 3_655 ? Ge2 Cd1 Ge4 61.811(19) 3_655 3_655 ? Ge4 Cd1 Ge4 180.00(2) . 3_655 ? Ge7 Ge2 Ge8 94.96(2) . . ? Ge7 Ge2 Cd1 111.56(2) . . ? Ge8 Ge2 Cd1 110.53(2) . . ? Ge7 Ge2 Ge5 54.543(17) . . ? Ge8 Ge2 Ge5 98.72(3) . . ? Cd1 Ge2 Ge5 59.30(2) . . ? Ge10 Ge3 Ge7 91.31(3) . . ? Ge10 Ge3 Ge9 102.48(3) . . ? Ge7 Ge3 Ge9 59.32(2) . . ? Ge10 Ge3 Ge6 58.99(3) . . ? Ge7 Ge3 Ge6 101.90(3) . . ? Ge9 Ge3 Ge6 60.82(3) . . ? Ge10 Ge4 Ge8 95.57(3) . . ? Ge10 Ge4 Cd1 110.76(2) . . ? Ge8 Ge4 Cd1 109.49(3) . . ? Ge10 Ge4 Ge5 54.30(2) . . ? Ge8 Ge4 Ge5 98.14(3) . . ? Cd1 Ge4 Ge5 58.777(19) . . ? Ge7 Ge5 Ge10 94.50(3) . . ? Ge7 Ge5 Cd1 111.97(2) . . ? Ge10 Ge5 Cd1 112.22(2) . . ? Ge7 Ge5 Ge2 54.39(2) . . ? Ge10 Ge5 Ge2 99.78(3) . . ? Cd1 Ge5 Ge2 59.884(13) . . ? Ge7 Ge5 Ge4 99.30(3) . . ? Ge10 Ge5 Ge4 54.28(2) . . ? Cd1 Ge5 Ge4 60.327(18) . . ? Ge2 Ge5 Ge4 61.31(2) . . ? Ge8 Ge6 Ge10 92.60(3) . . ? Ge8 Ge6 Ge3 101.46(3) . . ? Ge10 Ge6 Ge3 59.07(2) . . ? Ge8 Ge6 Ge9 58.74(2) . . ? Ge10 Ge6 Ge9 101.38(3) . . ? Ge3 Ge6 Ge9 59.22(3) . . ? Si3 Ge7 Ge2 125.94(4) . . ? Si3 Ge7 Ge5 120.50(4) . . ? Ge2 Ge7 Ge5 71.07(2) . . ? Si3 Ge7 Ge9 121.87(4) . . ? Ge2 Ge7 Ge9 81.25(2) . . ? Ge5 Ge7 Ge9 116.75(3) . . ? Si3 Ge7 Ge3 116.97(4) . . ? Ge2 Ge7 Ge3 116.90(3) . . ? Ge5 Ge7 Ge3 82.48(3) . . ? Ge9 Ge7 Ge3 61.33(3) . . ? Si1 Ge8 Ge2 123.37(4) . . ? Si1 Ge8 Ge4 124.52(4) . . ? Ge2 Ge8 Ge4 72.81(3) . . ? Si1 Ge8 Ge6 119.14(4) . . ? Ge2 Ge8 Ge6 116.90(3) . . ? Ge4 Ge8 Ge6 79.75(2) . . ? Si1 Ge8 Ge9 118.07(4) . . ? Ge2 Ge8 Ge9 81.24(2) . . ? Ge4 Ge8 Ge9 116.74(2) . . ? Ge6 Ge8 Ge9 62.57(2) . . ? Ge8 Ge9 Ge7 91.61(2) . . ? Ge8 Ge9 Ge3 101.96(2) . . ? Ge7 Ge9 Ge3 59.36(3) . . ? Ge8 Ge9 Ge6 58.689(18) . . ? Ge7 Ge9 Ge6 101.31(3) . . ? Ge3 Ge9 Ge6 59.95(2) . . ? Si2 Ge10 Ge4 128.21(4) . . ? Si2 Ge10 Ge5 119.82(4) . . ? Ge4 Ge10 Ge5 71.42(2) . . ? Si2 Ge10 Ge6 122.55(4) . . ? Ge4 Ge10 Ge6 79.78(2) . . ? Ge5 Ge10 Ge6 116.50(3) . . ? Si2 Ge10 Ge3 115.09(4) . . ? Ge4 Ge10 Ge3 116.53(3) . . ? Ge5 Ge10 Ge3 82.50(3) . . ? Ge6 Ge10 Ge3 61.94(2) . . ? Si12 Si1 Si13 110.13(7) . . ? Si12 Si1 Si11 111.72(7) . . ? Si13 Si1 Si11 113.99(8) . . ? Si12 Si1 Ge8 108.12(6) . . ? Si13 Si1 Ge8 106.34(6) . . ? Si11 Si1 Ge8 106.17(6) . . ? C32B Si32 C32A 109.2(3) . . ? C32B Si32 C32C 108.9(3) . . ? C32A Si32 C32C 109.7(3) . . ? C32B Si32 Si3 109.78(19) . . ? C32A Si32 Si3 110.52(19) . . ? C32C Si32 Si3 108.8(2) . . ? Si32 Si3 Si31 110.78(6) . . ? Si32 Si3 Si33 109.87(7) . . ? Si31 Si3 Si33 112.88(7) . . ? Si32 Si3 Ge7 108.83(6) . . ? Si31 Si3 Ge7 106.12(6) . . ? Si33 Si3 Ge7 108.19(6) . . ? C31C Si31 C31B 109.5(3) . . ? C31C Si31 C31A 109.6(3) . . ? C31B Si31 C31A 107.9(3) . . ? C31C Si31 Si3 109.9(2) . . ? C31B Si31 Si3 110.54(19) . . ? C31A Si31 Si3 109.35(19) . . ? Si22 Si2 Si23 110.85(7) . . ? Si22 Si2 Si21 110.82(7) . . ? Si23 Si2 Si21 112.39(7) . . ? Si22 Si2 Ge10 107.56(6) . . ? Si23 Si2 Ge10 107.82(6) . . ? Si21 Si2 Ge10 107.17(6) . . ? C22B Si22 C22A 108.9(4) . . ? C22B Si22 C22C 109.6(4) . . ? C22A Si22 C22C 107.9(3) . . ? C22B Si22 Si2 110.5(3) . . ? C22A Si22 Si2 110.9(2) . . ? C22C Si22 Si2 108.9(2) . . ? C21A Si21 C21B 109.1(3) . . ? C21A Si21 C21C 107.0(4) . . ? C21B Si21 C21C 108.3(3) . . ? C21A Si21 Si2 112.3(2) . . ? C21B Si21 Si2 110.7(2) . . ? C21C Si21 Si2 109.2(2) . . ? C12C Si12 C12B 109.5(3) . . ? C12C Si12 C12A 108.0(3) . . ? C12B Si12 C12A 109.2(3) . . ? C12C Si12 Si1 111.5(2) . . ? C12B Si12 Si1 109.2(2) . . ? C12A Si12 Si1 109.4(2) . . ? C11C Si11 C11B 109.2(5) . . ? C11C Si11 C11A 105.8(3) . . ? C11B Si11 C11A 109.8(5) . . ? C11C Si11 Si1 112.2(2) . . ? C11B Si11 Si1 109.0(2) . . ? C11A Si11 Si1 110.7(2) . . ? C33A Si33 C33C 107.6(3) . . ? C33A Si33 C33B 108.8(3) . . ? C33C Si33 C33B 109.8(3) . . ? C33A Si33 Si3 112.58(19) . . ? C33C Si33 Si3 109.4(2) . . ? C33B Si33 Si3 108.75(19) . . ? C23C Si23 C23B 112.2(6) . . ? C23C Si23 C23A 106.9(8) . . ? C23B Si23 C23A 108.2(7) . . ? C23C Si23 Si2 110.6(3) . . ? C23B Si23 Si2 109.7(3) . . ? C23A Si23 Si2 109.2(3) . . ? C13A Si13 C13C 108.9(4) . . ? C13A Si13 C13B 108.3(3) . . ? C13C Si13 C13B 108.9(4) . . ? C13A Si13 Si1 110.5(2) . . ? C13C Si13 Si1 109.6(2) . . ? C13B Si13 Si1 110.5(2) . . ? C4 C5 C4A 36.5(10) . . ? C1 C2 C3A 102.3(13) . . ? C1 C2 C3 134.3(15) . . ? C3A C2 C3 39.2(10) . . ? C4 C3 C2 111.6(14) . . ? C5 C4 C3 116.9(14) . . ? C3A C4A C5 112.1(14) . . ? C2 C3A C4A 115.7(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.469 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.087 # Attachment 'Zn_Ge18.CIF' data_fh29monc _database_code_depnum_ccdc_archive 'CCDC 725135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H162 Ge18 Si24 Zn' _chemical_formula_weight 2857.99 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' Si Si 0.0817 0.0704 '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' Ge Ge 0.1547 1.8001 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.325(4) _cell_length_b 25.671(5) _cell_length_c 15.773(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.51(3) _cell_angle_gamma 90.00 _cell_volume 6433(2) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 22235 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 26.15 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 4.566 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3562 _exptl_absorpt_correction_T_max 0.5795 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(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 19695 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.65 _reflns_number_total 6198 _reflns_number_gt 5047 _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^)+(0.0511P)^2^+8.9195P] 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 6198 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Zn1 Zn 0.5000 0.0000 0.0000 0.0434(2) Uani 1 4 d S . . Ge1 Ge 0.26164(3) 0.07031(2) -0.16438(3) 0.04819(13) Uani 1 1 d . . . Ge2 Ge 0.27684(4) 0.0000 0.04802(4) 0.04832(18) Uani 1 2 d S . . Ge3 Ge 0.36354(4) 0.0000 -0.15977(4) 0.04044(15) Uani 1 2 d S . . Ge4 Ge 0.36763(3) 0.057407(18) -0.00208(3) 0.04098(12) Uani 1 1 d . . . Ge5 Ge 0.16519(3) 0.05213(2) -0.07987(3) 0.05392(15) Uani 1 1 d . . . Ge6 Ge 0.14877(4) 0.0000 -0.22958(4) 0.05346(19) Uani 1 2 d S . . Si1 Si 0.23993(8) 0.14775(5) -0.25404(8) 0.0486(3) Uani 1 1 d . A . Si2 Si 0.27332(11) 0.0000 0.19654(11) 0.0509(4) Uani 1 2 d S . . Si20 Si 0.1397(7) 0.0000 0.1895(7) 0.034(4) Uiso 0.173(12) 2 d SP . 1 Si21 Si 0.3450(9) 0.0815(5) 0.2644(7) 0.053(4) Uiso 0.173(12) 1 d P . 1 Si22 Si 0.4001(7) 0.0000 0.3081(7) 0.035(3) Uiso 0.152(9) 2 d SP . 2 Si23 Si 0.1917(8) 0.0766(5) 0.1942(7) 0.064(5) Uiso 0.152(9) 1 d P . 2 Si24 Si 0.1398(6) 0.0210(6) 0.1862(6) 0.041(2) Uiso 0.164(6) 1 d P . 3 Si26 Si 0.3120(10) 0.0907(5) 0.2475(8) 0.067(4) Uiso 0.164(6) 1 d P . 3 Si27 Si 0.3994(6) 0.0236(5) 0.3064(6) 0.054(2) Uiso 0.174(4) 1 d P . 4 Si29 Si 0.1635(7) 0.0497(6) 0.2001(7) 0.069(3) Uiso 0.174(4) 1 d P . 4 Si25 Si 0.3719(7) 0.0592(5) 0.2868(7) 0.056(3) Uiso 0.164(6) 1 d P . 5 Si28 Si 0.2329(7) 0.0931(4) 0.2048(6) 0.065(3) Uiso 0.174(4) 1 d P . 6 Si10 Si 0.22155(12) 0.12160(7) -0.40392(9) 0.0733(5) Uani 1 1 d . . . Si11 Si 0.11589(10) 0.18603(7) -0.25554(11) 0.0722(4) Uani 1 1 d . . . Si12 Si 0.35966(10) 0.20011(7) -0.18379(11) 0.0663(4) Uani 1 1 d . . . C11B C 0.0265(4) 0.1389(3) -0.2965(5) 0.093(2) Uani 1 1 d . A . H11A H -0.0243 0.1558 -0.2965 0.139 Uiso 1 1 calc R . . H11B H 0.0404 0.1087 -0.2551 0.139 Uiso 1 1 calc R . . H11C H 0.0163 0.1275 -0.3593 0.139 Uiso 1 1 calc R . . C10C C 0.142(3) 0.0732(14) -0.4538(19) 0.112(13) Uani 0.50 1 d P A 1 H10A H 0.1385 0.0643 -0.5157 0.167 Uiso 0.50 1 calc PR A 1 H10B H 0.0877 0.0868 -0.4584 0.167 Uiso 0.50 1 calc PR A 1 H10C H 0.1565 0.0420 -0.4148 0.167 Uiso 0.50 1 calc PR A 1 C10B C 0.192(2) 0.1754(19) -0.484(2) 0.115(11) Uani 0.50 1 d P A 1 H10D H 0.1849 0.1630 -0.5456 0.173 Uiso 0.50 1 calc PR A 1 H10E H 0.2361 0.2021 -0.4632 0.173 Uiso 0.50 1 calc PR A 1 H10F H 0.1389 0.1903 -0.4872 0.173 Uiso 0.50 1 calc PR A 1 C10A C 0.3274(15) 0.1027(13) -0.3952(17) 0.145(14) Uani 0.50 1 d P A 1 H10G H 0.3239 0.0911 -0.4558 0.218 Uiso 0.50 1 calc PR A 1 H10H H 0.3492 0.0743 -0.3504 0.218 Uiso 0.50 1 calc PR A 1 H10I H 0.3653 0.1328 -0.3748 0.218 Uiso 0.50 1 calc PR A 1 C11A C 0.089(4) 0.247(3) -0.327(5) 0.16(2) Uani 0.50 1 d P A 1 H11D H 0.0376 0.2618 -0.3267 0.233 Uiso 0.50 1 calc PR A 1 H11E H 0.0810 0.2381 -0.3907 0.233 Uiso 0.50 1 calc PR A 1 H11F H 0.1355 0.2717 -0.3013 0.233 Uiso 0.50 1 calc PR A 1 C11C C 0.1315(18) 0.2056(11) -0.1335(15) 0.085(8) Uani 0.50 1 d P A 1 H11G H 0.0797 0.2216 -0.1346 0.127 Uiso 0.50 1 calc PR A 1 H11H H 0.1778 0.2307 -0.1092 0.127 Uiso 0.50 1 calc PR A 1 H11I H 0.1450 0.1747 -0.0939 0.127 Uiso 0.50 1 calc PR A 1 C12C C 0.366(3) 0.2340(12) -0.067(3) 0.091(9) Uani 0.50 1 d P A 1 H12A H 0.4176 0.2552 -0.0417 0.137 Uiso 0.50 1 calc PR A 1 H12B H 0.3678 0.2072 -0.0226 0.137 Uiso 0.50 1 calc PR A 1 H12C H 0.3170 0.2564 -0.0807 0.137 Uiso 0.50 1 calc PR A 1 C12B C 0.3476(19) 0.2649(8) -0.258(2) 0.092(6) Uani 0.50 1 d P A 1 H12D H 0.3976 0.2867 -0.2287 0.138 Uiso 0.50 1 calc PR A 1 H12E H 0.2976 0.2841 -0.2612 0.138 Uiso 0.50 1 calc PR A 1 H12F H 0.3415 0.2556 -0.3207 0.138 Uiso 0.50 1 calc PR A 1 C12A C 0.460(3) 0.156(2) -0.159(4) 0.084(9) Uani 0.50 1 d P A 1 H12G H 0.5114 0.1767 -0.1298 0.126 Uiso 0.50 1 calc PR A 1 H12H H 0.4586 0.1417 -0.2179 0.126 Uiso 0.50 1 calc PR A 1 H12I H 0.4606 0.1270 -0.1184 0.126 Uiso 0.50 1 calc PR A 1 C10F C 0.119(3) 0.0859(16) -0.458(2) 0.113(12) Uani 0.50 1 d P A 2 H10J H 0.1106 0.0747 -0.5204 0.169 Uiso 0.50 1 calc PR A 2 H10K H 0.0728 0.1091 -0.4614 0.169 Uiso 0.50 1 calc PR A 2 H10L H 0.1197 0.0554 -0.4204 0.169 Uiso 0.50 1 calc PR A 2 C10E C 0.220(3) 0.182(2) -0.474(2) 0.19(3) Uani 0.50 1 d P A 2 H10M H 0.2124 0.1714 -0.5365 0.288 Uiso 0.50 1 calc PR A 2 H10N H 0.2738 0.2003 -0.4443 0.288 Uiso 0.50 1 calc PR A 2 H10O H 0.1740 0.2045 -0.4765 0.288 Uiso 0.50 1 calc PR A 2 C10D C 0.2983(14) 0.0690(10) -0.4033(13) 0.120(10) Uani 0.50 1 d P A 2 H10P H 0.2881 0.0595 -0.4670 0.180 Uiso 0.50 1 calc PR A 2 H10Q H 0.2904 0.0383 -0.3707 0.180 Uiso 0.50 1 calc PR A 2 H10R H 0.3560 0.0819 -0.3718 0.180 Uiso 0.50 1 calc PR A 2 C11D C 0.086(3) 0.240(2) -0.345(4) 0.107(11) Uani 0.50 1 d P A 2 H11J H 0.0341 0.2570 -0.3475 0.161 Uiso 0.50 1 calc PR A 2 H11K H 0.0763 0.2254 -0.4054 0.161 Uiso 0.50 1 calc PR A 2 H11L H 0.1312 0.2658 -0.3274 0.161 Uiso 0.50 1 calc PR A 2 C11F C 0.131(2) 0.2128(18) -0.143(2) 0.148(17) Uani 0.50 1 d P A 2 H11M H 0.0779 0.2282 -0.1464 0.221 Uiso 0.50 1 calc PR A 2 H11N H 0.1746 0.2396 -0.1254 0.221 Uiso 0.50 1 calc PR A 2 H11O H 0.1477 0.1849 -0.0968 0.221 Uiso 0.50 1 calc PR A 2 C12D C 0.450(3) 0.168(2) -0.167(4) 0.104(15) Uani 0.50 1 d P A 2 H12J H 0.4982 0.1911 -0.1381 0.156 Uiso 0.50 1 calc PR A 2 H12K H 0.4484 0.1557 -0.2268 0.156 Uiso 0.50 1 calc PR A 2 H12L H 0.4557 0.1376 -0.1268 0.156 Uiso 0.50 1 calc PR A 2 C12E C 0.3627(18) 0.2478(7) -0.263(2) 0.102(8) Uani 0.50 1 d P A 2 H12M H 0.4128 0.2696 -0.2332 0.153 Uiso 0.50 1 calc PR A 2 H12N H 0.3121 0.2696 -0.2812 0.153 Uiso 0.50 1 calc PR A 2 H12O H 0.3648 0.2308 -0.3173 0.153 Uiso 0.50 1 calc PR A 2 C12F C 0.366(3) 0.2168(12) -0.076(3) 0.096(9) Uani 0.50 1 d P A 2 H12P H 0.4157 0.2387 -0.0448 0.144 Uiso 0.50 1 calc PR A 2 H12Q H 0.3706 0.1851 -0.0393 0.144 Uiso 0.50 1 calc PR A 2 H12R H 0.3153 0.2361 -0.0815 0.144 Uiso 0.50 1 calc PR A 2 C20A C 0.0755(17) 0.0517(13) 0.1192(17) 0.066(6) Uiso 0.25 1 d P . 1 H20A H 0.0983 0.0854 0.1473 0.099 Uiso 0.25 1 calc PR . 1 H20B H 0.0178 0.0480 0.1149 0.099 Uiso 0.25 1 calc PR . 1 H20C H 0.0755 0.0499 0.0572 0.099 Uiso 0.25 1 calc PR . 1 C20B C 0.0639(18) 0.0268(12) 0.1037(19) 0.080(8) Uiso 0.25 1 d P . 1 H20D H 0.0689 0.0648 0.1095 0.121 Uiso 0.25 1 calc PR . 1 H20E H 0.0098 0.0158 0.1040 0.121 Uiso 0.25 1 calc PR . 1 H20F H 0.0671 0.0160 0.0455 0.121 Uiso 0.25 1 calc PR . 1 C20C C 0.1484(19) 0.0390(12) 0.310(2) 0.093(8) Uiso 0.25 1 d P . 1 H20G H 0.2069 0.0495 0.3453 0.140 Uiso 0.25 1 calc PR . 1 H20H H 0.1300 0.0158 0.3473 0.140 Uiso 0.25 1 calc PR . 1 H20I H 0.1125 0.0700 0.2928 0.140 Uiso 0.25 1 calc PR . 1 C21A C 0.447(2) 0.0815(15) 0.295(2) 0.082(8) Uiso 0.25 1 d P . 1 H21A H 0.4704 0.1154 0.3218 0.124 Uiso 0.25 1 calc PR . 1 H21B H 0.4601 0.0749 0.2409 0.124 Uiso 0.25 1 calc PR . 1 H21C H 0.4729 0.0541 0.3413 0.124 Uiso 0.25 1 calc PR . 1 C22A C 0.3973(15) 0.0157(9) 0.4256(15) 0.074(6) Uiso 0.25 1 d P . 2 H22A H 0.3586 -0.0083 0.4373 0.111 Uiso 0.25 1 calc PR . 2 H22B H 0.3779 0.0516 0.4253 0.111 Uiso 0.25 1 calc PR . 2 H22C H 0.4539 0.0118 0.4743 0.111 Uiso 0.25 1 calc PR . 2 C22B C 0.473(2) 0.0537(15) 0.297(2) 0.083(8) Uiso 0.25 1 d P . 2 H22D H 0.4499 0.0880 0.3006 0.125 Uiso 0.25 1 calc PR . 2 H22E H 0.4784 0.0502 0.2376 0.125 Uiso 0.25 1 calc PR . 2 H22F H 0.5292 0.0503 0.3475 0.125 Uiso 0.25 1 calc PR . 2 C26A C 0.243(3) 0.1332(17) 0.154(3) 0.124(12) Uiso 0.25 1 d P . 3 H26A H 0.1844 0.1244 0.1394 0.186 Uiso 0.25 1 calc PR . 3 H26B H 0.2555 0.1281 0.0990 0.186 Uiso 0.25 1 calc PR . 3 H26C H 0.2536 0.1696 0.1739 0.186 Uiso 0.25 1 calc PR . 3 C26B C 0.410(3) 0.094(2) 0.290(3) 0.139(17) Uiso 0.25 1 d P . 3 H26D H 0.4306 0.0927 0.2400 0.208 Uiso 0.25 1 calc PR . 3 H26E H 0.4341 0.0655 0.3327 0.208 Uiso 0.25 1 calc PR . 3 H26F H 0.4278 0.1275 0.3229 0.208 Uiso 0.25 1 calc PR . 3 C26C C 0.329(3) 0.0970(18) 0.371(3) 0.129(13) Uiso 0.25 1 d P . 3 H26G H 0.2743 0.0958 0.3761 0.193 Uiso 0.25 1 calc PR . 3 H26H H 0.3566 0.1302 0.3951 0.193 Uiso 0.25 1 calc PR . 3 H26I H 0.3642 0.0682 0.4063 0.193 Uiso 0.25 1 calc PR . 3 C29A C 0.0924(15) 0.0803(11) 0.1247(15) 0.061(5) Uiso 0.25 1 d P . 4 H29A H 0.0685 0.0590 0.0686 0.092 Uiso 0.25 1 calc PR . 4 H29B H 0.1152 0.1126 0.1109 0.092 Uiso 0.25 1 calc PR . 4 H29C H 0.0484 0.0886 0.1467 0.092 Uiso 0.25 1 calc PR . 4 C29B C 0.209(3) 0.0958(17) 0.310(3) 0.134(13) Uiso 0.25 1 d P . 4 H29D H 0.2560 0.0783 0.3596 0.200 Uiso 0.25 1 calc PR . 4 H29E H 0.1647 0.1034 0.3323 0.200 Uiso 0.25 1 calc PR . 4 H29F H 0.2290 0.1284 0.2938 0.200 Uiso 0.25 1 calc PR . 4 C29C C 0.1371(13) 0.0000 0.3051(14) 0.089(5) Uiso 0.50 2 d SP . 4 H29G H 0.1897 -0.0158 0.3481 0.133 Uiso 0.25 1 calc PR . 4 H29H H 0.0969 -0.0275 0.2728 0.133 Uiso 0.25 1 calc PR . 4 H29I H 0.1133 0.0219 0.3395 0.133 Uiso 0.25 1 calc PR . 4 C25A C 0.4852(18) 0.0257(13) 0.291(2) 0.096(9) Uiso 0.25 1 d P . 5 H25A H 0.4857 0.0268 0.2292 0.145 Uiso 0.25 1 calc PR . 5 H25B H 0.4889 -0.0105 0.3119 0.145 Uiso 0.25 1 calc PR . 5 H25C H 0.5333 0.0454 0.3342 0.145 Uiso 0.25 1 calc PR . 5 C25B C 0.382(4) 0.057(2) 0.410(4) 0.19(2) Uiso 0.25 1 d P . 5 H25D H 0.3320 0.0721 0.4139 0.279 Uiso 0.25 1 calc PR . 5 H25E H 0.4322 0.0760 0.4494 0.279 Uiso 0.25 1 calc PR . 5 H25F H 0.3872 0.0202 0.4303 0.279 Uiso 0.25 1 calc PR . 5 C25C C 0.330(2) 0.1301(15) 0.202(3) 0.109(10) Uiso 0.25 1 d P . 5 H25G H 0.3312 0.1241 0.1412 0.163 Uiso 0.25 1 calc PR . 5 H25H H 0.3674 0.1591 0.2327 0.163 Uiso 0.25 1 calc PR . 5 H25I H 0.2723 0.1386 0.1942 0.163 Uiso 0.25 1 calc PR . 5 C28A C 0.2737(18) 0.1094(11) 0.3343(18) 0.078(6) Uiso 0.25 1 d P . 6 H28A H 0.2456 0.0871 0.3636 0.116 Uiso 0.25 1 calc PR . 6 H28B H 0.2617 0.1460 0.3419 0.116 Uiso 0.25 1 calc PR . 6 H28C H 0.3346 0.1035 0.3633 0.116 Uiso 0.25 1 calc PR . 6 C28B C 0.125(2) 0.1056(15) 0.137(2) 0.101(9) Uiso 0.25 1 d P . 6 H28D H 0.0903 0.0827 0.1577 0.152 Uiso 0.25 1 calc PR . 6 H28E H 0.1126 0.0990 0.0721 0.152 Uiso 0.25 1 calc PR . 6 H28F H 0.1122 0.1421 0.1453 0.152 Uiso 0.25 1 calc PR . 6 C28C C 0.2911(16) 0.1373(9) 0.1610(16) 0.057(5) Uiso 0.25 1 d P . 6 H28G H 0.3516 0.1331 0.1972 0.086 Uiso 0.25 1 calc PR . 6 H28H H 0.2748 0.1734 0.1662 0.086 Uiso 0.25 1 calc PR . 6 H28I H 0.2780 0.1293 0.0960 0.086 Uiso 0.25 1 calc PR . 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0281(4) 0.0620(7) 0.0410(5) 0.000 0.0147(4) 0.000 Ge1 0.0408(2) 0.0607(3) 0.0440(2) 0.0102(2) 0.01794(19) 0.0061(2) Ge2 0.0421(3) 0.0730(5) 0.0367(3) 0.000 0.0229(3) 0.000 Ge3 0.0358(3) 0.0557(4) 0.0339(3) 0.000 0.0182(2) 0.000 Ge4 0.0365(2) 0.0536(3) 0.0356(2) -0.00199(17) 0.01727(17) -0.00001(18) Ge5 0.0440(3) 0.0755(4) 0.0495(3) 0.0045(2) 0.0263(2) 0.0137(2) Ge6 0.0397(3) 0.0750(5) 0.0387(3) 0.000 0.0083(3) 0.000 Si1 0.0513(7) 0.0561(8) 0.0375(6) 0.0073(5) 0.0169(5) 0.0108(6) Si2 0.0455(9) 0.0786(13) 0.0378(8) 0.000 0.0263(7) 0.000 Si10 0.0915(11) 0.0932(13) 0.0382(7) 0.0116(7) 0.0290(7) 0.0236(9) Si11 0.0658(9) 0.0785(11) 0.0683(9) 0.0019(8) 0.0226(7) 0.0292(8) Si12 0.0649(9) 0.0633(10) 0.0676(9) 0.0085(7) 0.0232(7) -0.0008(7) C11B 0.056(3) 0.123(6) 0.089(4) -0.010(4) 0.020(3) 0.022(4) C10C 0.22(4) 0.080(14) 0.052(11) -0.014(8) 0.074(18) -0.022(19) C10B 0.136(15) 0.12(3) 0.063(11) 0.010(11) 0.009(9) -0.046(15) C10A 0.093(14) 0.27(4) 0.081(11) -0.054(19) 0.047(10) 0.018(18) C11A 0.18(4) 0.15(4) 0.18(4) 0.03(3) 0.11(3) 0.07(3) C11C 0.112(19) 0.092(13) 0.068(10) -0.042(9) 0.055(12) 0.003(11) C12C 0.106(14) 0.09(2) 0.072(9) -0.056(16) 0.028(9) -0.019(17) C12B 0.122(15) 0.039(12) 0.131(14) 0.038(11) 0.069(12) 0.016(10) C12A 0.045(9) 0.09(3) 0.111(15) 0.019(14) 0.026(9) 0.023(14) C10F 0.120(15) 0.13(3) 0.066(11) -0.041(12) 0.014(10) 0.007(15) C10E 0.41(7) 0.117(19) 0.057(15) 0.015(15) 0.10(3) -0.08(4) C10D 0.113(17) 0.19(2) 0.048(8) -0.006(11) 0.023(9) 0.093(17) C11D 0.094(17) 0.078(14) 0.14(2) 0.040(15) 0.033(16) 0.055(13) C11F 0.081(18) 0.19(3) 0.16(3) -0.02(2) 0.033(16) 0.06(2) C12D 0.06(2) 0.067(18) 0.16(3) 0.010(16) 0.015(16) 0.009(16) C12E 0.097(14) 0.026(10) 0.148(16) 0.022(10) 0.012(11) 0.005(9) C12F 0.107(15) 0.064(16) 0.087(17) -0.042(11) 0.006(11) -0.027(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Ge3 2.6807(13) . ? Zn1 Ge3 2.6807(13) 5_655 ? Zn1 Ge4 2.7152(6) 2_655 ? Zn1 Ge4 2.7152(6) 5_655 ? Zn1 Ge4 2.7152(6) 6 ? Zn1 Ge4 2.7152(6) . ? Ge1 Si1 2.3810(14) . ? Ge1 Ge3 2.5056(7) . ? Ge1 Ge4 2.5069(11) . ? Ge1 Ge6 2.5564(9) . ? Ge1 Ge5 2.5622(8) . ? Ge2 Si2 2.3675(17) . ? Ge2 Ge4 2.5025(7) 6 ? Ge2 Ge4 2.5025(7) . ? Ge2 Ge5 2.5472(11) 6 ? Ge2 Ge5 2.5472(11) . ? Ge3 Ge1 2.5056(7) 6 ? Ge3 Ge4 2.8675(8) . ? Ge3 Ge4 2.8675(8) 6 ? Ge5 Ge6 2.6291(9) . ? Ge5 Ge5 2.6765(13) 6 ? Ge6 Ge1 2.5564(9) 6 ? Ge6 Ge5 2.6291(9) 6 ? Si1 Si12 2.346(2) . ? Si1 Si10 2.3537(19) . ? Si1 Si11 2.355(2) . ? Si2 Si22 2.200(11) . ? Si2 Si27 2.263(9) . ? Si2 Si27 2.263(9) 6 ? Si2 Si20 2.272(11) . ? Si2 Si25 2.305(9) . ? Si2 Si25 2.305(9) 6 ? Si2 Si29 2.310(10) 6 ? Si2 Si29 2.310(10) . ? Si2 Si24 2.317(9) . ? Si2 Si24 2.317(9) 6 ? Si2 Si23 2.414(11) 6 ? Si20 C20B 1.62(3) 6 ? Si20 C20B 1.62(3) . ? Si20 C20A 1.80(3) 6 ? Si20 C20A 1.80(3) . ? Si20 C20C 2.10(3) . ? Si20 C20C 2.10(3) 6 ? Si21 C21A 1.64(4) . ? Si22 C22A 1.92(2) . ? Si22 C22A 1.92(2) 6 ? Si22 C22B 1.93(3) 6 ? Si22 C22B 1.93(3) . ? Si24 Si24 1.08(3) 6 ? Si26 C26B 1.56(5) . ? Si26 C26A 1.84(4) . ? Si26 C26C 1.86(4) . ? Si27 Si27 1.21(3) 6 ? Si29 C29A 1.54(2) . ? Si29 C29B 1.99(4) . ? Si29 C29C 2.28(2) . ? Si29 Si29 2.55(3) 6 ? Si25 C25B 1.88(6) . ? Si25 C25A 2.12(3) . ? Si25 C25C 2.20(4) . ? Si28 C28B 1.77(3) . ? Si28 C28C 1.83(3) . ? Si28 C28A 1.92(3) . ? Si10 C10C 1.79(4) . ? Si10 C10B 1.80(4) . ? Si10 C10A 1.85(2) . ? Si10 C10F 1.88(4) . ? Si10 C10E 1.89(4) . ? Si10 C10D 1.892(19) . ? Si11 C11F 1.82(3) . ? Si11 C11B 1.867(8) . ? Si11 C11A 1.87(6) . ? Si11 C11D 1.89(4) . ? Si11 C11C 1.901(17) . ? Si12 C12D 1.70(5) . ? Si12 C12F 1.72(4) . ? Si12 C12E 1.76(3) . ? Si12 C12A 1.99(5) . ? Si12 C12C 1.99(3) . ? Si12 C12B 2.00(2) . ? 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 Ge3 Zn1 Ge3 180.0 . 5_655 ? Ge3 Zn1 Ge4 115.80(2) . 2_655 ? Ge3 Zn1 Ge4 64.20(2) 5_655 2_655 ? Ge3 Zn1 Ge4 115.80(2) . 5_655 ? Ge3 Zn1 Ge4 64.20(2) 5_655 5_655 ? Ge4 Zn1 Ge4 65.74(2) 2_655 5_655 ? Ge3 Zn1 Ge4 64.20(2) . 6 ? Ge3 Zn1 Ge4 115.80(2) 5_655 6 ? Ge4 Zn1 Ge4 180.000(17) 2_655 6 ? Ge4 Zn1 Ge4 114.26(2) 5_655 6 ? Ge3 Zn1 Ge4 64.20(2) . . ? Ge3 Zn1 Ge4 115.80(2) 5_655 . ? Ge4 Zn1 Ge4 114.26(2) 2_655 . ? Ge4 Zn1 Ge4 180.00(2) 5_655 . ? Ge4 Zn1 Ge4 65.74(2) 6 . ? Si1 Ge1 Ge3 124.14(4) . . ? Si1 Ge1 Ge4 126.49(4) . . ? Ge3 Ge1 Ge4 69.79(3) . . ? Si1 Ge1 Ge6 115.87(4) . . ? Ge3 Ge1 Ge6 85.42(3) . . ? Ge4 Ge1 Ge6 116.66(3) . . ? Si1 Ge1 Ge5 118.68(4) . . ? Ge3 Ge1 Ge5 116.87(3) . . ? Ge4 Ge1 Ge5 78.97(3) . . ? Ge6 Ge1 Ge5 61.81(3) . . ? Si2 Ge2 Ge4 125.45(4) . 6 ? Si2 Ge2 Ge4 125.45(4) . . ? Ge4 Ge2 Ge4 72.16(3) 6 . ? Si2 Ge2 Ge5 118.19(4) . 6 ? Ge4 Ge2 Ge5 79.34(3) 6 6 ? Ge4 Ge2 Ge5 115.70(3) . 6 ? Si2 Ge2 Ge5 118.19(4) . . ? Ge4 Ge2 Ge5 115.70(3) 6 . ? Ge4 Ge2 Ge5 79.34(3) . . ? Ge5 Ge2 Ge5 63.39(4) 6 . ? Ge1 Ge3 Ge1 92.17(3) 6 . ? Ge1 Ge3 Zn1 111.98(2) 6 . ? Ge1 Ge3 Zn1 111.98(2) . . ? Ge1 Ge3 Ge4 99.71(3) 6 . ? Ge1 Ge3 Ge4 55.13(3) . . ? Zn1 Ge3 Ge4 58.48(2) . . ? Ge1 Ge3 Ge4 55.13(3) 6 6 ? Ge1 Ge3 Ge4 99.71(3) . 6 ? Zn1 Ge3 Ge4 58.48(2) . 6 ? Ge4 Ge3 Ge4 61.85(3) . 6 ? Ge2 Ge4 Ge1 95.95(3) . . ? Ge2 Ge4 Zn1 108.11(2) . . ? Ge1 Ge4 Zn1 110.80(3) . . ? Ge2 Ge4 Ge3 99.80(3) . . ? Ge1 Ge4 Ge3 55.08(2) . . ? Zn1 Ge4 Ge3 57.32(3) . . ? Ge2 Ge5 Ge1 93.49(3) . . ? Ge2 Ge5 Ge6 102.69(3) . . ? Ge1 Ge5 Ge6 58.98(3) . . ? Ge2 Ge5 Ge5 58.307(19) . 6 ? Ge1 Ge5 Ge5 100.497(18) . 6 ? Ge6 Ge5 Ge5 59.402(16) . 6 ? Ge1 Ge6 Ge1 89.84(4) . 6 ? Ge1 Ge6 Ge5 59.20(3) . . ? Ge1 Ge6 Ge5 101.93(4) 6 . ? Ge1 Ge6 Ge5 101.94(4) . 6 ? Ge1 Ge6 Ge5 59.20(3) 6 6 ? Ge5 Ge6 Ge5 61.20(3) . 6 ? Si12 Si1 Si10 112.19(8) . . ? Si12 Si1 Si11 113.40(9) . . ? Si10 Si1 Si11 110.59(8) . . ? Si12 Si1 Ge1 107.30(6) . . ? Si10 Si1 Ge1 106.52(7) . . ? Si11 Si1 Ge1 106.36(7) . . ? Si22 Si2 Si27 15.5(3) . . ? Si22 Si2 Si27 15.5(3) . 6 ? Si27 Si2 Si27 31.1(6) . 6 ? Si22 Si2 Si20 135.4(4) . . ? Si27 Si2 Si20 133.6(3) . . ? Si27 Si2 Si20 133.6(3) 6 . ? Si22 Si2 Si25 41.3(4) . . ? Si27 Si2 Si25 25.7(4) . . ? Si27 Si2 Si25 56.8(6) 6 . ? Si20 Si2 Si25 121.3(3) . . ? Si22 Si2 Si25 41.3(4) . 6 ? Si27 Si2 Si25 56.8(6) . 6 ? Si27 Si2 Si25 25.7(4) 6 6 ? Si20 Si2 Si25 121.3(3) . 6 ? Si25 Si2 Si25 82.5(8) . 6 ? Si22 Si2 Si29 123.3(4) . 6 ? Si27 Si2 Si29 133.0(4) . 6 ? Si27 Si2 Si29 112.7(4) 6 6 ? Si20 Si2 Si29 33.7(4) . 6 ? Si25 Si2 Si29 139.8(4) . 6 ? Si25 Si2 Si29 92.0(5) 6 6 ? Si22 Si2 Si29 123.3(4) . . ? Si27 Si2 Si29 112.7(4) . . ? Si27 Si2 Si29 133.0(4) 6 . ? Si20 Si2 Si29 33.7(4) . . ? Si25 Si2 Si29 92.0(5) . . ? Si25 Si2 Si29 139.8(4) 6 . ? Si29 Si2 Si29 67.0(8) 6 . ? Si22 Si2 Si24 135.0(3) . . ? Si27 Si2 Si24 128.5(4) . . ? Si27 Si2 Si24 138.4(3) 6 . ? Si20 Si2 Si24 13.5(4) . . ? Si25 Si2 Si24 111.3(4) . . ? Si25 Si2 Si24 132.1(4) 6 . ? Si29 Si2 Si24 47.3(7) 6 . ? Si29 Si2 Si24 20.6(4) . . ? Si22 Si2 Si24 135.0(3) . 6 ? Si27 Si2 Si24 138.4(3) . 6 ? Si27 Si2 Si24 128.5(4) 6 6 ? Si20 Si2 Si24 13.5(4) . 6 ? Si25 Si2 Si24 132.1(4) . 6 ? Si25 Si2 Si24 111.3(4) 6 6 ? Si29 Si2 Si24 20.6(4) 6 6 ? Si29 Si2 Si24 47.3(7) . 6 ? Si24 Si2 Si24 27.0(7) . 6 ? Si22 Si2 Ge2 112.3(3) . . ? Si27 Si2 Ge2 111.1(2) . . ? Si27 Si2 Ge2 111.1(2) 6 . ? Si20 Si2 Ge2 112.3(3) . . ? Si25 Si2 Ge2 107.8(2) . . ? Si25 Si2 Ge2 107.8(2) 6 . ? Si29 Si2 Ge2 111.8(3) 6 . ? Si29 Si2 Ge2 111.8(3) . . ? Si24 Si2 Ge2 110.5(2) . . ? Si24 Si2 Ge2 110.5(2) 6 . ? Si22 Si2 Si23 113.8(3) . 6 ? Si27 Si2 Si23 127.6(4) . 6 ? Si27 Si2 Si23 100.0(5) 6 6 ? Si20 Si2 Si23 54.6(4) . 6 ? Si25 Si2 Si23 146.3(4) . 6 ? Si25 Si2 Si23 76.0(5) 6 6 ? Si29 Si2 Si23 21.1(4) 6 6 ? Si29 Si2 Si23 88.1(7) . 6 ? Si24 Si2 Si23 68.1(6) . 6 ? Si24 Si2 Si23 41.1(4) 6 6 ? Ge2 Si2 Si23 103.4(3) . 6 ? C20B Si20 C20B 50(2) 6 . ? C20B Si20 C20A 22.3(12) 6 6 ? C20B Si20 C20A 72.7(19) . 6 ? C20B Si20 C20A 72.7(19) 6 . ? C20B Si20 C20A 22.3(12) . . ? C20A Si20 C20A 95(2) 6 . ? C20B Si20 C20C 134.6(14) 6 . ? C20B Si20 C20C 107.2(14) . . ? C20A Si20 C20C 135.4(13) 6 . ? C20A Si20 C20C 90.5(13) . . ? C20B Si20 C20C 107.2(14) 6 6 ? C20B Si20 C20C 134.6(14) . 6 ? C20A Si20 C20C 90.5(13) 6 6 ? C20A Si20 C20C 135.4(13) . 6 ? C20C Si20 C20C 57.1(18) . 6 ? C20B Si20 Si2 120.9(11) 6 . ? C20B Si20 Si2 120.9(11) . . ? C20A Si20 Si2 113.4(10) 6 . ? C20A Si20 Si2 113.4(10) . . ? C20C Si20 Si2 104.6(9) . . ? C20C Si20 Si2 104.6(9) 6 . ? C21A Si21 Si2 115.4(14) . . ? C22A Si22 C22A 24.3(14) . 6 ? C22A Si22 C22B 120.6(12) . 6 ? C22A Si22 C22B 102.0(12) 6 6 ? C22A Si22 C22B 102.0(12) . . ? C22A Si22 C22B 120.6(12) 6 . ? C22B Si22 C22B 91(2) 6 . ? C22A Si22 Si2 111.8(9) . . ? C22A Si22 Si2 111.8(9) 6 . ? C22B Si22 Si2 114.3(10) 6 . ? C22B Si22 Si2 114.3(10) . . ? Si24 Si24 Si2 76.5(4) 6 . ? C26B Si26 C26A 123(2) . . ? C26B Si26 C26C 82(2) . . ? C26A Si26 C26C 125(2) . . ? C26B Si26 Si2 108(2) . . ? C26A Si26 Si2 107.1(15) . . ? C26C Si26 Si2 109.4(15) . . ? Si27 Si27 Si2 74.5(3) 6 . ? C29A Si29 C29B 106.7(17) . . ? C29A Si29 C29C 121.0(13) . . ? C29B Si29 C29C 79.7(14) . . ? C29A Si29 Si2 132.4(10) . . ? C29B Si29 Si2 107.9(13) . . ? C29C Si29 Si2 96.6(6) . . ? C29A Si29 Si29 120.6(12) . 6 ? C29B Si29 Si29 126.5(13) . 6 ? C29C Si29 Si29 55.9(4) . 6 ? Si2 Si29 Si29 56.5(4) . 6 ? C25B Si25 C25A 104(2) . . ? C25B Si25 C25C 122(2) . . ? C25A Si25 C25C 115.6(14) . . ? C25B Si25 Si2 110.8(19) . . ? C25A Si25 Si2 101.6(10) . . ? C25C Si25 Si2 100.7(11) . . ? C28B Si28 C28C 105.7(15) . . ? C28B Si28 C28A 116.7(15) . . ? C28C Si28 C28A 104.0(12) . . ? C28B Si28 Si2 113.0(13) . . ? C28C Si28 Si2 111.4(9) . . ? C28A Si28 Si2 105.7(10) . . ? C10C Si10 C10B 105.6(15) . . ? C10C Si10 C10A 114.7(15) . . ? C10B Si10 C10A 104.4(18) . . ? C10C Si10 C10F 15(2) . . ? C10B Si10 C10F 95.9(16) . . ? C10A Si10 C10F 129.7(14) . . ? C10C Si10 C10E 118.9(15) . . ? C10B Si10 C10E 15(2) . . ? C10A Si10 C10E 92(2) . . ? C10F Si10 C10E 110.2(18) . . ? C10C Si10 C10D 85.5(15) . . ? C10B Si10 C10D 123.6(18) . . ? C10A Si10 C10D 30.5(12) . . ? C10F Si10 C10D 101.0(14) . . ? C10E Si10 C10D 116(2) . . ? C10C Si10 Si1 114.4(8) . . ? C10B Si10 Si1 111.9(16) . . ? C10A Si10 Si1 105.5(7) . . ? C10F Si10 Si1 108.6(10) . . ? C10E Si10 Si1 108.5(14) . . ? C10D Si10 Si1 112.6(6) . . ? C11F Si11 C11B 110.9(14) . . ? C11F Si11 C11A 100(3) . . ? C11B Si11 C11A 111(2) . . ? C11F Si11 C11D 110(3) . . ? C11B Si11 C11D 105.8(18) . . ? C11A Si11 C11D 9(5) . . ? C11F Si11 C11C 7(2) . . ? C11B Si11 C11C 106.5(10) . . ? C11A Si11 C11C 107(3) . . ? C11D Si11 C11C 116(2) . . ? C11F Si11 Si1 111.9(9) . . ? C11B Si11 Si1 111.2(2) . . ? C11A Si11 Si1 111(2) . . ? C11D Si11 Si1 107.1(16) . . ? C11C Si11 Si1 109.9(9) . . ? C12D Si12 C12F 106(3) . . ? C12D Si12 C12E 99(2) . . ? C12F Si12 C12E 121.3(15) . . ? C12D Si12 C12A 6(3) . . ? C12F Si12 C12A 104(2) . . ? C12E Si12 C12A 105.4(16) . . ? C12D Si12 C12C 111(3) . . ? C12F Si12 C12C 11(2) . . ? C12E Si12 C12C 109.8(15) . . ? C12A Si12 C12C 110(2) . . ? C12D Si12 C12B 112(2) . . ? C12F Si12 C12B 109.0(15) . . ? C12E Si12 C12B 14.5(13) . . ? C12A Si12 C12B 118.0(15) . . ? C12C Si12 C12B 97.5(15) . . ? C12D Si12 Si1 112(2) . . ? C12F Si12 Si1 107.8(14) . . ? C12E Si12 Si1 109.6(10) . . ? C12A Si12 Si1 107.8(17) . . ? C12C Si12 Si1 113.7(12) . . ? C12B Si12 Si1 109.5(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.922 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.086