# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dehnen, Stefanie' _publ_contact_author_email dehnen@chemie.uni-marburg.de loop_ _publ_author_name S.Dehnen S.Heimann data_1a _database_code_depnum_ccdc_archive 'CCDC 794768' #TrackingRef '- 1a_monoclinic_twin.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C24 H44 Ge4 O4 Te6' _chemical_formula_sum 'C24 H44 Ge4 O4 Te6' _chemical_formula_weight 1452.55 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.633(4) _cell_length_b 13.033(5) _cell_length_c 17.361(6) _cell_angle_alpha 90.00 _cell_angle_beta 131.78(5) _cell_angle_gamma 90.00 _cell_volume 1962.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1490 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 29.62 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 7.429 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details ? _exptl_special_details ; Space group choice was not unambiguous in this case due to twinning problems (see section on refinement special details). Only in P2~1~/c space group a reasonable structure model was found. ; _diffrn_ambient_temperature 100(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 IPDS2 _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1490 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6804 _reflns_number_gt 4517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe, X-Area ver. 1.54' _computing_cell_refinement 'Stoe, X-Area ver. 1.54' _computing_data_reduction 'Stoe, X-Area ver. 1.54' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Two main twin domains could be assigned, related by the following twin law (by rows): 0.99647 -0.00410 -0.00517, 1.01240 0.01127 1.01155, -0.98155 -0.98532 0.01632. This was taken into account during data integration and HKLF5 file was generated. DFIX restraint (1.50(2) /%A) was used for all C-C distances. For all C atoms displacement parameters also SIMU/DELU restraints were used. On the final difference Fourier map the highest peak of 3.64 e//%A^3^ was located 0.03 /%A from Te6 atom (the deepest hole of -1.70 e//%A^3^ was located 0.86 /%A from Te6 atom). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.099(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6804 _refine_ls_number_parameters 174 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.1115 _refine_ls_wR_factor_ref 0.2938 _refine_ls_wR_factor_gt 0.2688 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.083 _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 Te1 Te 0.21512(11) -0.02982(8) 0.00009(8) 0.0375(4) Uani 1 1 d U . . Te2 Te 0.46883(12) 0.21325(8) -0.00199(8) 0.0372(5) Uani 1 1 d U . . Te6 Te 0.71347(12) 0.01755(8) 0.21741(8) 0.0372(5) Uani 1 1 d U . . Ge4 Ge 0.44375(18) 0.09618(12) 0.10713(12) 0.0354(5) Uani 1 1 d U . . Ge5 Ge 0.26624(19) -0.12903(12) -0.10358(12) 0.0349(5) Uani 1 1 d U . . O1 O 0.5379(16) 0.0004(9) 0.2920(10) 0.043(2) Uani 1 1 d U . . O2 O 0.2807(16) -0.3251(13) -0.0080(11) 0.054(3) Uani 1 1 d U . . C1 C 0.030(2) -0.2666(12) -0.1476(15) 0.042(3) Uani 1 1 d U . . H1A H -0.0606 -0.3106 -0.1981 0.051 Uiso 1 1 calc R . . H1B H -0.0032 -0.2120 -0.1266 0.051 Uiso 1 1 calc R . . C2 C 0.4016(18) 0.1928(11) 0.1774(12) 0.040(3) Uani 1 1 d DU . . C3 C 0.449(2) 0.0443(14) 0.2955(12) 0.040(3) Uani 1 1 d U . . C4 C 0.0727(17) -0.2162(10) -0.2030(13) 0.039(3) Uani 1 1 d DU . . C5 C 0.343(2) 0.1288(11) 0.2254(14) 0.043(3) Uani 1 1 d U . . H5A H 0.3314 0.1764 0.2640 0.051 Uiso 1 1 calc R . . H5B H 0.2406 0.0994 0.1681 0.051 Uiso 1 1 calc R . . C6 C 0.548(2) 0.2504(12) 0.2606(14) 0.049(4) Uani 1 1 d DU . . H6A H 0.5290 0.2988 0.2943 0.073 Uiso 1 1 calc R . . H6B H 0.5815 0.2881 0.2297 0.073 Uiso 1 1 calc R . . H6C H 0.6284 0.2017 0.3118 0.073 Uiso 1 1 calc R . . C7 C 0.104(2) -0.2968(11) -0.2497(13) 0.042(3) Uani 1 1 d DU . . H7A H 0.0109 -0.3384 -0.2987 0.063 Uiso 1 1 calc R . . H7B H 0.1887 -0.3409 -0.1948 0.063 Uiso 1 1 calc R . . H7C H 0.1316 -0.2633 -0.2858 0.063 Uiso 1 1 calc R . . C8 C 0.270(2) 0.2643(14) 0.0942(14) 0.046(4) Uani 1 1 d DU . . H8A H 0.2478 0.3128 0.1262 0.068 Uiso 1 1 calc R . . H8B H 0.1772 0.2235 0.0422 0.068 Uiso 1 1 calc R . . H8C H 0.2996 0.3021 0.0612 0.068 Uiso 1 1 calc R . . C10 C -0.055(2) -0.1443(13) -0.2841(13) 0.045(4) Uani 1 1 d DU . . H10A H -0.1504 -0.1835 -0.3342 0.068 Uiso 1 1 calc R . . H10B H -0.0269 -0.1102 -0.3197 0.068 Uiso 1 1 calc R . . H10C H -0.0712 -0.0927 -0.2510 0.068 Uiso 1 1 calc R . . C22 C 0.424(3) 0.0068(13) 0.3688(14) 0.046(4) Uani 1 1 d U . . H22A H 0.4911 -0.0519 0.4094 0.069 Uiso 1 1 calc R . . H22B H 0.3158 -0.0139 0.3275 0.069 Uiso 1 1 calc R . . H22C H 0.4479 0.0626 0.4155 0.069 Uiso 1 1 calc R . . C33 C 0.095(2) -0.4014(19) -0.0141(14) 0.053(5) Uani 1 1 d U . . H33A H 0.1827 -0.4411 0.0446 0.079 Uiso 1 1 calc R . . H33B H 0.0166 -0.4483 -0.0693 0.079 Uiso 1 1 calc R . . H33C H 0.0508 -0.3605 0.0081 0.079 Uiso 1 1 calc R . . C44 C 0.149(2) -0.3313(12) -0.0533(17) 0.049(4) Uani 1 1 d U . . 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 Te1 0.0333(6) 0.0391(6) 0.0432(6) -0.0018(4) 0.0268(5) -0.0016(4) Te2 0.0335(6) 0.0373(6) 0.0411(6) 0.0030(4) 0.0250(5) 0.0016(4) Te6 0.0337(6) 0.0374(6) 0.0396(6) 0.0031(4) 0.0241(5) 0.0023(4) Ge4 0.0311(9) 0.0359(8) 0.0381(8) 0.0003(6) 0.0226(7) 0.0007(6) Ge5 0.0309(9) 0.0376(8) 0.0369(8) 0.0004(6) 0.0228(7) -0.0001(6) O1 0.055(6) 0.031(4) 0.056(6) -0.013(5) 0.043(6) -0.008(4) O2 0.046(6) 0.071(9) 0.049(6) 0.015(6) 0.033(6) 0.000(6) C1 0.035(7) 0.031(6) 0.061(8) -0.002(6) 0.033(6) -0.002(5) C2 0.048(8) 0.033(6) 0.045(7) 0.007(4) 0.033(6) 0.007(5) C3 0.047(8) 0.050(7) 0.031(6) 0.008(6) 0.029(6) 0.008(6) C4 0.032(7) 0.024(5) 0.056(7) -0.001(4) 0.028(6) 0.000(5) C5 0.059(9) 0.028(6) 0.045(7) 0.010(5) 0.036(7) 0.005(5) C6 0.050(8) 0.031(7) 0.054(8) 0.002(6) 0.030(7) 0.008(6) C7 0.044(9) 0.030(6) 0.046(7) -0.001(5) 0.028(7) -0.003(5) C8 0.051(8) 0.046(8) 0.049(7) 0.020(7) 0.037(7) 0.020(7) C10 0.045(7) 0.046(8) 0.044(7) 0.003(6) 0.030(6) 0.005(6) C22 0.076(12) 0.035(6) 0.048(8) 0.019(6) 0.050(9) 0.012(7) C33 0.042(9) 0.078(12) 0.042(7) 0.001(8) 0.029(7) -0.014(8) C44 0.051(7) 0.025(6) 0.066(9) 0.003(6) 0.037(7) -0.010(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 Te1 Ge4 2.576(2) . ? Te1 Ge5 2.587(2) . ? Te2 Ge5 2.556(2) 3_655 ? Te2 Ge4 2.596(2) . ? Te6 Ge4 2.560(2) . ? Te6 Ge5 2.587(2) 3_655 ? Ge4 C2 2.028(18) . ? Ge5 C4 2.039(15) . ? Ge5 Te2 2.556(2) 3_655 ? Ge5 Te6 2.587(2) 3_655 ? O1 C3 1.22(2) . ? O2 C44 1.17(3) . ? C1 C4 1.49(3) . ? C1 C44 1.51(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C6 1.507(16) . ? C2 C8 1.534(15) . ? C2 C5 1.61(2) . ? C3 C5 1.49(2) . ? C3 C22 1.56(2) . ? C4 C7 1.510(16) . ? C4 C10 1.511(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C33 C44 1.50(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 Te1 Ge5 102.42(7) . . ? Ge5 Te2 Ge4 83.82(7) 3_655 . ? Ge4 Te6 Ge5 83.92(7) . 3_655 ? C2 Ge4 Te6 117.8(4) . . ? C2 Ge4 Te1 106.4(5) . . ? Te6 Ge4 Te1 116.49(8) . . ? C2 Ge4 Te2 105.3(5) . . ? Te6 Ge4 Te2 95.93(7) . . ? Te1 Ge4 Te2 114.35(8) . . ? C4 Ge5 Te2 119.4(4) . 3_655 ? C4 Ge5 Te1 103.4(5) . . ? Te2 Ge5 Te1 116.23(8) 3_655 . ? C4 Ge5 Te6 106.1(5) . 3_655 ? Te2 Ge5 Te6 96.25(8) 3_655 3_655 ? Te1 Ge5 Te6 115.53(7) . 3_655 ? C4 C1 C44 119.3(15) . . ? C4 C1 H1A 107.5 . . ? C44 C1 H1A 107.5 . . ? C4 C1 H1B 107.5 . . ? C44 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C6 C2 C8 112.5(14) . . ? C6 C2 C5 111.0(15) . . ? C8 C2 C5 107.4(14) . . ? C6 C2 Ge4 108.3(12) . . ? C8 C2 Ge4 107.6(11) . . ? C5 C2 Ge4 110.0(10) . . ? O1 C3 C5 125.0(15) . . ? O1 C3 C22 121.4(15) . . ? C5 C3 C22 113.3(15) . . ? C1 C4 C7 109.8(13) . . ? C1 C4 C10 109.3(14) . . ? C7 C4 C10 111.7(14) . . ? C1 C4 Ge5 110.6(11) . . ? C7 C4 Ge5 108.5(11) . . ? C10 C4 Ge5 106.8(10) . . ? C3 C5 C2 113.8(15) . . ? C3 C5 H5A 108.8 . . ? C2 C5 H5A 108.8 . . ? C3 C5 H5B 108.8 . . ? C2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C44 C33 H33A 109.5 . . ? C44 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C44 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C44 C33 119.5(18) . . ? O2 C44 C1 121.9(17) . . ? C33 C44 C1 118.5(17) . . ? 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 Ge5 Te6 Ge4 C2 -112.9(5) 3_655 . . . ? Ge5 Te6 Ge4 Te1 118.90(8) 3_655 . . . ? Ge5 Te6 Ge4 Te2 -2.09(6) 3_655 . . . ? Ge5 Te1 Ge4 C2 172.2(4) . . . . ? Ge5 Te1 Ge4 Te6 -54.22(9) . . . . ? Ge5 Te1 Ge4 Te2 56.40(8) . . . . ? Ge5 Te2 Ge4 C2 123.1(4) 3_655 . . . ? Ge5 Te2 Ge4 Te6 2.12(6) 3_655 . . . ? Ge5 Te2 Ge4 Te1 -120.51(9) 3_655 . . . ? Ge4 Te1 Ge5 C4 -172.8(4) . . . . ? Ge4 Te1 Ge5 Te2 54.35(9) . . . 3_655 ? Ge4 Te1 Ge5 Te6 -57.35(9) . . . 3_655 ? Te6 Ge4 C2 C6 33.2(12) . . . . ? Te1 Ge4 C2 C6 166.1(10) . . . . ? Te2 Ge4 C2 C6 -72.2(11) . . . . ? Te6 Ge4 C2 C8 155.1(10) . . . . ? Te1 Ge4 C2 C8 -72.0(12) . . . . ? Te2 Ge4 C2 C8 49.7(12) . . . . ? Te6 Ge4 C2 C5 -88.2(10) . . . . ? Te1 Ge4 C2 C5 44.7(10) . . . . ? Te2 Ge4 C2 C5 166.4(9) . . . . ? C44 C1 C4 C7 65(2) . . . . ? C44 C1 C4 C10 -171.9(15) . . . . ? C44 C1 C4 Ge5 -54.6(17) . . . . ? Te2 Ge5 C4 C1 85.4(10) 3_655 . . . ? Te1 Ge5 C4 C1 -45.6(10) . . . . ? Te6 Ge5 C4 C1 -167.6(9) 3_655 . . . ? Te2 Ge5 C4 C7 -35.2(12) 3_655 . . . ? Te1 Ge5 C4 C7 -166.2(10) . . . . ? Te6 Ge5 C4 C7 71.8(10) 3_655 . . . ? Te2 Ge5 C4 C10 -155.8(10) 3_655 . . . ? Te1 Ge5 C4 C10 73.2(12) . . . . ? Te6 Ge5 C4 C10 -48.8(12) 3_655 . . . ? O1 C3 C5 C2 -26(3) . . . . ? C22 C3 C5 C2 161.0(14) . . . . ? C6 C2 C5 C3 -65.8(18) . . . . ? C8 C2 C5 C3 170.9(15) . . . . ? Ge4 C2 C5 C3 54.0(16) . . . . ? C4 C1 C44 O2 18(3) . . . . ? C4 C1 C44 C33 -165.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.777 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.777 _refine_diff_density_max 3.64 _refine_diff_density_min -1.70 _refine_diff_density_rms 0.42 # start Validation Reply Form _vrf_PLAT029_moclabs ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.78 RESPONSE: The dataset was affected by twinning; the apparent presence of additional twin domains required omitting some data in calculations. ; _vrf_PLAT030_moclabs ; PROBLEM: _diffrn_reflns_number .LE. _reflns_number_total RESPONSE: HKLF5 file format was used ; # end Validation Reply Form # Attachment '- 2-rev2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 794769' #TrackingRef '- 2-rev2.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C12 H20 Ge4 O8 Te5, 0.32 (H2O)' _chemical_formula_sum 'C12 H20.64 Ge4 O8.30 Te5' _chemical_formula_weight 1226.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C cca' _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 10.100(3) _cell_length_b 50.56(1) _cell_length_c 12.418(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6341(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17916 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 29.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4376 _exptl_absorpt_coefficient_mu 8.3 _exptl_absorpt_correction_type none _exptl_special_details ; The choice of crystal system was based on Laue symmetry of the diffraction pattern. The chosen space group was in accordance with systematic absences. The presence of the centre of symmetry is confirmed by statistical tests/ structure. ; _diffrn_ambient_temperature 100(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 IPDS2 _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17666 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 63 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.65 _diffrn_reflns_theta_max 26.76 _reflns_number_total 3302 _reflns_number_gt 2098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe, X-Area ver. 1.54' _computing_cell_refinement 'Stoe, X-Area ver. 1.54' _computing_data_reduction 'Stoe, X-Area ver. 1.54' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The structure was found to be non-merohedrally twinned. Better refinement results were achieved when only the main twin domain was taken in data integration. In refinement anti-bumping DFIX restraints were used (-2.70(1) for O1B...O1B at 1.5-x,-y,z distance, -2.00(1) for H2C...H2A at x+0.5,y,1-z distance). DFIX restraint was used for the carboxyl group C1A-O2A bond (1.25(1) /%A). However, due to considerable disorder the relevant C-O bond lengths are not reliable. To afford a fully anisotropic model the following restraints were used: ISOR (for C3B, C1A atoms), EADP (for the following atom pairs: C3B/C3A, O1A/O1B, O2A/O2B, C1A/C1B). On the final difference Fourier map the highest peak of 1.91 e//%A^3^ was located 1.00 /%A from Te2 atom (the deepest hole of -2.07 e//%A^3^ was located 0.93 /%A from Te1 atom). ; _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^)+(0.0660P)^2^+182.8084P] 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 3302 _refine_ls_number_parameters 152 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.004 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 Te1 Te 0.70697(7) 0.120360(16) 0.24690(7) 0.0504(2) Uani 1 1 d . . . Te2 Te 0.98695(7) 0.121096(16) 0.48971(6) 0.0504(2) Uani 1 1 d . . . Te3 Te 1.0000 0.05982(2) 0.2500 0.0551(3) Uani 1 2 d S . . Ge2 Ge 0.85430(11) 0.09072(2) 0.36458(10) 0.0444(3) Uani 1 1 d . A . Ge1 Ge 0.91657(10) 0.14309(2) 0.17833(10) 0.0418(3) Uani 1 1 d . . . C1A C 0.5786(10) 0.0226(13) 0.404(3) 0.061(5) Uani 0.183(13) 1 d PDU A 1 C3A C 0.698(7) 0.0401(14) 0.335(7) 0.069(5) Uani 0.183(13) 1 d P A 1 H3A1 H 0.6610 0.0494 0.2720 0.083 Uiso 0.183(13) 1 calc PR A 1 H3A2 H 0.7723 0.0287 0.3125 0.083 Uiso 0.183(13) 1 calc PR A 1 O1A O 0.584(8) 0.0274(14) 0.485(7) 0.119(5) Uani 0.183(13) 1 d P A 1 O2A O 0.4640(18) 0.0199(13) 0.440(4) 0.107(5) Uani 0.183(13) 1 d PD A 1 H2A H 0.4328 0.0054 0.4198 0.161 Uiso 0.183(13) 1 calc PR A 1 C1B C 0.5782(15) 0.0317(3) 0.4299(16) 0.061(5) Uani 0.817(13) 1 d P A 2 C3B C 0.6385(17) 0.0531(3) 0.3723(16) 0.069(5) Uani 0.817(13) 1 d PU A 2 H3B1 H 0.5720 0.0668 0.3552 0.083 Uiso 0.817(13) 1 calc PR A 2 H3B2 H 0.6778 0.0466 0.3041 0.083 Uiso 0.817(13) 1 calc PR A 2 O1B O 0.6287(16) 0.0186(3) 0.5069(14) 0.119(5) Uani 0.817(13) 1 d PD A 2 O2B O 0.4648(14) 0.0249(3) 0.3945(15) 0.107(5) Uani 0.817(13) 1 d P A 2 H2B H 0.4700 0.0099 0.3655 0.161 Uiso 0.817(13) 1 calc PR A 2 C2 C 0.7507(13) 0.0648(2) 0.4492(12) 0.066(4) Uani 1 1 d . . . H2C H 0.8058 0.0560 0.5047 0.080 Uiso 1 1 calc RD A 1 H2D H 0.6730 0.0731 0.4840 0.080 Uiso 1 1 calc R A 1 C4 C 0.8791(13) 0.1806(2) 0.1410(11) 0.058(3) Uani 1 1 d . . . H4A H 0.8379 0.1894 0.2039 0.070 Uiso 1 1 calc R . . H4B H 0.9638 0.1897 0.1258 0.070 Uiso 1 1 calc R . . C5 C 0.7915(13) 0.1837(2) 0.0478(13) 0.066(4) Uani 1 1 d . . . H5A H 0.7047 0.1753 0.0624 0.079 Uiso 1 1 calc R . . H5B H 0.8310 0.1751 -0.0163 0.079 Uiso 1 1 calc R . . C6 C 0.7738(14) 0.2135(3) 0.0277(18) 0.092(6) Uani 1 1 d . . . O4 O 0.6876(12) 0.2173(2) -0.0590(11) 0.110(4) Uani 1 1 d . . . H4 H 0.6695 0.2335 -0.0647 0.165 Uiso 1 1 calc R . . O5 O 0.8278(12) 0.2306(2) 0.0741(12) 0.118(5) Uani 1 1 d . . . O6 O 0.5000 0.2500 0.2500 0.105(17) Uani 0.63(5) 4 d SP . . 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 Te1 0.0338(3) 0.0577(4) 0.0596(4) 0.0237(4) 0.0021(3) 0.0025(3) Te2 0.0504(4) 0.0540(4) 0.0469(4) 0.0008(4) 0.0064(3) -0.0007(4) Te3 0.0470(5) 0.0354(5) 0.0830(8) 0.000 -0.0077(6) 0.000 Ge2 0.0371(5) 0.0401(5) 0.0561(7) 0.0156(6) -0.0009(5) -0.0032(5) Ge1 0.0407(5) 0.0344(5) 0.0504(6) 0.0082(5) 0.0115(5) 0.0037(5) C1A 0.051(7) 0.057(10) 0.074(10) 0.003(8) -0.010(7) -0.027(7) C3A 0.060(9) 0.053(9) 0.094(12) 0.020(9) -0.007(9) -0.019(7) O1A 0.126(10) 0.089(9) 0.143(12) 0.077(8) -0.060(9) -0.048(8) O2A 0.092(8) 0.087(8) 0.143(14) 0.060(9) 0.001(9) -0.031(7) C1B 0.051(7) 0.057(10) 0.074(10) 0.003(8) -0.010(7) -0.027(7) C3B 0.060(9) 0.053(9) 0.094(12) 0.020(9) -0.007(9) -0.019(7) O1B 0.126(10) 0.089(9) 0.143(12) 0.077(8) -0.060(9) -0.048(8) O2B 0.092(8) 0.087(8) 0.143(14) 0.060(9) 0.001(9) -0.031(7) C2 0.052(6) 0.053(6) 0.094(10) 0.034(7) 0.016(7) -0.006(6) C4 0.065(7) 0.038(6) 0.071(8) 0.016(6) 0.023(6) 0.006(5) C5 0.061(7) 0.047(7) 0.091(10) 0.020(7) -0.010(7) 0.014(6) C6 0.056(8) 0.056(8) 0.163(17) 0.033(10) 0.009(10) -0.001(6) O4 0.118(8) 0.069(6) 0.143(10) 0.036(7) -0.060(7) 0.014(6) O5 0.129(8) 0.046(5) 0.181(12) 0.012(7) -0.091(8) -0.004(6) O6 0.08(2) 0.06(2) 0.17(4) 0.000 0.000 0.000 _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 Te1 Ge1 2.5548(14) . ? Te1 Ge2 2.5683(14) . ? Te2 Ge1 2.5573(15) 3_755 ? Te2 Ge2 2.5630(15) . ? Te3 Ge2 2.5749(14) . ? Te3 Ge2 2.5749(14) 3_755 ? Ge2 C2 1.979(12) . ? Ge1 C4 1.991(11) . ? Ge1 Ge1 2.451(2) 3_755 ? Ge1 Te2 2.5573(15) 3_755 ? C1A O1A 1.04(9) . ? C1A O2A 1.250(10) . ? C1A C3A 1.72(8) . ? C3A C2 1.96(8) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? O2A H2A 0.8400 . ? C1B O1B 1.27(2) . ? C1B O2B 1.27(2) . ? C1B C3B 1.43(2) . ? C3B C2 1.60(2) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? O2B H2B 0.8400 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C4 C5 1.464(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.541(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O5 1.17(2) . ? C6 O4 1.40(2) . ? O4 H4 0.8400 . ? 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 Ge1 Te1 Ge2 88.40(5) . . ? Ge1 Te2 Ge2 87.99(5) 3_755 . ? Ge2 Te3 Ge2 105.30(6) . 3_755 ? C2 Ge2 Te2 110.6(4) . . ? C2 Ge2 Te1 112.5(4) . . ? Te2 Ge2 Te1 107.34(5) . . ? C2 Ge2 Te3 101.2(4) . . ? Te2 Ge2 Te3 113.57(5) . . ? Te1 Ge2 Te3 111.76(6) . . ? C4 Ge1 Ge1 107.5(4) . 3_755 ? C4 Ge1 Te1 110.4(4) . . ? Ge1 Ge1 Te1 109.13(7) 3_755 . ? C4 Ge1 Te2 107.3(4) . 3_755 ? Ge1 Ge1 Te2 109.30(6) 3_755 3_755 ? Te1 Ge1 Te2 113.09(5) . 3_755 ? O1A C1A O2A 74(5) . . ? O1A C1A C3A 109(6) . . ? O2A C1A C3A 152(5) . . ? C1A C3A C2 99(5) . . ? C1A C3A H3A1 111.9 . . ? C2 C3A H3A1 111.9 . . ? C1A C3A H3A2 111.9 . . ? C2 C3A H3A2 111.9 . . ? H3A1 C3A H3A2 109.6 . . ? O1B C1B O2B 118.9(16) . . ? O1B C1B C3B 126.7(15) . . ? O2B C1B C3B 114.3(16) . . ? C1B C3B C2 106.5(14) . . ? C1B C3B H3B1 110.4 . . ? C2 C3B H3B1 110.4 . . ? C1B C3B H3B2 110.4 . . ? C2 C3B H3B2 110.4 . . ? H3B1 C3B H3B2 108.6 . . ? C1B O2B H2B 109.5 . . ? C3B C2 C3A 31(2) . . ? C3B C2 Ge2 107.6(10) . . ? C3A C2 Ge2 101(2) . . ? C3B C2 H2C 130.4 . . ? C3A C2 H2C 111.7 . . ? Ge2 C2 H2C 111.7 . . ? C3B C2 H2D 81.7 . . ? C3A C2 H2D 111.7 . . ? Ge2 C2 H2D 111.7 . . ? H2C C2 H2D 109.4 . . ? C5 C4 Ge1 113.6(9) . . ? C5 C4 H4A 108.9 . . ? Ge1 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? Ge1 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 107.6(12) . . ? C4 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? C4 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O5 C6 O4 124.6(14) . . ? O5 C6 C5 126.0(16) . . ? O4 C6 C5 109.3(13) . . ? C6 O4 H4 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O5 0.84 1.82 2.64(2) 166 13_655 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.90 _refine_diff_density_min -2.07 _refine_diff_density_rms 0.25 # Attachment '- 3-rev.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 794770' #TrackingRef '- 3-rev.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C20 H20 Ge4 O16 Te5, 2(C4 H8 O)' _chemical_formula_sum 'C28 H36 Ge4 O18 Te5' _chemical_formula_weight 1588.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.901(4) _cell_length_b 23.406(6) _cell_length_c 19.298(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.57(4) _cell_angle_gamma 90.00 _cell_volume 5375(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14918 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 52.24 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 4.930 _exptl_absorpt_correction_type none _exptl_special_details ; The choice of crystal system was based on Laue symmetry of the diffraction pattern. The chosen space group was in accordance with systematic absences. ; _diffrn_ambient_temperature 100(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 IPDS2 _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32249 _diffrn_reflns_av_R_equivalents 0.2528 _diffrn_reflns_av_sigmaI/netI 0.3767 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8337 _reflns_number_gt 2357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe, X-Area ver. 1.54' _computing_cell_refinement 'Stoe, X-Area ver. 1.54' _computing_data_reduction 'Stoe, X-Area ver. 1.54' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. SQUEEZE procedure was used to remove part of heavily disordered solvent. All C-C bond lengths were restrained to 1.54(1) /%A with a DFIX restraint. Correspondingly, all carboxyl C-O bond lengths were restrained to 1.25(2) /%A. Within the residual THF solvent molecule all distances (C-C and C-O) were restrained to 1.5(1) /%A. On the final difference Fourier map the highest peak of 0.49 e//%A^3^ was located 1.69 /%A from Te5 atom (the deepest hole of -0.47 e//%A^3^ was located 1.24 /%A from Te3 atom). ; _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^)+(0.0000P)^2^] 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 8337 _refine_ls_number_parameters 460 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2188 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 0.643 _refine_ls_restrained_S_all 0.643 _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 Te1 Te 0.49622(13) 0.99628(5) 0.87323(8) 0.0563(4) Uani 1 1 d . . . Te5 Te 0.44797(14) 1.17545(5) 0.82836(9) 0.0616(4) Uani 1 1 d . . . Te2 Te 0.62771(14) 1.11640(5) 1.00768(8) 0.0550(4) Uani 1 1 d . . . Te3 Te 0.67245(14) 1.07402(6) 0.71092(9) 0.0606(4) Uani 1 1 d . . . Te4 Te 0.81368(14) 1.18679(5) 0.84941(9) 0.0630(5) Uani 1 1 d . . . Ge2 Ge 0.7900(2) 1.07902(8) 0.82381(13) 0.0562(6) Uani 1 1 d . . . Ge1 Ge 0.6829(2) 1.03682(8) 0.92094(13) 0.0525(6) Uani 1 1 d . . . Ge4 Ge 0.6216(2) 1.18896(8) 0.90796(13) 0.0572(6) Uani 1 1 d . . . Ge3 Ge 0.4902(2) 1.07504(9) 0.78093(14) 0.0573(6) Uani 1 1 d . . . C2 C 0.9399(17) 1.0418(8) 0.8092(12) 0.079(9) Uani 1 1 d D . . H2 H 0.9581 1.0213 0.8534 0.095 Uiso 1 1 calc R . . O12 O 0.7948(13) 0.9476(5) 0.8148(9) 0.063(5) Uani 1 1 d D . . O22 O 0.8335(16) 0.9149(5) 0.7118(9) 0.078(5) Uani 1 1 d D . . O32 O 1.1017(13) 1.1553(5) 0.7257(9) 0.067(4) Uani 1 1 d D . . O42 O 0.9491(13) 1.1152(6) 0.6922(9) 0.063(4) Uani 1 1 d D . . C12 C 0.9385(17) 0.9964(7) 0.7528(10) 0.053(4) Uani 1 1 d D . . H12A H 1.0128 0.9774 0.7525 0.064 Uiso 1 1 calc R . . H12B H 0.9283 1.0156 0.7075 0.064 Uiso 1 1 calc R . . C22 C 0.8482(18) 0.9507(7) 0.7598(9) 0.053(4) Uani 1 1 d D . . C32 C 1.0371(18) 1.0843(6) 0.7978(11) 0.069(7) Uani 1 1 d D . . H32A H 1.0412 1.1106 0.8380 0.083 Uiso 1 1 calc R . . H32B H 1.1086 1.0627 0.7964 0.083 Uiso 1 1 calc R . . C42 C 1.0262(17) 1.1190(8) 0.7329(11) 0.067(4) Uani 1 1 d D . . C1 C 0.770(2) 0.9776(6) 0.9707(11) 0.063(5) Uani 1 1 d D . . H1 H 0.8328 0.9661 0.9398 0.076 Uiso 1 1 calc R . . O11 O 0.9198(14) 1.0674(6) 0.9652(9) 0.071(4) Uani 1 1 d D . . O21 O 0.9623(15) 1.0649(5) 1.0747(9) 0.075(5) Uani 1 1 d D . . O31 O 0.7175(12) 0.8237(5) 1.0054(10) 0.067(5) Uani 1 1 d D . . O41 O 0.8725(15) 0.8649(5) 0.9695(11) 0.084(6) Uani 1 1 d D . . C11 C 0.8234(15) 0.9984(7) 1.0399(11) 0.064(7) Uani 1 1 d D . . H11A H 0.7642 1.0117 1.0718 0.077 Uiso 1 1 calc R . . H11B H 0.8648 0.9667 1.0625 0.077 Uiso 1 1 calc R . . C21 C 0.9043(19) 1.0477(8) 1.0237(10) 0.071(4) Uani 1 1 d D . . C31 C 0.7022(16) 0.9226(6) 0.9868(13) 0.063(5) Uani 1 1 d D . . H31A H 0.6670 0.9269 1.0328 0.076 Uiso 1 1 calc R . . H31B H 0.6409 0.9187 0.9520 0.076 Uiso 1 1 calc R . . C41 C 0.7720(15) 0.8676(6) 0.9868(11) 0.046(5) Uani 1 1 d D . . O01 O 0.6990(14) 0.8291(6) 0.7374(13) 0.093(7) Uani 1 1 d D . . C01 C 0.582(2) 0.843(2) 0.761(2) 0.106(11) Uani 1 1 d D . . H01A H 0.5267 0.8294 0.7269 0.127 Uiso 1 1 calc R . . H01B H 0.5742 0.8853 0.7651 0.127 Uiso 1 1 calc R . . C02 C 0.560(4) 0.8152(18) 0.833(4) 0.17(3) Uani 1 1 d D . . H02E H 0.5673 0.8427 0.8721 0.199 Uiso 1 1 calc R . . H02F H 0.4850 0.7964 0.8351 0.199 Uiso 1 1 calc R . . C03 C 0.657(3) 0.7718(11) 0.8317(17) 0.085(9) Uani 1 1 d D . . H03C H 0.6808 0.7619 0.8794 0.102 Uiso 1 1 calc R . . H03D H 0.6321 0.7363 0.8079 0.102 Uiso 1 1 calc R . . C04 C 0.750(3) 0.7984(9) 0.7940(13) 0.072(8) Uani 1 1 d D . . H04A H 0.7920 0.8247 0.8247 0.086 Uiso 1 1 calc R . . H04B H 0.8016 0.7688 0.7765 0.086 Uiso 1 1 calc R . . O02 O 0.167(3) 0.7791(11) 0.865(3) 0.178(19) Uani 1 1 d D . . C05 C 0.244(3) 0.7853(14) 0.817(2) 0.107(14) Uani 1 1 d D . . H05G H 0.2624 0.7485 0.7951 0.129 Uiso 1 1 calc R . . H05H H 0.3128 0.8032 0.8362 0.129 Uiso 1 1 calc R . . C06 C 0.1840(15) 0.8233(6) 0.7704(12) 0.042(5) Uani 1 1 d D . . H06A H 0.2314 0.8574 0.7627 0.050 Uiso 1 1 calc R . . H06B H 0.1753 0.8036 0.7252 0.050 Uiso 1 1 calc R . . C07 C 0.075(3) 0.8422(11) 0.7921(15) 0.080(9) Uani 1 1 d D . . H07C H 0.0206 0.8432 0.7527 0.096 Uiso 1 1 calc R . . H07D H 0.0783 0.8805 0.8138 0.096 Uiso 1 1 calc R . . C08 C 0.043(3) 0.7968(12) 0.8445(18) 0.101(11) Uani 1 1 d D . . H08A H 0.0002 0.7649 0.8231 0.121 Uiso 1 1 calc R . . H08B H 0.0006 0.8126 0.8840 0.121 Uiso 1 1 calc R . . O43 O 0.3093(15) 0.9026(6) 0.7138(12) 0.092(7) Uani 1 1 d D . . O34 O 0.4237(14) 1.3366(6) 1.0662(9) 0.069(5) Uani 1 1 d D . . C34 C 0.4893(19) 1.2661(7) 0.9956(11) 0.063(7) Uani 1 1 d D . . H34A H 0.4257 1.2817 0.9681 0.076 Uiso 1 1 calc R . . H34B H 0.4698 1.2265 1.0090 0.076 Uiso 1 1 calc R . . O44 O 0.5873(13) 1.2957(5) 1.0990(9) 0.056(4) Uani 1 1 d D . . O24 O 0.4735(16) 1.3927(6) 0.8917(11) 0.086(6) Uani 1 1 d D . . C33 C 0.372(2) 0.9959(7) 0.6902(12) 0.071(7) Uani 1 1 d D . . H33A H 0.3479 0.9940 0.6410 0.085 Uiso 1 1 calc R . . H33B H 0.4520 0.9843 0.6928 0.085 Uiso 1 1 calc R . . C13 C 0.375(2) 1.1012(9) 0.6555(13) 0.076(5) Uani 1 1 d D . . H13A H 0.3812 1.1404 0.6743 0.091 Uiso 1 1 calc R . . H13B H 0.4443 1.0924 0.6300 0.091 Uiso 1 1 calc R . . C14 C 0.593(2) 1.3092(6) 0.8908(10) 0.070(8) Uani 1 1 d D . . H14A H 0.6680 1.3119 0.8697 0.084 Uiso 1 1 calc R . . H14B H 0.5388 1.2967 0.8544 0.084 Uiso 1 1 calc R . . O33 O 0.2370(16) 0.9699(5) 0.7787(10) 0.077(6) Uani 1 1 d D . . C43 C 0.302(2) 0.9543(8) 0.7323(11) 0.069(7) Uani 1 1 d D . . C3 C 0.361(2) 1.0582(7) 0.7161(12) 0.076(5) Uani 1 1 d D . . H3 H 0.2875 1.0640 0.7399 0.091 Uiso 1 1 calc R . . C4 C 0.595(2) 1.2649(8) 0.9499(11) 0.084(9) Uani 1 1 d D . . H4 H 0.6616 1.2739 0.9803 0.101 Uiso 1 1 calc R . . C24 C 0.5580(17) 1.3677(6) 0.9178(11) 0.058(7) Uani 1 1 d D . . O13 O 0.2873(16) 1.1260(7) 0.5509(11) 0.095(6) Uani 1 1 d D . . C23 C 0.2734(17) 1.0980(10) 0.6056(11) 0.076(5) Uani 1 1 d D . . O14 O 0.6168(18) 1.3910(7) 0.9625(12) 0.099(7) Uani 1 1 d D . . O23 O 0.1853(15) 1.0701(6) 0.6155(8) 0.074(5) Uani 1 1 d D . . C44 C 0.5044(15) 1.3016(8) 1.0605(9) 0.049(5) Uani 1 1 d 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 Te1 0.0524(10) 0.0528(7) 0.0636(10) 0.0036(6) -0.0013(8) 0.0018(6) Te5 0.0588(11) 0.0589(8) 0.0672(11) -0.0018(6) -0.0023(9) 0.0080(7) Te2 0.0530(10) 0.0528(7) 0.0592(10) 0.0016(6) 0.0014(8) 0.0025(6) Te3 0.0531(11) 0.0714(8) 0.0572(10) 0.0031(7) 0.0018(8) 0.0012(7) Te4 0.0600(11) 0.0524(7) 0.0769(12) 0.0014(7) 0.0073(9) -0.0016(6) Ge2 0.0537(16) 0.0561(11) 0.0590(16) 0.0037(10) 0.0051(12) -0.0004(10) Ge1 0.0522(16) 0.0500(10) 0.0553(15) 0.0030(9) 0.0010(12) 0.0055(9) Ge4 0.0568(17) 0.0503(11) 0.0645(17) -0.0003(10) 0.0032(13) 0.0011(10) Ge3 0.0507(16) 0.0579(11) 0.0632(16) 0.0005(10) -0.0051(13) 0.0024(10) C2 0.036(15) 0.101(16) 0.10(2) 0.050(15) 0.041(15) 0.025(12) O12 0.059(11) 0.042(7) 0.089(14) -0.020(7) -0.033(10) 0.001(6) O22 0.102(15) 0.055(8) 0.077(13) -0.001(7) 0.016(11) -0.003(8) O32 0.055(10) 0.071(8) 0.074(11) 0.003(6) 0.008(8) -0.005(5) O42 0.041(10) 0.073(8) 0.077(12) 0.012(7) -0.004(9) -0.002(7) C12 0.075(13) 0.061(8) 0.023(8) -0.009(7) 0.018(8) 0.009(7) C22 0.075(13) 0.061(8) 0.023(8) -0.009(7) 0.018(8) 0.009(7) C32 0.075(17) 0.012(8) 0.12(2) -0.005(9) 0.005(15) -0.022(8) C42 0.055(10) 0.071(8) 0.074(11) 0.003(6) 0.008(8) -0.005(5) C1 0.074(12) 0.052(7) 0.062(11) -0.005(7) -0.043(10) 0.007(7) O11 0.066(9) 0.074(8) 0.073(11) -0.007(7) -0.002(9) 0.006(7) O21 0.070(12) 0.065(8) 0.090(14) 0.003(8) -0.023(11) -0.015(7) O31 0.050(10) 0.045(7) 0.106(14) 0.004(7) 0.009(9) -0.015(6) O41 0.066(13) 0.052(8) 0.134(19) 0.000(8) 0.014(12) 0.002(7) C11 0.022(11) 0.061(11) 0.11(2) 0.045(12) -0.001(12) 0.017(9) C21 0.066(9) 0.074(8) 0.073(11) -0.007(7) -0.002(9) 0.006(7) C31 0.074(12) 0.052(7) 0.062(11) -0.005(7) -0.043(10) 0.007(7) C41 0.042(15) 0.056(11) 0.038(13) 0.011(8) 0.004(12) 0.002(10) O01 0.047(12) 0.078(10) 0.15(2) -0.021(11) -0.019(13) -0.021(8) C01 0.025(16) 0.22(3) 0.07(3) -0.04(2) 0.015(16) -0.014(18) C02 0.09(3) 0.14(3) 0.27(9) 0.02(3) -0.03(4) -0.01(2) C03 0.09(2) 0.089(16) 0.07(2) 0.032(14) -0.021(18) -0.027(16) C04 0.12(2) 0.054(12) 0.045(14) 0.028(10) 0.003(15) -0.005(12) O02 0.13(3) 0.14(2) 0.26(5) -0.02(2) -0.10(4) -0.006(18) C05 0.039(19) 0.11(2) 0.17(4) 0.00(2) 0.07(2) 0.003(15) C06 0.032(12) 0.015(7) 0.078(15) 0.020(7) -0.002(10) 0.001(7) C07 0.08(2) 0.094(16) 0.063(19) -0.001(13) -0.039(17) 0.007(14) C08 0.12(3) 0.12(2) 0.07(2) -0.016(16) -0.01(2) 0.019(18) O43 0.076(13) 0.040(8) 0.16(2) -0.007(8) 0.026(13) -0.011(7) O34 0.075(12) 0.074(9) 0.059(11) -0.007(7) 0.007(9) 0.040(8) C34 0.043(15) 0.035(9) 0.11(2) 0.017(11) 0.005(14) -0.001(9) O44 0.052(10) 0.049(7) 0.067(11) -0.005(6) 0.000(9) 0.002(6) O24 0.093(15) 0.061(8) 0.104(16) 0.007(8) -0.044(13) 0.016(8) C33 0.09(2) 0.068(12) 0.056(16) -0.028(11) 0.000(15) -0.002(12) C13 0.051(10) 0.076(8) 0.101(13) 0.001(7) -0.033(9) -0.006(7) C14 0.12(2) 0.031(9) 0.062(16) 0.017(9) -0.025(16) -0.007(10) O33 0.088(14) 0.063(8) 0.080(14) 0.015(8) -0.027(12) -0.031(8) C43 0.09(2) 0.092(18) 0.029(14) 0.025(11) 0.024(15) -0.006(14) C3 0.051(10) 0.076(8) 0.101(13) 0.001(7) -0.033(9) -0.006(7) C4 0.09(2) 0.070(14) 0.09(2) 0.011(13) -0.03(2) -0.039(13) C24 0.057(17) 0.049(11) 0.066(18) 0.028(11) -0.003(14) -0.014(11) O13 0.075(14) 0.096(11) 0.114(18) 0.034(10) -0.019(13) 0.000(9) C23 0.051(10) 0.076(8) 0.101(13) 0.001(7) -0.033(9) -0.006(7) O14 0.104(17) 0.070(10) 0.120(18) 0.017(10) -0.052(15) 0.019(9) O23 0.099(14) 0.063(8) 0.058(11) -0.015(7) -0.002(10) -0.008(8) C44 0.026(13) 0.091(15) 0.030(12) 0.005(10) 0.000(11) -0.007(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 Te1 Ge3 2.564(3) . ? Te1 Ge1 2.578(3) . ? Te5 Ge3 2.573(3) . ? Te5 Ge4 2.582(3) . ? Te2 Ge4 2.567(3) . ? Te2 Ge1 2.593(3) . ? Te3 Ge3 2.567(3) . ? Te3 Ge2 2.580(3) . ? Te4 Ge4 2.560(3) . ? Te4 Ge2 2.585(3) . ? Ge2 C2 2.01(2) . ? Ge2 Ge1 2.482(4) . ? Ge1 C1 1.972(18) . ? Ge4 C4 1.98(2) . ? Ge3 C3 2.01(2) . ? C2 C12 1.521(18) . ? C2 C32 1.543(17) . ? C2 H2 1.0000 . ? O12 C22 1.245(16) . ? O22 C22 1.259(16) . ? O32 C42 1.246(16) . ? O42 C42 1.206(16) . ? C12 C22 1.524(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C32 C42 1.498(18) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C1 C31 1.550(18) . ? C1 C11 1.554(18) . ? C1 H1 1.0000 . ? O11 C21 1.235(17) . ? O21 C21 1.261(16) . ? O31 C41 1.269(15) . ? O41 C41 1.247(15) . ? C11 C21 1.537(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C31 C41 1.531(17) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O01 C04 1.44(3) . ? O01 C01 1.50(3) . ? C01 C02 1.57(6) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? C02 C03 1.54(5) . ? C02 H02E 0.9900 . ? C02 H02F 0.9900 . ? C03 C04 1.47(4) . ? C03 H03C 0.9900 . ? C03 H03D 0.9900 . ? C04 H04A 0.9900 . ? C04 H04B 0.9900 . ? O02 C05 1.32(5) . ? O02 C08 1.58(4) . ? C05 C06 1.45(4) . ? C05 H05G 0.9900 . ? C05 H05H 0.9900 . ? C06 C07 1.44(3) . ? C06 H06A 0.9900 . ? C06 H06B 0.9900 . ? C07 C08 1.52(4) . ? C07 H07C 0.9900 . ? C07 H07D 0.9900 . ? C08 H08A 0.9900 . ? C08 H08B 0.9900 . ? O43 C43 1.266(17) . ? O34 C44 1.269(16) . ? C34 C44 1.511(18) . ? C34 C4 1.548(18) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O44 C44 1.237(15) . ? O24 C24 1.264(16) . ? C33 C43 1.523(18) . ? C33 C3 1.548(17) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C13 C23 1.536(18) . ? C13 C3 1.554(19) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C24 1.522(18) . ? C14 C4 1.543(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O33 C43 1.243(17) . ? C3 H3 1.0000 . ? C4 H4 1.0000 . ? C24 O14 1.233(16) . ? O13 C23 1.256(18) . ? C23 O23 1.251(16) . ? 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 Te1 Ge1 90.09(9) . . ? Ge3 Te5 Ge4 99.53(9) . . ? Ge4 Te2 Ge1 89.81(9) . . ? Ge3 Te3 Ge2 90.51(10) . . ? Ge4 Te4 Ge2 90.42(9) . . ? C2 Ge2 Ge1 113.4(6) . . ? C2 Ge2 Te3 109.7(7) . . ? Ge1 Ge2 Te3 109.99(11) . . ? C2 Ge2 Te4 110.8(5) . . ? Ge1 Ge2 Te4 107.46(11) . . ? Te3 Ge2 Te4 105.24(9) . . ? C1 Ge1 Ge2 112.2(8) . . ? C1 Ge1 Te1 111.1(5) . . ? Ge2 Ge1 Te1 108.90(11) . . ? C1 Ge1 Te2 109.0(6) . . ? Ge2 Ge1 Te2 109.69(9) . . ? Te1 Ge1 Te2 105.77(10) . . ? C4 Ge4 Te4 110.1(7) . . ? C4 Ge4 Te2 106.9(6) . . ? Te4 Ge4 Te2 107.41(10) . . ? C4 Ge4 Te5 103.0(7) . . ? Te4 Ge4 Te5 116.61(11) . . ? Te2 Ge4 Te5 112.41(10) . . ? C3 Ge3 Te1 107.9(6) . . ? C3 Ge3 Te3 108.4(8) . . ? Te1 Ge3 Te3 109.93(10) . . ? C3 Ge3 Te5 104.4(5) . . ? Te1 Ge3 Te5 114.44(11) . . ? Te3 Ge3 Te5 111.39(10) . . ? C12 C2 C32 110.5(16) . . ? C12 C2 Ge2 113.6(15) . . ? C32 C2 Ge2 114.2(13) . . ? C12 C2 H2 105.9 . . ? C32 C2 H2 105.9 . . ? Ge2 C2 H2 105.9 . . ? C2 C12 C22 115.5(15) . . ? C2 C12 H12A 108.4 . . ? C22 C12 H12A 108.4 . . ? C2 C12 H12B 108.4 . . ? C22 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O12 C22 O22 121.4(17) . . ? O12 C22 C12 118.8(15) . . ? O22 C22 C12 119.7(16) . . ? C42 C32 C2 114.2(17) . . ? C42 C32 H32A 108.7 . . ? C2 C32 H32A 108.7 . . ? C42 C32 H32B 108.7 . . ? C2 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? O42 C42 O32 121.5(18) . . ? O42 C42 C32 124.3(17) . . ? O32 C42 C32 114.0(16) . . ? C31 C1 C11 107.4(15) . . ? C31 C1 Ge1 114.3(13) . . ? C11 C1 Ge1 114.0(11) . . ? C31 C1 H1 106.9 . . ? C11 C1 H1 106.9 . . ? Ge1 C1 H1 106.9 . . ? C21 C11 C1 108.3(15) . . ? C21 C11 H11A 110.0 . . ? C1 C11 H11A 110.0 . . ? C21 C11 H11B 110.0 . . ? C1 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? O11 C21 O21 120.6(19) . . ? O11 C21 C11 124.4(18) . . ? O21 C21 C11 114.8(17) . . ? C41 C31 C1 114.5(16) . . ? C41 C31 H31A 108.6 . . ? C1 C31 H31A 108.6 . . ? C41 C31 H31B 108.6 . . ? C1 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? O41 C41 O31 121.9(15) . . ? O41 C41 C31 124.4(15) . . ? O31 C41 C31 113.7(16) . . ? C04 O01 C01 105(3) . . ? O01 C01 C02 110(3) . . ? O01 C01 H01A 109.6 . . ? C02 C01 H01A 109.6 . . ? O01 C01 H01B 109.6 . . ? C02 C01 H01B 109.6 . . ? H01A C01 H01B 108.1 . . ? C03 C02 C01 97(4) . . ? C03 C02 H02E 112.4 . . ? C01 C02 H02E 112.4 . . ? C03 C02 H02F 112.4 . . ? C01 C02 H02F 112.4 . . ? H02E C02 H02F 109.9 . . ? C04 C03 C02 108(3) . . ? C04 C03 H03C 110.2 . . ? C02 C03 H03C 110.2 . . ? C04 C03 H03D 110.2 . . ? C02 C03 H03D 110.2 . . ? H03C C03 H03D 108.5 . . ? O01 C04 C03 106(2) . . ? O01 C04 H04A 110.5 . . ? C03 C04 H04A 110.5 . . ? O01 C04 H04B 110.5 . . ? C03 C04 H04B 110.5 . . ? H04A C04 H04B 108.7 . . ? C05 O02 C08 116(4) . . ? O02 C05 C06 100(3) . . ? O02 C05 H05G 111.8 . . ? C06 C05 H05G 111.8 . . ? O02 C05 H05H 111.8 . . ? C06 C05 H05H 111.8 . . ? H05G C05 H05H 109.5 . . ? C07 C06 C05 116(2) . . ? C07 C06 H06A 108.2 . . ? C05 C06 H06A 108.2 . . ? C07 C06 H06B 108.2 . . ? C05 C06 H06B 108.2 . . ? H06A C06 H06B 107.4 . . ? C06 C07 C08 102(2) . . ? C06 C07 H07C 111.4 . . ? C08 C07 H07C 111.4 . . ? C06 C07 H07D 111.4 . . ? C08 C07 H07D 111.4 . . ? H07C C07 H07D 109.2 . . ? C07 C08 O02 97(3) . . ? C07 C08 H08A 112.4 . . ? O02 C08 H08A 112.4 . . ? C07 C08 H08B 112.4 . . ? O02 C08 H08B 112.4 . . ? H08A C08 H08B 110.0 . . ? C44 C34 C4 113.0(17) . . ? C44 C34 H34A 109.0 . . ? C4 C34 H34A 109.0 . . ? C44 C34 H34B 109.0 . . ? C4 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C43 C33 C3 112.4(17) . . ? C43 C33 H33A 109.1 . . ? C3 C33 H33A 109.1 . . ? C43 C33 H33B 109.1 . . ? C3 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C23 C13 C3 110.6(17) . . ? C23 C13 H13A 109.5 . . ? C3 C13 H13A 109.5 . . ? C23 C13 H13B 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C24 C14 C4 110.9(17) . . ? C24 C14 H14A 109.5 . . ? C4 C14 H14A 109.5 . . ? C24 C14 H14B 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O33 C43 O43 122.0(18) . . ? O33 C43 C33 123.0(17) . . ? O43 C43 C33 115.0(18) . . ? C33 C3 C13 110.9(18) . . ? C33 C3 Ge3 108.6(15) . . ? C13 C3 Ge3 104.8(13) . . ? C33 C3 H3 110.8 . . ? C13 C3 H3 110.8 . . ? Ge3 C3 H3 110.8 . . ? C14 C4 C34 113(2) . . ? C14 C4 Ge4 107.7(14) . . ? C34 C4 Ge4 112.5(12) . . ? C14 C4 H4 107.6 . . ? C34 C4 H4 107.6 . . ? Ge4 C4 H4 107.6 . . ? O14 C24 O24 121.2(17) . . ? O14 C24 C14 118.9(18) . . ? O24 C24 C14 119.8(19) . . ? O23 C23 O13 121.2(19) . . ? O23 C23 C13 125.7(19) . . ? O13 C23 C13 113.1(19) . . ? O44 C44 O34 128.3(17) . . ? O44 C44 C34 121.6(17) . . ? O34 C44 C34 110.1(16) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.49 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.11 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.010 0.500 0.000 568 247 ' ' 2 0.014 1.000 0.500 568 247 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_RINTA01_3 ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The data quality was limited, no absorption correction was applied due to considerable twinning problems. ; _vrf_PLAT026_3 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 28 Perc. RESPONSE: The data quality was limited and considerable twinning problems were present. ; _vrf_PLAT029_3 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.88 RESPONSE: The data quality was limited and considerable twinning problems were present. ; # end Validation Reply Form # Attachment '- 4-rev.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 794771' #TrackingRef '- 4-rev.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety '(C6 H13 Ge N2 Te2), (N2H5), 0.5(N2H4)' _chemical_formula_sum 'C6 H20 Ge N5 Te2' _chemical_formula_weight 490.06 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 31.866(7) _cell_length_b 15.441(4) _cell_length_c 12.271(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.94(3) _cell_angle_gamma 90.00 _cell_volume 5806(3) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21909 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 26.73 _exptl_crystal_description 'cut needle' _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 6.030 _exptl_absorpt_correction_type none _exptl_special_details ; There are pseudosymmetry elements in the crystal structure: pseudosymmetry centres at 0.207, 0.373, 0.253 and 0.207, 0.123, 0.253, respectively. Also a non-crystallographic translation could be found relating the molecules with Ge1 and Ge2 atoms, respectively, by a 0, 0.5, 0 translation along the [010] direction. However, no chemically reasonable structure model in centrosymmetric space group types could have been found and the structure is interpreted as a racemic twin in non-centrosymmetric space group Cc. ; _diffrn_ambient_temperature 100(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 IPDS2 _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21516 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.63 _diffrn_reflns_theta_max 26.73 _reflns_number_total 11569 _reflns_number_gt 10471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe, X-Area ver. 1.54' _computing_cell_refinement 'Stoe, X-Area ver. 1.54' _computing_data_reduction 'Stoe, X-Area ver. 1.54' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The N-N bond lengths within all hydrazinium cations were restrained to 1.440(2) /%A, all N-H bond lengths were restrained to 0.860(1) /%A with the corresponding DFIX restraints. EADP restraints were also used to afford a fully anisotropic model (for the following atom pairs: N12/N22, N11/N21, N101/N100, C13/C43, C13/C33, N104/N105, N102/N103, N108/N109, N104/N102, N107/N106). Amine H atoms have been found on the difference Fourier map and refined with Ueq=1.5U~eq~(parent atom). Hydrazinium H atoms could not have been all localized. This is probably connected with refinement problems arising from pseudosymmetry and the possibility of H atoms disorder. Hydrazinium H atoms were gradually localized on difference Fourier maps and carefully introduced to the model (as long as they conformed with the possible hydrogen bonding scheme). An anti-bumping DFIX restraint was used to set the H...N (from the -NH~2~ moiety) distance at value not smaller than 2.09(1) /%A to ensure the right molecular geometry. The identified NH~3~^+^ groups H atoms were constrained with AFIX 33 constraint. For the remaining N-bonded H atoms no constraints were used (to avoid drift of restrained distances values). On the final difference Fourier map the highest peak of 1.78 e//%A^3^ was located 0.83 /%A from Te6 atom (the deepest hole of -2.08 e//%A^3^ was located 0.77 /%A from Te8 atom). First 16 peaks at the difference Fourier map are localized in the neighbourhood of Te atoms. ; _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^)+(0.0487P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.46(3) _refine_ls_number_reflns 11569 _refine_ls_number_parameters 500 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.770 _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 C11 C 0.6435(4) 0.0579(9) 0.4781(12) 0.016(2) Uani 1 1 d U . . C63 C 0.7843(5) 0.5488(11) 0.7747(13) 0.023(3) Uani 1 1 d U . . H63A H 0.7749 0.5823 0.7044 0.035 Uiso 1 1 calc R . . H63B H 0.7616 0.5069 0.7780 0.035 Uiso 1 1 calc R . . H63C H 0.8114 0.5179 0.7767 0.035 Uiso 1 1 calc R . . C64 C 0.7855(5) 0.9568(11) 0.2849(12) 0.022(3) Uani 1 1 d U . . H64A H 0.8122 0.9878 0.2839 0.032 Uiso 1 1 calc R . . H64B H 0.7631 0.9987 0.2911 0.032 Uiso 1 1 calc R . . H64C H 0.7750 0.9235 0.2147 0.032 Uiso 1 1 calc R . . C22 C 0.6736(5) 0.4980(11) 0.5392(12) 0.021(3) Uani 1 1 d U . . H22C H 0.6697 0.4418 0.5008 0.032 Uiso 1 1 calc R . . H22D H 0.6689 0.4918 0.6145 0.032 Uiso 1 1 calc R . . H22E H 0.7033 0.5190 0.5472 0.032 Uiso 1 1 calc R . . C31 C 0.6746(5) -0.0080(11) 0.5500(13) 0.023(3) Uani 1 1 d U . . H31A H 0.7048 0.0094 0.5567 0.034 Uiso 1 1 calc R . . H31B H 0.6692 -0.0651 0.5140 0.034 Uiso 1 1 calc R . . H31C H 0.6699 -0.0108 0.6256 0.034 Uiso 1 1 calc R . . C53 C 0.7918(5) 0.6068(10) 0.8708(13) 0.017(3) Uani 1 1 d U . . C34 C 0.7668(5) 0.8237(11) 0.6521(13) 0.023(3) Uani 1 1 d U . . H34A H 0.7378 0.8483 0.6443 0.034 Uiso 1 1 calc R . . H34B H 0.7890 0.8621 0.6987 0.034 Uiso 1 1 calc R . . H34C H 0.7687 0.7667 0.6883 0.034 Uiso 1 1 calc R . . C23 C 0.7585(5) 0.6756(11) 1.1362(13) 0.026(3) Uani 1 1 d U . . H23C H 0.7610 0.7311 1.1761 0.038 Uiso 1 1 calc R . . H23D H 0.7789 0.6338 1.1829 0.038 Uiso 1 1 calc R . . H23E H 0.7286 0.6537 1.1218 0.038 Uiso 1 1 calc R . . C42 C 0.6424(5) 0.6496(10) 0.5356(13) 0.020(3) Uani 1 1 d U . . H42A H 0.6731 0.6655 0.5727 0.024 Uiso 1 1 calc R . . H42B H 0.6292 0.6963 0.4818 0.024 Uiso 1 1 calc R . . C52 C 0.6181(4) 0.6412(10) 0.6230(11) 0.014(2) Uani 1 1 d U . . C51 C 0.6190(4) 0.1412(10) 0.6256(11) 0.013(2) Uani 1 1 d U . . C41 C 0.6456(5) 0.1453(10) 0.5417(12) 0.020(2) Uani 1 1 d U . . H41A H 0.6764 0.1587 0.5819 0.024 Uiso 1 1 calc R . . H41B H 0.6344 0.1922 0.4864 0.024 Uiso 1 1 calc R . . C54 C 0.7947(5) 0.8976(11) 0.3827(14) 0.020(3) Uani 1 1 d U . . C21 C 0.6529(5) 0.0686(11) 0.3612(13) 0.021(3) Uani 1 1 d U . . H21C H 0.6814 0.0964 0.3716 0.031 Uiso 1 1 calc R . . H21D H 0.6301 0.1045 0.3118 0.031 Uiso 1 1 calc R . . H21E H 0.6532 0.0115 0.3265 0.031 Uiso 1 1 calc R . . C32 C 0.6492(5) 0.5754(10) 0.3516(12) 0.020(3) Uani 1 1 d U . . H32A H 0.6766 0.6069 0.3606 0.030 Uiso 1 1 calc R . . H32B H 0.6251 0.6086 0.3027 0.030 Uiso 1 1 calc R . . H32C H 0.6510 0.5187 0.3172 0.030 Uiso 1 1 calc R . . C12 C 0.6409(4) 0.5625(9) 0.4699(12) 0.014(2) Uani 1 1 d U . . C13 C 0.7693(5) 0.6880(10) 1.0252(13) 0.0205(17) Uani 1 1 d U . . C43 C 0.7669(5) 0.6035(11) 0.9590(14) 0.0205(17) Uani 1 1 d U . . H43A H 0.7787 0.5560 1.0128 0.025 Uiso 1 1 calc R . . H43B H 0.7360 0.5902 0.9213 0.025 Uiso 1 1 calc R . . C33 C 0.7398(5) 0.7547(10) 0.9526(13) 0.0205(17) Uani 1 1 d U . . H33A H 0.7093 0.7388 0.9437 0.031 Uiso 1 1 calc R . . H33B H 0.7453 0.7570 0.8779 0.031 Uiso 1 1 calc R . . H33C H 0.7456 0.8116 0.9889 0.031 Uiso 1 1 calc R . . C14 C 0.7741(4) 0.8143(9) 0.5376(11) 0.013(2) Uani 1 1 d U . . C44 C 0.7718(5) 0.8991(10) 0.4738(13) 0.019(3) Uani 1 1 d U . . H44A H 0.7407 0.9140 0.4394 0.023 Uiso 1 1 calc R . . H44B H 0.7847 0.9454 0.5285 0.023 Uiso 1 1 calc R . . C24 C 0.7424(5) 0.7495(11) 0.4646(12) 0.020(3) Uani 1 1 d U . . H24C H 0.7454 0.6935 0.5036 0.030 Uiso 1 1 calc R . . H24D H 0.7492 0.7425 0.3918 0.030 Uiso 1 1 calc R . . H24E H 0.7125 0.7707 0.4515 0.030 Uiso 1 1 calc R . . C62 C 0.6269(5) 0.7040(10) 0.7222(13) 0.022(3) Uani 1 1 d U . . H62A H 0.6028 0.7454 0.7106 0.033 Uiso 1 1 calc R . . H62B H 0.6542 0.7353 0.7275 0.033 Uiso 1 1 calc R . . H62C H 0.6296 0.6717 0.7926 0.033 Uiso 1 1 calc R . . C61 C 0.6271(5) 0.2048(10) 0.7220(14) 0.023(3) Uani 1 1 d U . . H61A H 0.6046 0.2501 0.7042 0.035 Uiso 1 1 calc R . . H61B H 0.6559 0.2312 0.7335 0.035 Uiso 1 1 calc R . . H61C H 0.6258 0.1746 0.7913 0.035 Uiso 1 1 calc R . . N21 N 0.5586(4) 0.0789(8) 0.6686(10) 0.0147(16) Uani 1 1 d DU . . H1 H 0.559(5) 0.0234(11) 0.674(13) 0.022 Uiso 1 1 d D . . H2 H 0.572(5) 0.096(9) 0.736(5) 0.022 Uiso 1 1 d D . . N22 N 0.5602(4) 0.5735(8) 0.6720(10) 0.0141(15) Uani 1 1 d DU . . H3 H 0.866(3) 0.721(2) 0.821(8) 0.021 Uiso 1 1 d D . . H4 H 0.845(5) 0.637(7) 0.779(8) 0.021 Uiso 1 1 d D . . N23 N 0.8539(4) 0.6738(9) 0.8327(10) 0.020(2) Uani 1 1 d DU . . H5 H 0.571(5) 0.586(10) 0.742(4) 0.030 Uiso 1 1 d D . . H6 H 0.557(5) 0.5182(15) 0.673(15) 0.030 Uiso 1 1 d D . . N24 N 0.8549(4) 0.8303(9) 0.3339(11) 0.022(2) Uani 1 1 d DU . . H7 H 0.861(6) 0.776(3) 0.332(16) 0.033 Uiso 1 1 d D . . H8 H 0.844(6) 0.862(9) 0.276(9) 0.033 Uiso 1 1 d D . . N13 N 0.8230(4) 0.6638(8) 0.8945(9) 0.0127(19) Uani 1 1 d DU . . N14 N 0.8256(4) 0.8388(7) 0.3989(9) 0.0126(19) Uani 1 1 d U . . N11 N 0.5892(4) 0.0837(8) 0.6087(10) 0.0147(16) Uani 1 1 d U . . N12 N 0.5891(4) 0.5829(8) 0.6068(9) 0.0141(15) Uani 1 1 d U . . N100 N 0.4620(4) 0.2534(5) 0.4889(9) 0.0251(16) Uani 1 1 d DU . . H101 H 0.4401 0.2812 0.5095 0.038 Uiso 1 1 calc RD . . H102 H 0.4592 0.2629 0.4140 0.038 Uiso 1 1 calc RD . . H103 H 0.4882 0.2740 0.5307 0.038 Uiso 1 1 calc RD . . N101 N 0.4595(4) 0.1619(5) 0.5087(9) 0.0251(16) Uani 1 1 d DU . . H104 H 0.463(5) 0.1219(11) 0.463(7) 0.038 Uiso 1 1 d D . . N102 N 0.4325(3) 0.0842(7) 0.9648(8) 0.0262(13) Uani 1 1 d DU . . H121 H 0.409(3) 0.078(11) 0.985(13) 0.039 Uiso 1 1 d D . . H122 H 0.426(5) 0.037(6) 0.927(12) 0.039 Uiso 1 1 d D . . N103 N 0.4667(3) 0.0307(7) 1.0336(9) 0.0262(13) Uani 1 1 d DU . . N104 N 0.4229(3) 0.5201(7) 0.9511(8) 0.0262(13) Uani 1 1 d DU . . H141 H 0.4030 0.4767 0.9301 0.039 Uiso 1 1 calc RD . . H142 H 0.4298 0.5410 0.8889 0.039 Uiso 1 1 calc RD . . H143 H 0.4114 0.5634 0.9842 0.039 Uiso 1 1 calc RD . . N105 N 0.4617(3) 0.4872(7) 1.0305(8) 0.0262(4) Uani 1 1 d DU . . H151 H 0.4799 0.5162(13) 1.0822 0.039 Uiso 1 1 d D . . N106 N 0.4492(4) 0.3185(6) 1.2537(9) 0.0291(18) Uani 1 1 d DU . . H161 H 0.428(3) 0.335(11) 1.197(9) 0.044 Uiso 1 1 d D . . N107 N 0.4556(5) 0.4091(6) 1.2810(11) 0.0291(18) Uani 1 1 d DU . . H171 H 0.444(5) 0.4502(14) 1.231(5) 0.044 Uiso 1 1 d D . . N108 N 0.4911(3) 0.2779(8) 1.0925(7) 0.0267(17) Uani 1 1 d DU . . H181 H 0.513(3) 0.311(8) 1.097(4) 0.040 Uiso 1 1 d D . . N109 N 0.4567(3) 0.2642(7) 0.9898(8) 0.0267(17) Uani 1 1 d DU . . H191 H 0.4304 0.2685 1.0050 0.040 Uiso 1 1 calc RD . . H192 H 0.4594 0.2105 0.9620 0.040 Uiso 1 1 calc RD . . H193 H 0.4585 0.3048 0.9377 0.040 Uiso 1 1 calc RD . . N110 N 0.4447(4) 0.0695(6) 0.7581(10) 0.027(2) Uani 1 1 d DU . . N111 N 0.4641(4) 0.1489(6) 0.7339(10) 0.027(3) Uani 1 1 d DU . . H111 H 0.4468 0.1944 0.7402 0.040 Uiso 1 1 calc RD . . H112 H 0.4670 0.1469 0.6622 0.040 Uiso 1 1 calc RD . . H113 H 0.4909 0.1556 0.7840 0.040 Uiso 1 1 calc RD . . Ge4 Ge 0.83520(5) 0.77324(9) 0.54739(12) 0.0126(3) Uani 1 1 d U . . Ge3 Ge 0.83153(5) 0.72308(9) 1.04742(12) 0.0128(3) Uani 1 1 d U . . Ge1 Ge 0.58153(5) 0.02253(9) 0.45821(12) 0.0121(3) Uani 1 1 d U . . Ge2 Ge 0.57968(5) 0.52349(9) 0.45472(12) 0.0124(3) Uani 1 1 d U . . Te6 Te 0.84662(3) 0.87921(6) 1.02955(7) 0.0168(2) Uani 1 1 d U . . Te8 Te 0.89524(4) 0.85961(7) 0.67768(7) 0.0186(2) Uani 1 1 d U . . Te4 Te 0.52084(3) 0.61114(6) 0.32405(6) 0.0163(2) Uani 1 1 d U . . Te7 Te 0.84522(3) 0.61729(6) 0.51807(7) 0.0170(2) Uani 1 1 d U . . Te1 Te 0.56751(3) -0.13411(6) 0.47656(7) 0.0162(2) Uani 1 1 d U . . Te3 Te 0.56829(3) 0.36603(6) 0.47609(7) 0.0177(2) Uani 1 1 d U . . Te5 Te 0.88390(4) 0.63138(6) 1.18766(7) 0.0203(2) Uani 1 1 d U . . Te2 Te 0.52725(3) 0.11622(6) 0.32444(6) 0.0173(2) Uani 1 1 d U . . 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 C11 0.013(5) 0.013(6) 0.022(6) 0.002(4) 0.007(4) -0.004(4) C63 0.026(7) 0.022(7) 0.024(7) -0.004(5) 0.009(6) 0.000(6) C64 0.024(7) 0.024(7) 0.017(6) 0.006(5) 0.008(6) 0.004(6) C22 0.015(5) 0.024(7) 0.024(6) 0.001(5) 0.003(5) 0.001(5) C31 0.011(5) 0.028(7) 0.026(6) 0.000(5) -0.001(5) 0.005(5) C53 0.016(6) 0.017(7) 0.021(6) -0.001(5) 0.008(5) 0.001(5) C34 0.021(7) 0.025(8) 0.028(7) -0.001(5) 0.016(6) 0.004(5) C23 0.030(8) 0.026(8) 0.026(7) -0.001(5) 0.018(6) -0.007(6) C42 0.015(6) 0.017(6) 0.028(6) -0.003(5) 0.008(5) -0.007(5) C52 0.015(6) 0.014(6) 0.012(5) 0.000(4) 0.002(4) 0.002(5) C51 0.013(6) 0.012(6) 0.015(5) 0.001(4) 0.003(4) 0.001(4) C41 0.021(6) 0.022(6) 0.019(5) -0.004(5) 0.009(5) -0.011(5) C54 0.017(7) 0.015(7) 0.030(7) 0.002(5) 0.009(6) 0.003(5) C21 0.016(6) 0.023(7) 0.029(6) -0.001(5) 0.015(5) -0.005(5) C32 0.020(6) 0.019(7) 0.022(6) 0.001(5) 0.010(5) -0.006(5) C12 0.013(5) 0.012(6) 0.019(5) 0.000(4) 0.006(4) -0.003(4) C13 0.019(3) 0.019(4) 0.028(4) -0.003(3) 0.014(3) -0.001(3) C43 0.019(3) 0.019(4) 0.028(4) -0.003(3) 0.014(3) -0.001(3) C33 0.019(3) 0.019(4) 0.028(4) -0.003(3) 0.014(3) -0.001(3) C14 0.013(5) 0.013(6) 0.015(5) 0.001(4) 0.005(4) -0.001(4) C44 0.019(6) 0.017(6) 0.025(6) 0.004(5) 0.009(5) -0.001(5) C24 0.014(5) 0.024(7) 0.024(6) 0.004(5) 0.007(5) -0.003(5) C62 0.021(7) 0.015(7) 0.025(7) -0.003(5) 0.002(6) 0.002(6) C61 0.026(7) 0.016(7) 0.027(7) -0.008(5) 0.006(6) 0.000(6) N21 0.013(4) 0.018(4) 0.017(4) -0.002(3) 0.011(3) 0.000(3) N22 0.013(4) 0.018(4) 0.014(3) 0.002(3) 0.008(3) 0.000(3) N23 0.020(5) 0.027(6) 0.018(5) -0.001(4) 0.013(4) -0.002(5) N24 0.024(6) 0.026(6) 0.021(5) 0.001(5) 0.013(5) 0.002(5) N13 0.009(4) 0.015(5) 0.015(4) 0.004(4) 0.004(4) 0.004(4) N14 0.011(5) 0.013(5) 0.013(4) 0.000(4) 0.003(4) 0.000(4) N11 0.013(4) 0.018(4) 0.017(4) -0.002(3) 0.011(3) 0.000(3) N12 0.013(4) 0.018(4) 0.014(3) 0.002(3) 0.008(3) 0.000(3) N100 0.025(4) 0.020(4) 0.034(4) -0.005(3) 0.014(3) -0.003(3) N101 0.025(4) 0.020(4) 0.034(4) -0.005(3) 0.014(3) -0.003(3) N102 0.023(3) 0.028(3) 0.032(3) 0.003(3) 0.014(3) 0.003(3) N103 0.023(3) 0.028(3) 0.032(3) 0.003(3) 0.014(3) 0.003(3) N104 0.023(3) 0.028(3) 0.032(3) 0.003(3) 0.014(3) 0.003(3) N105 0.0225(3) 0.0281(7) 0.0319(8) 0.0033(13) 0.0139(4) 0.0027(6) N106 0.043(5) 0.018(4) 0.028(4) -0.003(3) 0.011(3) 0.002(3) N107 0.043(5) 0.018(4) 0.028(4) -0.003(3) 0.011(3) 0.002(3) N108 0.027(4) 0.026(4) 0.029(4) 0.002(3) 0.010(3) -0.003(3) N109 0.027(4) 0.026(4) 0.029(4) 0.002(3) 0.010(3) -0.003(3) N110 0.029(6) 0.021(5) 0.036(6) 0.007(5) 0.016(5) 0.005(5) N111 0.023(5) 0.030(7) 0.028(5) 0.004(5) 0.008(4) -0.007(5) Ge4 0.0119(7) 0.0123(7) 0.0142(6) 0.0007(5) 0.0045(5) -0.0003(5) Ge3 0.0127(6) 0.0129(7) 0.0140(6) -0.0002(5) 0.0055(5) 0.0005(5) Ge1 0.0104(6) 0.0122(7) 0.0147(6) 0.0003(5) 0.0051(5) 0.0002(5) Ge2 0.0103(6) 0.0120(7) 0.0158(6) 0.0001(5) 0.0050(5) 0.0001(5) Te6 0.0185(4) 0.0131(4) 0.0207(5) 0.0011(4) 0.0087(4) -0.0031(4) Te8 0.0186(5) 0.0155(4) 0.0201(4) -0.0014(4) 0.0027(4) -0.0034(3) Te4 0.0155(5) 0.0153(4) 0.0174(4) 0.0001(3) 0.0031(4) 0.0036(3) Te7 0.0173(4) 0.0123(4) 0.0227(5) -0.0017(4) 0.0076(4) 0.0012(4) Te1 0.0177(4) 0.0123(4) 0.0207(4) 0.0013(4) 0.0089(3) 0.0010(4) Te3 0.0189(4) 0.0129(4) 0.0228(4) 0.0018(4) 0.0083(4) 0.0000(4) Te5 0.0248(6) 0.0178(4) 0.0180(4) 0.0010(4) 0.0053(4) 0.0077(4) Te2 0.0192(5) 0.0156(4) 0.0165(4) 0.0001(3) 0.0037(4) 0.0054(3) _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 C11 C31 1.52(2) . ? C11 C41 1.55(2) . ? C11 C21 1.553(18) . ? C11 Ge1 1.998(13) . ? C63 C53 1.45(2) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C54 1.47(2) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C22 C12 1.520(19) . ? C22 H22C 0.9800 . ? C22 H22D 0.9800 . ? C22 H22E 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C53 N13 1.299(19) . ? C53 C43 1.508(19) . ? C34 C14 1.492(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C23 C13 1.506(19) . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C42 C52 1.491(18) . ? C42 C12 1.563(19) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C52 N12 1.264(19) . ? C52 C62 1.52(2) . ? C51 N11 1.275(18) . ? C51 C41 1.503(18) . ? C51 C61 1.50(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C54 N14 1.314(19) . ? C54 C44 1.49(2) . ? C21 H21C 0.9800 . ? C21 H21D 0.9800 . ? C21 H21E 0.9800 . ? C32 C12 1.556(18) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C12 Ge2 2.001(13) . ? C13 C33 1.51(2) . ? C13 C43 1.53(2) . ? C13 Ge3 1.999(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C14 C44 1.52(2) . ? C14 C24 1.524(19) . ? C14 Ge4 2.021(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N21 N11 1.375(15) . ? N22 N12 1.385(14) . ? N23 N13 1.406(15) . ? N24 N14 1.390(16) . ? N13 Ge3 2.038(12) . ? N14 Ge4 2.033(11) . ? N11 Ge1 2.028(12) . ? N12 Ge2 2.027(12) . ? N100 N101 1.439(3) . ? N100 H101 0.9100 . ? N100 H102 0.9100 . ? N100 H103 0.9100 . ? N102 N103 1.441(3) . ? N104 N105 1.440(3) . ? N104 H141 0.9100 . ? N104 H142 0.9100 . ? N104 H143 0.9100 . ? N108 N109 1.440(3) . ? N109 H191 0.9100 . ? N109 H192 0.9100 . ? N109 H193 0.9100 . ? N110 N111 1.442(3) . ? N111 H111 0.9100 . ? N111 H112 0.9100 . ? N111 H113 0.9100 . ? Ge4 Te7 2.4684(19) . ? Ge4 Te8 2.513(2) . ? Ge3 Te6 2.4799(19) . ? Ge3 Te5 2.485(2) . ? Ge1 Te1 2.4810(19) . ? Ge1 Te2 2.4940(19) . ? Ge2 Te3 2.4827(19) . ? Ge2 Te4 2.5034(19) . ? 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 C31 C11 C41 111.0(12) . . ? C31 C11 C21 110.2(11) . . ? C41 C11 C21 112.3(11) . . ? C31 C11 Ge1 110.6(9) . . ? C41 C11 Ge1 101.8(8) . . ? C21 C11 Ge1 110.6(10) . . ? C53 C63 H63A 109.5 . . ? C53 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C53 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C54 C64 H64A 109.5 . . ? C54 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C54 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C12 C22 H22C 109.5 . . ? C12 C22 H22D 109.5 . . ? H22C C22 H22D 109.5 . . ? C12 C22 H22E 109.5 . . ? H22C C22 H22E 109.5 . . ? H22D C22 H22E 109.5 . . ? C11 C31 H31A 109.5 . . ? C11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N13 C53 C63 123.1(13) . . ? N13 C53 C43 112.5(13) . . ? C63 C53 C43 124.2(14) . . ? C14 C34 H34A 109.5 . . ? C14 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C14 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C13 C23 H23C 109.5 . . ? C13 C23 H23D 109.5 . . ? H23C C23 H23D 109.5 . . ? C13 C23 H23E 109.5 . . ? H23C C23 H23E 109.5 . . ? H23D C23 H23E 109.5 . . ? C52 C42 C12 110.4(11) . . ? C52 C42 H42A 109.6 . . ? C12 C42 H42A 109.6 . . ? C52 C42 H42B 109.6 . . ? C12 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? N12 C52 C42 116.8(13) . . ? N12 C52 C62 123.1(12) . . ? C42 C52 C62 120.0(13) . . ? N11 C51 C41 116.9(13) . . ? N11 C51 C61 122.7(12) . . ? C41 C51 C61 120.4(13) . . ? C51 C41 C11 110.7(12) . . ? C51 C41 H41A 109.5 . . ? C11 C41 H41A 109.5 . . ? C51 C41 H41B 109.5 . . ? C11 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? N14 C54 C64 121.7(13) . . ? N14 C54 C44 113.5(13) . . ? C64 C54 C44 124.8(13) . . ? C11 C21 H21C 109.5 . . ? C11 C21 H21D 109.5 . . ? H21C C21 H21D 109.5 . . ? C11 C21 H21E 109.5 . . ? H21C C21 H21E 109.5 . . ? H21D C21 H21E 109.5 . . ? C12 C32 H32A 109.5 . . ? C12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C22 C12 C32 109.9(11) . . ? C22 C12 C42 110.8(11) . . ? C32 C12 C42 112.5(11) . . ? C22 C12 Ge2 110.8(9) . . ? C32 C12 Ge2 111.2(9) . . ? C42 C12 Ge2 101.4(8) . . ? C23 C13 C33 111.1(12) . . ? C23 C13 C43 112.4(13) . . ? C33 C13 C43 109.7(13) . . ? C23 C13 Ge3 112.1(11) . . ? C33 C13 Ge3 109.3(10) . . ? C43 C13 Ge3 102.0(9) . . ? C53 C43 C13 113.2(13) . . ? C53 C43 H43A 108.9 . . ? C13 C43 H43A 108.9 . . ? C53 C43 H43B 108.9 . . ? C13 C43 H43B 108.9 . . ? H43A C43 H43B 107.8 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 C14 C44 113.8(12) . . ? C34 C14 C24 111.6(11) . . ? C44 C14 C24 109.5(11) . . ? C34 C14 Ge4 111.8(10) . . ? C44 C14 Ge4 102.1(8) . . ? C24 C14 Ge4 107.4(9) . . ? C54 C44 C14 114.1(13) . . ? C54 C44 H44A 108.7 . . ? C14 C44 H44A 108.7 . . ? C54 C44 H44B 108.7 . . ? C14 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C14 C24 H24C 109.5 . . ? C14 C24 H24D 109.5 . . ? H24C C24 H24D 109.5 . . ? C14 C24 H24E 109.5 . . ? H24C C24 H24E 109.5 . . ? H24D C24 H24E 109.5 . . ? C52 C62 H62A 109.5 . . ? C52 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C52 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N11 N21 H1 95(10) . . ? N11 N21 H2 105(10) . . ? H1 N21 H2 104(10) . . ? N12 N22 H5 113(10) . . ? N12 N22 H6 102(10) . . ? H5 N22 H6 103(10) . . ? N13 N23 H3 128(3) . . ? N13 N23 H4 102(10) . . ? H3 N23 H4 120(10) . . ? N14 N24 H7 107(10) . . ? N14 N24 H8 105(10) . . ? H7 N24 H8 125(10) . . ? C53 N13 N23 124.0(12) . . ? C53 N13 Ge3 114.2(9) . . ? N23 N13 Ge3 120.7(9) . . ? C54 N14 N24 124.9(12) . . ? C54 N14 Ge4 113.7(9) . . ? N24 N14 Ge4 120.5(9) . . ? C51 N11 N21 123.8(12) . . ? C51 N11 Ge1 111.8(8) . . ? N21 N11 Ge1 122.4(9) . . ? C52 N12 N22 123.9(12) . . ? C52 N12 Ge2 112.6(8) . . ? N22 N12 Ge2 122.0(9) . . ? N101 N100 H101 109.5 . . ? N101 N100 H102 109.5 . . ? H101 N100 H102 109.5 . . ? N101 N100 H103 109.5 . . ? H101 N100 H103 109.5 . . ? H102 N100 H103 109.5 . . ? N100 N101 H104 125.0(15) . . ? N103 N102 H121 111(10) . . ? N103 N102 H122 82(10) . . ? H121 N102 H122 88(10) . . ? N105 N104 H141 109.5 . . ? N105 N104 H142 109.5 . . ? H141 N104 H142 109.5 . . ? N105 N104 H143 109.5 . . ? H141 N104 H143 109.5 . . ? H142 N104 H143 109.5 . . ? N104 N105 H151 126.5(11) . . ? N107 N106 H161 87(10) . . ? N106 N107 H171 121.6(19) . . ? N109 N108 H181 124(2) . . ? N108 N109 H191 109.5 . . ? N108 N109 H192 109.5 . . ? H191 N109 H192 109.5 . . ? N108 N109 H193 109.5 . . ? H191 N109 H193 109.5 . . ? H192 N109 H193 109.5 . . ? N110 N111 H111 109.5 . . ? N110 N111 H112 109.5 . . ? H111 N111 H112 109.5 . . ? N110 N111 H113 109.5 . . ? H111 N111 H113 109.5 . . ? H112 N111 H113 109.5 . . ? C14 Ge4 N14 83.4(5) . . ? C14 Ge4 Te7 117.3(4) . . ? N14 Ge4 Te7 110.4(3) . . ? C14 Ge4 Te8 115.1(4) . . ? N14 Ge4 Te8 101.9(3) . . ? Te7 Ge4 Te8 120.27(7) . . ? C13 Ge3 N13 82.9(5) . . ? C13 Ge3 Te6 117.4(4) . . ? N13 Ge3 Te6 109.6(3) . . ? C13 Ge3 Te5 113.1(5) . . ? N13 Ge3 Te5 106.0(3) . . ? Te6 Ge3 Te5 120.37(8) . . ? C11 Ge1 N11 83.9(5) . . ? C11 Ge1 Te1 116.9(4) . . ? N11 Ge1 Te1 110.6(3) . . ? C11 Ge1 Te2 113.9(4) . . ? N11 Ge1 Te2 102.5(4) . . ? Te1 Ge1 Te2 121.04(7) . . ? C12 Ge2 N12 83.3(5) . . ? C12 Ge2 Te3 116.9(4) . . ? N12 Ge2 Te3 109.6(3) . . ? C12 Ge2 Te4 115.9(4) . . ? N12 Ge2 Te4 103.9(3) . . ? Te3 Ge2 Te4 119.44(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.78 _refine_diff_density_min -2.08 _refine_diff_density_rms 0.19