# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jian Zhou' _publ_contact_author_address ; Department of Chemistry and Biology, Yulin Normal University, Yulin 537000, PR China Yulin 537000 ; _publ_contact_author_email jianzhou888888@163.com _publ_author_name 'Jian Zhou' # Attachment '- 1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 823775' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ge S10 Sb4, C8 H26 Co N6, C8 H26 Co N6' _chemical_formula_sum 'C16 H52 Co2 Ge N12 S10 Sb4' _chemical_formula_weight 1410.73 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' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.684(3) _cell_length_b 17.133(4) _cell_length_c 33.478(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8422(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5352 _exptl_absorpt_coefficient_mu 4.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4493 _exptl_absorpt_correction_T_max 0.7130 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42078 _diffrn_reflns_av_R_equivalents 0.1152 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7457 _reflns_number_gt 6174 _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^)+(0.0000P)^2^+710.1786P] 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 7457 _refine_ls_number_parameters 434 _refine_ls_number_restraints 756 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.2334 _refine_ls_wR_factor_gt 0.2293 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.128 _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 Ge1 Ge 0.41434(15) 1.03725(12) 0.35959(6) 0.0283(5) Uani 1 1 d . A 1 Sb1 Sb 0.21680(10) 1.13070(9) 0.38912(4) 0.0328(3) Uani 1 1 d . . 1 Sb2 Sb 0.45091(10) 1.23691(8) 0.37431(4) 0.0288(3) Uani 1 1 d . A 1 Sb3 Sb 0.59917(10) 1.40623(8) 0.38196(4) 0.0316(3) Uani 1 1 d . A 1 Sb4 Sb 0.42675(9) 1.48899(7) 0.45283(4) 0.0274(3) Uani 1 1 d . . 1 S1 S 0.4697(4) 0.9273(3) 0.34064(16) 0.0362(12) Uani 1 1 d . A 1 S2 S 0.3016(4) 1.0132(3) 0.40472(17) 0.0405(14) Uani 1 1 d . A 1 S3 S 0.3537(4) 1.1155(3) 0.31599(15) 0.0341(12) Uani 1 1 d . A 1 S4 S 0.5200(4) 1.1105(3) 0.39086(17) 0.0399(14) Uani 1 1 d . A 1 S5 S 0.3148(4) 1.2284(3) 0.41995(16) 0.0377(13) Uani 1 1 d . A 1 S6 S 0.5365(4) 1.3048(3) 0.42730(14) 0.0298(11) Uani 1 1 d . A 1 S7 S 0.6016(4) 1.3272(4) 0.32372(16) 0.0421(14) Uani 1 1 d . A 1 S8 S 0.4627(5) 1.4809(4) 0.37286(16) 0.0462(15) Uani 1 1 d . A 1 S9 S 0.4148(4) 1.4936(3) 0.53559(14) 0.0308(11) Uani 1 1 d . . 1 S10 S 0.3765(4) 1.6276(3) 0.45087(17) 0.0422(15) Uani 1 1 d . . 1 Co1 Co 0.18425(18) 0.94540(14) 0.26050(7) 0.0239(6) Uani 1 1 d . B 1 Co2 Co 0.6079(2) 1.78900(17) 0.44606(12) 0.0481(9) Uani 1 1 d D C 1 N1 N 0.0527(13) 0.8888(10) 0.2559(6) 0.042(2) Uani 1 1 d U B 1 H1A H 0.0216 0.8961 0.2787 0.050 Uiso 1 1 calc R B 1 H1B H 0.0207 0.9111 0.2360 0.050 Uiso 1 1 calc R B 1 N2 N 0.2249(13) 0.8285(10) 0.2398(6) 0.042(2) Uani 1 1 d U B 1 H2A H 0.2621 0.8347 0.2183 0.050 Uiso 1 1 calc R B 1 N3 N 0.2283(14) 0.8984(11) 0.3155(5) 0.043(2) Uani 1 1 d U B 1 H3A H 0.2780 0.9248 0.3236 0.052 Uiso 1 1 calc R B 1 H3B H 0.1844 0.9061 0.3339 0.052 Uiso 1 1 calc R B 1 N4 N 0.3178(13) 0.9818(10) 0.2406(5) 0.040(2) Uani 1 1 d U B 1 H4A H 0.3475 1.0043 0.2611 0.048 Uiso 1 1 calc R B 1 H4B H 0.3498 0.9395 0.2330 0.048 Uiso 1 1 calc R B 1 N5 N 0.1501(13) 1.0182(10) 0.2073(5) 0.038(2) Uani 1 1 d U B 1 H5A H 0.1050 0.9938 0.1934 0.045 Uiso 1 1 calc R B 1 N6 N 0.1315(13) 1.0498(10) 0.2887(5) 0.038(2) Uani 1 1 d U B 1 H6A H 0.0993 1.0369 0.3106 0.046 Uiso 1 1 calc R B 1 H6B H 0.1779 1.0807 0.2963 0.046 Uiso 1 1 calc R B 1 N7 N 0.5393(18) 1.7313(14) 0.3964(7) 0.072(3) Uani 1 1 d U C 1 H7C H 0.4951 1.6996 0.4057 0.087 Uiso 1 1 calc R C 1 H7D H 0.5137 1.7670 0.3802 0.087 Uiso 1 1 calc R C 1 N8 N 0.7314(18) 1.7358(13) 0.4193(7) 0.070(3) Uani 1 1 d U C 1 H8C H 0.7789 1.7699 0.4199 0.084 Uiso 1 1 calc R C 1 N9 N 0.6299(18) 1.6936(13) 0.4853(7) 0.070(3) Uani 1 1 d U C 1 H9A H 0.6131 1.7069 0.5103 0.084 Uiso 1 1 calc R C 1 H9B H 0.5958 1.6526 0.4776 0.084 Uiso 1 1 calc R C 1 N10 N 0.572(2) 1.9116(12) 0.4328(16) 0.071(3) Uani 0.46(2) 1 d PDU C 1 N11 N 0.704(3) 1.8576(15) 0.4830(14) 0.071(3) Uani 0.46(2) 1 d PDU C 1 N12 N 0.491(3) 1.7958(18) 0.4877(13) 0.072(3) Uani 0.46(2) 1 d PDU C 1 C1 C 0.0606(15) 0.8071(13) 0.2483(7) 0.047(3) Uani 1 1 d DU B 1 H1C H 0.0583 0.7792 0.2735 0.057 Uiso 1 1 calc R B 1 H1D H 0.0092 0.7902 0.2323 0.057 Uiso 1 1 calc R B 1 C2 C 0.1471(15) 0.7868(14) 0.2270(7) 0.047(3) Uani 1 1 d DU B 1 H2B H 0.1386 0.7961 0.1987 0.056 Uiso 1 1 calc R B 1 H2C H 0.1586 0.7314 0.2305 0.056 Uiso 1 1 calc R B 1 C3 C 0.2811(17) 0.7932(14) 0.2733(7) 0.045(2) Uani 1 1 d U B 1 H3C H 0.2786 0.7367 0.2713 0.053 Uiso 1 1 calc R B 1 H3D H 0.3442 0.8088 0.2700 0.053 Uiso 1 1 calc R B 1 C4 C 0.2497(18) 0.8170(13) 0.3143(7) 0.045(3) Uani 1 1 d U B 1 H4C H 0.1962 0.7870 0.3215 0.053 Uiso 1 1 calc R B 1 H4D H 0.2971 0.8057 0.3336 0.053 Uiso 1 1 calc R B 1 C5 C 0.3133(16) 1.0366(13) 0.2073(7) 0.040(3) Uani 1 1 d U B 1 H5B H 0.3674 1.0316 0.1909 0.048 Uiso 1 1 calc R B 1 H5C H 0.3106 1.0896 0.2175 0.048 Uiso 1 1 calc R B 1 C6 C 0.2302(15) 1.0198(13) 0.1828(6) 0.039(2) Uani 1 1 d U B 1 H6C H 0.2235 1.0596 0.1624 0.047 Uiso 1 1 calc R B 1 H6D H 0.2373 0.9698 0.1695 0.047 Uiso 1 1 calc R B 1 C7 C 0.1164(16) 1.0958(13) 0.2198(6) 0.040(3) Uani 1 1 d U B 1 H7A H 0.0714 1.1143 0.2009 0.047 Uiso 1 1 calc R B 1 H7B H 0.1665 1.1327 0.2202 0.047 Uiso 1 1 calc R B 1 C8 C 0.0743(16) 1.0909(13) 0.2611(6) 0.040(3) Uani 1 1 d U B 1 H8A H 0.0634 1.1433 0.2711 0.049 Uiso 1 1 calc R B 1 H8B H 0.0160 1.0645 0.2593 0.049 Uiso 1 1 calc R B 1 C9 C 0.606(2) 1.6869(17) 0.3751(10) 0.073(3) Uani 1 1 d U C 1 H9C H 0.5895 1.6864 0.3471 0.088 Uiso 1 1 calc R C 1 H9D H 0.6036 1.6335 0.3846 0.088 Uiso 1 1 calc R C 1 C10 C 0.708(2) 1.7149(17) 0.3781(9) 0.072(3) Uani 1 1 d U C 1 H10A H 0.7485 1.6735 0.3690 0.086 Uiso 1 1 calc R C 1 H10B H 0.7175 1.7598 0.3609 0.086 Uiso 1 1 calc R C 1 C11 C 0.752(2) 1.6648(16) 0.4438(9) 0.071(3) Uani 1 1 d U C 1 H11A H 0.7214 1.6201 0.4320 0.085 Uiso 1 1 calc R C 1 H11B H 0.8168 1.6549 0.4432 0.085 Uiso 1 1 calc R C 1 C12 C 0.723(2) 1.6729(17) 0.4849(9) 0.071(3) Uani 1 1 d U C 1 H12A H 0.7313 1.6240 0.4990 0.085 Uiso 1 1 calc R C 1 H12B H 0.7583 1.7128 0.4981 0.085 Uiso 1 1 calc R C 1 C13 C 0.656(2) 1.9551(15) 0.4351(8) 0.072(3) Uani 1 1 d DU C 1 C14 C 0.690(2) 1.9400(14) 0.4784(8) 0.073(3) Uani 1 1 d DU C 1 C15 C 0.480(2) 1.9312(16) 0.4548(8) 0.074(3) Uani 1 1 d DU C 1 C16 C 0.460(2) 1.8741(14) 0.4894(8) 0.074(3) Uani 1 1 d DU C 1 N10' N 0.648(3) 1.8885(15) 0.4076(9) 0.071(3) Uani 0.54(2) 1 d PDU C 2 N11' N 0.640(3) 1.8739(19) 0.4938(8) 0.071(3) Uani 0.54(2) 1 d PDU C 2 N12' N 0.4666(16) 1.832(2) 0.4522(10) 0.072(3) Uani 0.54(2) 1 d PDU 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 Ge1 0.0275(12) 0.0337(11) 0.0237(10) -0.0055(9) 0.0025(9) -0.0053(9) Sb1 0.0323(8) 0.0402(8) 0.0259(7) -0.0050(6) 0.0070(6) -0.0067(7) Sb2 0.0323(8) 0.0349(7) 0.0192(6) 0.0043(5) -0.0019(6) -0.0075(6) Sb3 0.0321(8) 0.0403(8) 0.0225(7) 0.0033(6) 0.0015(6) -0.0130(6) Sb4 0.0299(7) 0.0229(6) 0.0294(7) 0.0029(5) -0.0086(6) -0.0027(6) S1 0.041(3) 0.034(3) 0.034(3) -0.006(2) 0.000(2) -0.002(2) S2 0.054(4) 0.032(3) 0.035(3) -0.004(2) 0.014(3) -0.010(3) S3 0.035(3) 0.040(3) 0.027(3) -0.002(2) -0.010(2) -0.002(2) S4 0.041(3) 0.040(3) 0.039(3) 0.005(2) -0.020(3) -0.011(3) S5 0.041(3) 0.040(3) 0.032(3) -0.007(2) 0.009(2) -0.013(3) S6 0.041(3) 0.029(3) 0.020(2) 0.0032(19) -0.002(2) -0.008(2) S7 0.045(4) 0.052(3) 0.029(3) -0.004(2) 0.012(3) -0.006(3) S8 0.069(4) 0.048(3) 0.022(3) 0.003(2) -0.012(3) 0.011(3) S9 0.029(3) 0.038(3) 0.025(2) -0.002(2) 0.002(2) -0.008(2) S10 0.054(4) 0.031(3) 0.042(3) -0.006(2) -0.031(3) 0.004(3) Co1 0.0261(14) 0.0257(13) 0.0199(13) -0.0025(10) 0.0010(11) 0.0012(11) Co2 0.0254(16) 0.0218(14) 0.097(3) 0.0025(16) 0.0038(17) -0.0020(12) N1 0.044(5) 0.040(4) 0.041(4) -0.004(4) 0.000(4) -0.001(4) N2 0.044(5) 0.041(4) 0.041(4) -0.004(4) 0.000(4) -0.001(4) N3 0.046(5) 0.043(4) 0.042(4) -0.003(4) 0.002(4) -0.002(4) N4 0.042(5) 0.039(4) 0.037(4) -0.003(4) 0.002(4) -0.001(4) N5 0.041(5) 0.037(4) 0.035(4) -0.002(4) 0.000(4) 0.000(4) N6 0.043(5) 0.037(5) 0.036(5) -0.005(4) 0.001(4) -0.001(4) N7 0.087(7) 0.054(5) 0.075(6) 0.006(5) 0.004(6) -0.028(5) N8 0.085(7) 0.052(5) 0.072(6) 0.003(5) 0.005(6) -0.027(5) N9 0.086(7) 0.052(5) 0.073(6) 0.005(5) 0.005(6) -0.027(5) N10 0.087(7) 0.053(5) 0.074(6) 0.006(5) 0.003(6) -0.025(6) N11 0.087(7) 0.053(5) 0.074(6) 0.005(5) 0.003(6) -0.026(5) N12 0.087(7) 0.054(6) 0.074(6) 0.006(5) 0.004(6) -0.026(6) C1 0.048(5) 0.045(5) 0.050(5) -0.005(5) 0.000(5) -0.002(5) C2 0.048(5) 0.045(5) 0.048(5) -0.007(5) 0.000(5) -0.001(5) C3 0.047(5) 0.043(5) 0.044(5) -0.003(4) 0.002(4) 0.001(4) C4 0.046(5) 0.043(5) 0.044(5) -0.002(5) -0.001(5) -0.002(5) C5 0.043(6) 0.040(5) 0.036(5) -0.001(5) 0.000(5) 0.000(5) C6 0.042(5) 0.040(5) 0.036(5) -0.001(4) 0.001(4) 0.000(5) C7 0.043(5) 0.039(5) 0.036(5) -0.002(4) 0.000(5) -0.001(5) C8 0.044(5) 0.039(5) 0.038(5) -0.002(5) 0.001(5) 0.001(5) C9 0.089(7) 0.056(6) 0.075(6) 0.004(5) 0.004(6) -0.029(6) C10 0.087(7) 0.055(6) 0.074(6) 0.004(5) 0.005(6) -0.028(6) C11 0.085(7) 0.053(6) 0.075(6) 0.004(5) 0.005(6) -0.026(6) C12 0.087(7) 0.053(6) 0.073(6) 0.004(5) 0.002(6) -0.025(6) C13 0.088(7) 0.052(6) 0.075(6) 0.007(5) 0.002(6) -0.026(6) C14 0.088(7) 0.054(6) 0.076(6) 0.008(5) 0.001(6) -0.024(6) C15 0.089(7) 0.056(5) 0.076(6) 0.006(5) 0.003(6) -0.024(6) C16 0.089(7) 0.056(6) 0.077(6) 0.006(5) 0.004(6) -0.024(6) N10' 0.087(7) 0.053(5) 0.074(6) 0.006(5) 0.002(6) -0.026(5) N11' 0.087(7) 0.053(5) 0.074(6) 0.005(5) 0.003(6) -0.025(5) N12' 0.088(7) 0.053(5) 0.075(6) 0.006(5) 0.003(6) -0.026(5) _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 Ge1 S1 2.147(6) . ? Ge1 S3 2.173(6) . ? Ge1 S4 2.254(6) . ? Ge1 S2 2.279(6) . ? Sb1 S2 2.424(6) . ? Sb1 S5 2.437(6) . ? Sb1 S10 2.480(5) 7_655 ? Sb2 S4 2.455(6) . ? Sb2 S6 2.466(5) . ? Sb2 S5 2.520(6) . ? Sb3 S7 2.374(6) . ? Sb3 S8 2.397(7) . ? Sb3 S6 2.484(5) . ? Sb4 S9 2.377(5) 5_686 ? Sb4 S10 2.488(6) . ? Sb4 S8 2.732(6) . ? Sb4 S9 2.777(5) . ? S9 Sb4 2.377(5) 5_686 ? S10 Sb1 2.480(5) 7_665 ? Co1 N3 2.112(19) . ? Co1 N4 2.163(19) . ? Co1 N6 2.166(17) . ? Co1 N1 2.167(19) . ? Co1 N2 2.202(18) . ? Co1 N5 2.232(18) . ? Co2 N9 2.12(2) . ? Co2 N7 2.18(2) . ? Co2 N10 2.21(2) . ? Co2 N12 2.22(2) . ? Co2 N11 2.22(2) . ? Co2 N8 2.22(3) . ? N1 C1 1.43(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.41(3) . ? N2 C3 1.52(3) . ? N2 H2A 0.9100 . ? N3 C4 1.43(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5 1.46(3) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C6 1.43(3) . ? N5 C7 1.48(3) . ? N5 H5A 0.9100 . ? N6 C8 1.43(3) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C9 1.44(4) . ? N7 H7C 0.9000 . ? N7 H7D 0.9000 . ? N8 C10 1.47(3) . ? N8 C11 1.50(4) . ? N8 H8C 0.9100 . ? N9 C12 1.41(4) . ? N9 H9A 0.9000 . ? N9 H9B 0.9000 . ? N10 C13 1.452(19) . ? N10 C15 1.56(5) . ? N11 C14 1.435(19) . ? N12 C16 1.418(18) . ? C1 C2 1.497(17) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.50(3) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.50(3) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.52(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.58(4) . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.45(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.554(18) . ? C15 C16 1.546(18) . ? 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 S1 Ge1 S3 119.9(2) . . ? S1 Ge1 S4 111.4(2) . . ? S3 Ge1 S4 104.5(2) . . ? S1 Ge1 S2 108.2(2) . . ? S3 Ge1 S2 105.0(2) . . ? S4 Ge1 S2 107.0(2) . . ? S2 Sb1 S5 100.1(2) . . ? S2 Sb1 S10 94.9(2) . 7_655 ? S5 Sb1 S10 89.30(19) . 7_655 ? S4 Sb2 S6 92.48(18) . . ? S4 Sb2 S5 98.0(2) . . ? S6 Sb2 S5 89.73(18) . . ? S7 Sb3 S8 102.3(2) . . ? S7 Sb3 S6 96.22(19) . . ? S8 Sb3 S6 98.1(2) . . ? S9 Sb4 S10 100.1(2) 5_686 . ? S9 Sb4 S8 88.70(19) 5_686 . ? S10 Sb4 S8 94.58(19) . . ? S9 Sb4 S9 84.01(17) 5_686 . ? S10 Sb4 S9 88.89(18) . . ? S8 Sb4 S9 172.37(19) . . ? Ge1 S2 Sb1 94.6(2) . . ? Ge1 S4 Sb2 95.8(2) . . ? Sb1 S5 Sb2 104.6(2) . . ? Sb2 S6 Sb3 94.55(17) . . ? Sb3 S8 Sb4 93.66(18) . . ? Sb4 S9 Sb4 95.99(17) 5_686 . ? Sb1 S10 Sb4 101.90(19) 7_665 . ? N3 Co1 N4 95.8(7) . . ? N3 Co1 N6 92.6(7) . . ? N4 Co1 N6 102.7(7) . . ? N3 Co1 N1 99.5(7) . . ? N4 Co1 N1 156.2(7) . . ? N6 Co1 N1 94.7(7) . . ? N3 Co1 N2 81.0(7) . . ? N4 Co1 N2 85.4(7) . . ? N6 Co1 N2 170.2(7) . . ? N1 Co1 N2 79.2(7) . . ? N3 Co1 N5 168.0(7) . . ? N4 Co1 N5 78.2(7) . . ? N6 Co1 N5 78.8(7) . . ? N1 Co1 N5 89.6(7) . . ? N2 Co1 N5 108.6(7) . . ? N9 Co2 N7 101.1(9) . . ? N9 Co2 N10 153.2(16) . . ? N7 Co2 N10 99.5(14) . . ? N9 Co2 N12 76.6(12) . . ? N7 Co2 N12 98.4(16) . . ? N10 Co2 N12 83.7(15) . . ? N9 Co2 N11 88.1(11) . . ? N7 Co2 N11 163.9(17) . . ? N10 Co2 N11 76.3(13) . . ? N12 Co2 N11 97(2) . . ? N9 Co2 N8 79.0(9) . . ? N7 Co2 N8 83.3(10) . . ? N10 Co2 N8 120.4(13) . . ? N12 Co2 N8 155.4(11) . . ? N11 Co2 N8 85.5(15) . . ? C1 N1 Co1 112.3(14) . . ? C1 N1 H1A 109.2 . . ? Co1 N1 H1A 109.2 . . ? C1 N1 H1B 109.2 . . ? Co1 N1 H1B 109.2 . . ? H1A N1 H1B 107.9 . . ? C2 N2 C3 117.5(19) . . ? C2 N2 Co1 109.7(14) . . ? C3 N2 Co1 106.1(13) . . ? C2 N2 H2A 107.7 . . ? C3 N2 H2A 107.7 . . ? Co1 N2 H2A 107.7 . . ? C4 N3 Co1 114.4(15) . . ? C4 N3 H3A 108.7 . . ? Co1 N3 H3A 108.7 . . ? C4 N3 H3B 108.7 . . ? Co1 N3 H3B 108.7 . . ? H3A N3 H3B 107.6 . . ? C5 N4 Co1 112.3(14) . . ? C5 N4 H4A 109.1 . . ? Co1 N4 H4A 109.1 . . ? C5 N4 H4B 109.1 . . ? Co1 N4 H4B 109.1 . . ? H4A N4 H4B 107.9 . . ? C6 N5 C7 114.8(18) . . ? C6 N5 Co1 106.5(13) . . ? C7 N5 Co1 110.5(13) . . ? C6 N5 H5A 108.3 . . ? C7 N5 H5A 108.3 . . ? Co1 N5 H5A 108.3 . . ? C8 N6 Co1 109.6(13) . . ? C8 N6 H6A 109.7 . . ? Co1 N6 H6A 109.7 . . ? C8 N6 H6B 109.7 . . ? Co1 N6 H6B 109.7 . . ? H6A N6 H6B 108.2 . . ? C9 N7 Co2 108(2) . . ? C9 N7 H7C 110.2 . . ? Co2 N7 H7C 110.2 . . ? C9 N7 H7D 110.2 . . ? Co2 N7 H7D 110.2 . . ? H7C N7 H7D 108.5 . . ? C10 N8 C11 111(2) . . ? C10 N8 Co2 107(2) . . ? C11 N8 Co2 106.0(18) . . ? C10 N8 H8C 110.8 . . ? C11 N8 H8C 110.8 . . ? Co2 N8 H8C 110.8 . . ? C12 N9 Co2 109.6(18) . . ? C12 N9 H9A 109.8 . . ? Co2 N9 H9A 109.8 . . ? C12 N9 H9B 109.8 . . ? Co2 N9 H9B 109.8 . . ? H9A N9 H9B 108.2 . . ? C13 N10 C15 127(3) . . ? C13 N10 Co2 105.7(17) . . ? C15 N10 Co2 108(2) . . ? C14 N11 Co2 111.6(18) . . ? C16 N12 Co2 109(2) . . ? C2 C1 N1 112.4(19) . . ? C2 C1 H1C 109.1 . . ? N1 C1 H1C 109.1 . . ? C2 C1 H1D 109.1 . . ? N1 C1 H1D 109.1 . . ? H1C C1 H1D 107.9 . . ? C1 C2 N2 115.1(19) . . ? C1 C2 H2B 108.5 . . ? N2 C2 H2B 108.5 . . ? C1 C2 H2C 108.5 . . ? N2 C2 H2C 108.5 . . ? H2B C2 H2C 107.5 . . ? C4 C3 N2 113.4(19) . . ? C4 C3 H3C 108.9 . . ? N2 C3 H3C 108.9 . . ? C4 C3 H3D 108.9 . . ? N2 C3 H3D 108.9 . . ? H3C C3 H3D 107.7 . . ? N3 C4 C3 111(2) . . ? N3 C4 H4C 109.4 . . ? C3 C4 H4C 109.4 . . ? N3 C4 H4D 109.4 . . ? C3 C4 H4D 109.4 . . ? H4C C4 H4D 108.0 . . ? N4 C5 C6 109.4(19) . . ? N4 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? N4 C5 H5C 109.8 . . ? C6 C5 H5C 109.8 . . ? H5B C5 H5C 108.2 . . ? N5 C6 C5 110.9(18) . . ? N5 C6 H6C 109.5 . . ? C5 C6 H6C 109.5 . . ? N5 C6 H6D 109.5 . . ? C5 C6 H6D 109.5 . . ? H6C C6 H6D 108.1 . . ? N5 C7 C8 110.2(18) . . ? N5 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N5 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N6 C8 C7 112.0(19) . . ? N6 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N6 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N7 C9 C10 117(2) . . ? N7 C9 H9C 107.9 . . ? C10 C9 H9C 107.9 . . ? N7 C9 H9D 107.9 . . ? C10 C9 H9D 107.9 . . ? H9C C9 H9D 107.2 . . ? N8 C10 C9 111(3) . . ? N8 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 N8 113(3) . . ? C12 C11 H11A 109.1 . . ? N8 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? N8 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N9 C12 C11 109(3) . . ? N9 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N9 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N10 C13 C14 104(3) . . ? N11 C14 C13 108(3) . . ? C16 C15 N10 113(3) . . ? N12 C16 C15 120(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.072 _refine_diff_density_min -1.906 _refine_diff_density_rms 0.296 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 830619' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ge S6 Sb2, C6 H24 Mn N6 ' _chemical_formula_sum 'C6 H24 Ge Mn N6 S6 Sb2 ' _chemical_formula_weight 743.80 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' Mn Mn 0.3368 0.7283 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall ' -P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3741(12) _cell_length_b 17.6065(15) _cell_length_c 18.5620(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4370.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 4.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6123 _exptl_absorpt_correction_T_max 0.7235 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22156 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3884 _reflns_number_gt 3507 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0000P)^2^+5.2329P] 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 3884 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 Sb1 Sb -0.23645(2) -0.599515(15) -0.194165(17) 0.02854(11) Uani 1 1 d . . . Sb2 Sb -0.00962(2) -0.522444(17) -0.095894(18) 0.03264(11) Uani 1 1 d . . . Ge1 Ge 0.00516(3) -0.61479(3) -0.27683(3) 0.02804(13) Uani 1 1 d . . . S1 S -0.01849(8) -0.66039(6) -0.16691(6) 0.0304(2) Uani 1 1 d . . . S2 S 0.01536(10) -0.59962(6) 0.00831(7) 0.0382(3) Uani 1 1 d . . . S3 S -0.19321(10) -0.50893(7) -0.10033(7) 0.0426(3) Uani 1 1 d . . . S4 S -0.13776(9) -0.54866(8) -0.29496(7) 0.0429(3) Uani 1 1 d . . . S5 S 0.11876(9) -0.52059(6) -0.27179(9) 0.0486(4) Uani 1 1 d . . . S6 S 0.04627(9) -0.69553(7) -0.35749(7) 0.0442(3) Uani 1 1 d . . . Mn1 Mn 0.22111(5) -0.69137(4) -0.59734(4) 0.03344(18) Uani 1 1 d . . . N3 N 0.2039(3) -0.5654(2) -0.5689(2) 0.0384(9) Uani 1 1 d . . . H3A H 0.2515 -0.5518 -0.5371 0.046 Uiso 1 1 calc R . . H3B H 0.2114 -0.5369 -0.6088 0.046 Uiso 1 1 calc R . . N2 N 0.3591(3) -0.6682(2) -0.6660(3) 0.0531(12) Uani 1 1 d . . . H2A H 0.3774 -0.6193 -0.6618 0.064 Uiso 1 1 calc R . . H2B H 0.4103 -0.6976 -0.6513 0.064 Uiso 1 1 calc R . . N5 N 0.2275(3) -0.8195(2) -0.5880(2) 0.0403(10) Uani 1 1 d . . . H5A H 0.1656 -0.8381 -0.5808 0.048 Uiso 1 1 calc R . . H5B H 0.2516 -0.8395 -0.6291 0.048 Uiso 1 1 calc R . . N4 N 0.0609(3) -0.6844(2) -0.5548(3) 0.0434(10) Uani 1 1 d . . . H4A H 0.0212 -0.7174 -0.5784 0.052 Uiso 1 1 calc R . . H4B H 0.0591 -0.6953 -0.5075 0.052 Uiso 1 1 calc R . . N1 N 0.1586(3) -0.6843(3) -0.7126(2) 0.0494(11) Uani 1 1 d . . . H1A H 0.1381 -0.7306 -0.7268 0.059 Uiso 1 1 calc R . . H1B H 0.1055 -0.6529 -0.7134 0.059 Uiso 1 1 calc R . . N6 N 0.2901(4) -0.7096(2) -0.4865(3) 0.0599(13) Uani 1 1 d . . . H6A H 0.3556 -0.6981 -0.4879 0.072 Uiso 1 1 calc R . . H6B H 0.2604 -0.6788 -0.4543 0.072 Uiso 1 1 calc R . . C4 C 0.0276(4) -0.6055(3) -0.5677(3) 0.0448(12) Uani 1 1 d . . . H4C H -0.0364 -0.5970 -0.5445 0.054 Uiso 1 1 calc R . . H4D H 0.0197 -0.5968 -0.6189 0.054 Uiso 1 1 calc R . . C6 C 0.2770(4) -0.7894(3) -0.4646(3) 0.0522(14) Uani 1 1 d . . . H6C H 0.2102 -0.7966 -0.4455 0.063 Uiso 1 1 calc R . . H6D H 0.3245 -0.8016 -0.4268 0.063 Uiso 1 1 calc R . . C5 C 0.2927(4) -0.8409(3) -0.5269(3) 0.0481(13) Uani 1 1 d . . . H5C H 0.3621 -0.8385 -0.5420 0.058 Uiso 1 1 calc R . . H5D H 0.2783 -0.8928 -0.5126 0.058 Uiso 1 1 calc R . . C3 C 0.1045(4) -0.5518(3) -0.5374(3) 0.0452(12) Uani 1 1 d . . . H3C H 0.0842 -0.4999 -0.5473 0.054 Uiso 1 1 calc R . . H3D H 0.1080 -0.5581 -0.4856 0.054 Uiso 1 1 calc R . . C2 C 0.3340(5) -0.6856(3) -0.7418(3) 0.0597(16) Uani 1 1 d . . . H2C H 0.3841 -0.6633 -0.7731 0.072 Uiso 1 1 calc R . . H2D H 0.3354 -0.7402 -0.7488 0.072 Uiso 1 1 calc R . . C1 C 0.2346(4) -0.6564(4) -0.7621(3) 0.0570(15) Uani 1 1 d . . . H1C H 0.2353 -0.6013 -0.7613 0.068 Uiso 1 1 calc R . . H1D H 0.2186 -0.6726 -0.8108 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.02587(16) 0.03056(17) 0.0292(2) 0.00131(12) -0.00048(11) -0.00356(10) Sb2 0.03767(18) 0.03398(18) 0.0263(2) 0.00078(12) -0.00155(12) -0.00583(11) Ge1 0.0226(2) 0.0334(2) 0.0281(3) -0.0006(2) 0.00242(17) -0.00116(16) S1 0.0380(5) 0.0285(5) 0.0247(7) -0.0001(4) -0.0026(4) 0.0019(4) S2 0.0564(7) 0.0311(5) 0.0272(7) -0.0036(5) -0.0110(5) 0.0042(5) S3 0.0433(7) 0.0538(7) 0.0308(7) -0.0136(5) -0.0111(5) 0.0146(5) S4 0.0333(6) 0.0622(8) 0.0333(8) 0.0173(6) 0.0060(5) 0.0131(5) S5 0.0308(6) 0.0339(6) 0.0813(11) -0.0088(6) 0.0188(6) -0.0056(5) S6 0.0449(7) 0.0570(7) 0.0308(7) -0.0138(6) 0.0058(5) 0.0014(5) Mn1 0.0380(4) 0.0331(4) 0.0291(4) -0.0005(3) -0.0013(3) 0.0032(3) N3 0.043(2) 0.0315(19) 0.041(3) 0.0006(17) -0.0013(19) 0.0005(16) N2 0.038(2) 0.045(2) 0.076(4) -0.016(2) 0.004(2) -0.0015(18) N5 0.046(2) 0.035(2) 0.040(3) -0.0065(18) -0.0006(18) 0.0013(17) N4 0.044(2) 0.0358(19) 0.050(3) -0.0051(19) 0.0097(19) -0.0044(17) N1 0.050(2) 0.064(3) 0.034(3) -0.001(2) -0.0016(19) -0.004(2) N6 0.082(3) 0.048(2) 0.050(3) -0.003(2) -0.028(3) 0.003(2) C4 0.038(3) 0.047(3) 0.049(4) -0.002(2) 0.006(2) 0.002(2) C6 0.053(3) 0.061(3) 0.042(4) 0.011(3) -0.007(2) 0.009(3) C5 0.051(3) 0.040(3) 0.054(4) 0.010(2) 0.002(3) 0.006(2) C3 0.054(3) 0.039(2) 0.042(3) -0.006(2) 0.008(2) 0.001(2) C2 0.072(4) 0.053(3) 0.054(4) -0.012(3) 0.030(3) 0.000(3) C1 0.076(4) 0.062(4) 0.033(4) 0.005(3) 0.005(3) -0.006(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 Sb1 S3 2.4315(12) . ? Sb1 S4 2.4585(12) . ? Sb1 S5 2.4658(12) 6 ? Sb2 S2 2.3873(13) . ? Sb2 S3 2.4682(13) . ? Sb2 S2 2.6959(12) 5_545 ? Sb2 S1 2.7659(11) . ? Ge1 S6 2.1365(13) . ? Ge1 S1 2.2153(13) . ? Ge1 S5 2.2511(12) . ? Ge1 S4 2.2633(12) . ? S2 Sb2 2.6959(12) 5_545 ? S5 Sb1 2.4658(12) 6_655 ? Mn1 N5 2.265(4) . ? Mn1 N6 2.277(5) . ? Mn1 N2 2.280(5) . ? Mn1 N4 2.287(4) . ? Mn1 N3 2.292(4) . ? Mn1 N1 2.301(4) . ? N3 C3 1.471(6) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N2 C2 1.478(8) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N5 C5 1.479(7) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N4 C4 1.477(6) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N1 C1 1.455(7) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N6 C6 1.473(7) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C4 C3 1.506(7) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C6 C5 1.486(8) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C2 C1 1.475(8) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? 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 S3 Sb1 S4 100.29(5) . . ? S3 Sb1 S5 90.04(5) . 6 ? S4 Sb1 S5 91.22(5) . 6 ? S2 Sb2 S3 102.77(5) . . ? S2 Sb2 S2 88.23(4) . 5_545 ? S3 Sb2 S2 85.12(4) . 5_545 ? S2 Sb2 S1 83.82(4) . . ? S3 Sb2 S1 91.50(4) . . ? S2 Sb2 S1 170.47(4) 5_545 . ? S6 Ge1 S1 116.17(5) . . ? S6 Ge1 S5 110.22(5) . . ? S1 Ge1 S5 108.97(6) . . ? S6 Ge1 S4 117.09(6) . . ? S1 Ge1 S4 101.70(4) . . ? S5 Ge1 S4 101.37(5) . . ? Ge1 S1 Sb2 96.58(4) . . ? Sb2 S2 Sb2 91.77(4) . 5_545 ? Sb1 S3 Sb2 101.37(4) . . ? Ge1 S4 Sb1 98.80(5) . . ? Ge1 S5 Sb1 95.98(4) . 6_655 ? N5 Mn1 N6 77.00(16) . . ? N5 Mn1 N2 100.98(16) . . ? N6 Mn1 N2 101.7(2) . . ? N5 Mn1 N4 93.57(14) . . ? N6 Mn1 N4 94.33(19) . . ? N2 Mn1 N4 160.38(17) . . ? N5 Mn1 N3 161.87(17) . . ? N6 Mn1 N3 88.21(16) . . ? N2 Mn1 N3 92.15(15) . . ? N4 Mn1 N3 76.95(13) . . ? N5 Mn1 N1 97.99(16) . . ? N6 Mn1 N1 174.27(17) . . ? N2 Mn1 N1 76.36(17) . . ? N4 Mn1 N1 88.72(17) . . ? N3 Mn1 N1 97.22(16) . . ? C3 N3 Mn1 109.9(3) . . ? C3 N3 H3A 109.7 . . ? Mn1 N3 H3A 109.7 . . ? C3 N3 H3B 109.7 . . ? Mn1 N3 H3B 109.7 . . ? H3A N3 H3B 108.2 . . ? C2 N2 Mn1 108.1(3) . . ? C2 N2 H2A 110.1 . . ? Mn1 N2 H2A 110.1 . . ? C2 N2 H2B 110.1 . . ? Mn1 N2 H2B 110.1 . . ? H2A N2 H2B 108.4 . . ? C5 N5 Mn1 109.6(3) . . ? C5 N5 H5A 109.8 . . ? Mn1 N5 H5A 109.8 . . ? C5 N5 H5B 109.8 . . ? Mn1 N5 H5B 109.8 . . ? H5A N5 H5B 108.2 . . ? C4 N4 Mn1 106.1(3) . . ? C4 N4 H4A 110.5 . . ? Mn1 N4 H4A 110.5 . . ? C4 N4 H4B 110.5 . . ? Mn1 N4 H4B 110.5 . . ? H4A N4 H4B 108.7 . . ? C1 N1 Mn1 110.6(4) . . ? C1 N1 H1A 109.5 . . ? Mn1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? Mn1 N1 H1B 109.5 . . ? H1A N1 H1B 108.1 . . ? C6 N6 Mn1 109.7(3) . . ? C6 N6 H6A 109.7 . . ? Mn1 N6 H6A 109.7 . . ? C6 N6 H6B 109.7 . . ? Mn1 N6 H6B 109.7 . . ? H6A N6 H6B 108.2 . . ? N4 C4 C3 109.0(4) . . ? N4 C4 H4C 109.9 . . ? C3 C4 H4C 109.9 . . ? N4 C4 H4D 109.9 . . ? C3 C4 H4D 109.9 . . ? H4C C4 H4D 108.3 . . ? N6 C6 C5 110.5(5) . . ? N6 C6 H6C 109.6 . . ? C5 C6 H6C 109.6 . . ? N6 C6 H6D 109.6 . . ? C5 C6 H6D 109.6 . . ? H6C C6 H6D 108.1 . . ? N5 C5 C6 111.0(4) . . ? N5 C5 H5C 109.4 . . ? C6 C5 H5C 109.4 . . ? N5 C5 H5D 109.4 . . ? C6 C5 H5D 109.4 . . ? H5C C5 H5D 108.0 . . ? N3 C3 C4 111.5(4) . . ? N3 C3 H3C 109.3 . . ? C4 C3 H3C 109.3 . . ? N3 C3 H3D 109.3 . . ? C4 C3 H3D 109.3 . . ? H3C C3 H3D 108.0 . . ? C1 C2 N2 112.1(4) . . ? C1 C2 H2C 109.2 . . ? N2 C2 H2C 109.2 . . ? C1 C2 H2D 109.2 . . ? N2 C2 H2D 109.2 . . ? H2C C2 H2D 107.9 . . ? N1 C1 C2 110.5(5) . . ? N1 C1 H1C 109.6 . . ? C2 C1 H1C 109.6 . . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 . . ? H1C C1 H1D 108.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.038 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.158