Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cameron Evans' 'Kenneth M. Mackay' 'Brian K. Nicholson' _publ_contact_author_name 'Prof B Nicholson' _publ_contact_author_address ; Prof B Nicholson Department of Chemistry University of Waikato Private Bag 3105 Hamilton NEW ZEALAND ; data_cegecoa _database_code_CSD 158417 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2[C8 H20 N2], C24 Co10 Ge2 O24, 1.5[C H2 Cl2], 0.5[C4 H10 O]' _chemical_formula_sum 'C43.50 H48 Cl3 Co10 Ge2 N2 O24.50' _chemical_formula_weight 1831.67 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pcca' 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, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 30.3922(6) _cell_length_b 23.5597(5) _cell_length_c 17.2684(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12364.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7232 _exptl_absorpt_coefficient_mu 3.769 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Seimens SMART CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74629 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10909 _reflns_number_gt 8077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. Refinement was complicated by the presence of solvent and disorder. The compound was modelled as follows: The [Ge2Co10(CO)24]2- anion was fully ordered and was completely refined anisotropically. One complete cation in the asymmetric unit was disordered and was refined with half-occupancy carbon atoms, but was otherwise well behaved. One half-cation (on a two-fold axis) was ordered and well behaved One half cation (on a different two-fold axis) was disordered and refined with half-occupancy carbon atoms. One CH2Cl2 molecule was ordered and behaved well Another half CH2Cl2 (on a two-fold axis) was well-behaved. One other solvent molecule lying on a two-fold axis was very poorly ordered. It was modelled as a half-diethylether molecule, but did not refine sensibly. No H atoms were included because of the disorder in the species containing H 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^)+(0.0698P)^2^+116.3046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens not included _refine_ls_hydrogen_treatment not included _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10909 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.16162(3) 0.24846(3) 0.89631(4) 0.02374(18) Uani 1 1 d . . . Ge2 Ge 0.11969(3) 0.23187(3) 1.04646(4) 0.02576(19) Uani 1 1 d . . . Co1 Co 0.11052(3) 0.30038(4) 0.81811(6) 0.0275(2) Uani 1 1 d . . . Co2 Co 0.12023(3) 0.18776(4) 0.81500(6) 0.0288(2) Uani 1 1 d . . . Co3 Co 0.18855(4) 0.24936(4) 0.76634(6) 0.0295(3) Uani 1 1 d . . . Co4 Co 0.07792(3) 0.24128(4) 0.92884(6) 0.0268(2) Uani 1 1 d . . . Co5 Co 0.13168(3) 0.32536(4) 0.96674(6) 0.0252(2) Uani 1 1 d . . . Co6 Co 0.19623(3) 0.24915(4) 1.02091(6) 0.0262(2) Uani 1 1 d . . . Co7 Co 0.14382(3) 0.16009(4) 0.95755(6) 0.0272(2) Uani 1 1 d . . . Co8 Co 0.14747(4) 0.31124(4) 1.11590(6) 0.0294(3) Uani 1 1 d . . . Co9 Co 0.06581(3) 0.30579(4) 1.05401(6) 0.0288(2) Uani 1 1 d . . . Co10 Co 0.08989(4) 0.23353(5) 1.17179(6) 0.0332(3) Uani 1 1 d . . . O11 O 0.1175(2) 0.4237(3) 0.8168(4) 0.0554(18) Uani 1 1 d . . . O12 O 0.0834(2) 0.2906(3) 0.6568(4) 0.0513(17) Uani 1 1 d . . . O21 O 0.0442(2) 0.1646(4) 0.7188(5) 0.071(2) Uani 1 1 d . . . O22 O 0.1680(2) 0.1369(3) 0.6915(4) 0.060(2) Uani 1 1 d . . . O23 O 0.1158(3) 0.0701(3) 0.8535(4) 0.061(2) Uani 1 1 d . . . O31 O 0.2687(2) 0.1854(3) 0.8027(4) 0.0524(17) Uani 1 1 d . . . O32 O 0.2212(2) 0.3637(3) 0.7970(4) 0.0561(18) Uani 1 1 d . . . O33 O 0.1804(2) 0.2617(3) 0.5975(3) 0.0530(17) Uani 1 1 d . . . O41 O 0.0156(2) 0.1479(3) 0.9241(4) 0.0518(17) Uani 1 1 d . . . O42 O 0.01719(19) 0.3098(3) 0.8388(4) 0.0484(17) Uani 1 1 d . . . O51 O 0.1918(2) 0.4209(3) 0.9567(4) 0.0485(16) Uani 1 1 d . . . O52 O 0.0644(2) 0.4118(3) 0.9704(4) 0.0463(16) Uani 1 1 d . . . O61 O 0.2771(2) 0.2760(4) 0.9372(4) 0.067(2) Uani 1 1 d . . . O62 O 0.2312(2) 0.1630(3) 1.1256(4) 0.0512(17) Uani 1 1 d . . . O63 O 0.2390(2) 0.3404(3) 1.1070(4) 0.0541(18) Uani 1 1 d . . . O71 O 0.0933(2) 0.0815(3) 1.0528(4) 0.0602(19) Uani 1 1 d . . . O72 O 0.2283(2) 0.1031(3) 0.9482(4) 0.0567(18) Uani 1 1 d . . . O81 O 0.1661(3) 0.2932(3) 1.2775(4) 0.0589(19) Uani 1 1 d . . . O82 O 0.1351(2) 0.4322(3) 1.1330(4) 0.0557(18) Uani 1 1 d . . . O91 O -0.0201(2) 0.2755(3) 0.9949(4) 0.0535(17) Uani 1 1 d . . . O92 O 0.0271(3) 0.3779(3) 1.1719(4) 0.061(2) Uani 1 1 d . . . O101 O 0.0512(3) 0.2850(3) 1.3112(4) 0.071(2) Uani 1 1 d . . . O102 O 0.1412(3) 0.1366(3) 1.2257(4) 0.066(2) Uani 1 1 d . . . O103 O 0.0110(2) 0.1754(3) 1.1174(4) 0.0600(19) Uani 1 1 d . . . C11 C 0.1156(3) 0.3751(4) 0.8229(5) 0.040(2) Uani 1 1 d . . . C12 C 0.0946(3) 0.2932(4) 0.7197(5) 0.0362(19) Uani 1 1 d . . . C22 C 0.1575(3) 0.1695(4) 0.7395(5) 0.041(2) Uani 1 1 d . . . C21 C 0.0734(3) 0.1740(4) 0.7577(5) 0.039(2) Uani 1 1 d . . . C23 C 0.1218(3) 0.1186(4) 0.8646(5) 0.039(2) Uani 1 1 d . . . C31 C 0.2377(3) 0.2099(4) 0.7888(5) 0.037(2) Uani 1 1 d . . . C32 C 0.2061(3) 0.3201(4) 0.7871(5) 0.037(2) Uani 1 1 d . . . C33 C 0.1835(3) 0.2574(4) 0.6627(5) 0.0353(19) Uani 1 1 d . . . C41 C 0.0397(3) 0.1848(4) 0.9246(5) 0.037(2) Uani 1 1 d . . . C42 C 0.0511(3) 0.2920(4) 0.8564(4) 0.0316(18) Uani 1 1 d . . . C51 C 0.1687(3) 0.3834(3) 0.9599(4) 0.0304(18) Uani 1 1 d . . . C52 C 0.0800(3) 0.3675(4) 0.9873(5) 0.0341(19) Uani 1 1 d . . . C61 C 0.2451(3) 0.2654(4) 0.9676(5) 0.042(2) Uani 1 1 d . . . C62 C 0.2173(3) 0.1968(4) 1.0854(5) 0.0352(19) Uani 1 1 d . . . C63 C 0.2071(3) 0.3146(4) 1.0920(5) 0.0362(19) Uani 1 1 d . . . C71 C 0.1135(3) 0.1136(4) 1.0174(5) 0.042(2) Uani 1 1 d . . . C72 C 0.1961(3) 0.1275(4) 0.9523(5) 0.037(2) Uani 1 1 d . . . C81 C 0.1536(3) 0.2940(4) 1.2142(5) 0.043(2) Uani 1 1 d . . . C82 C 0.1394(3) 0.3846(4) 1.1260(5) 0.0364(19) Uani 1 1 d . . . C91 C 0.0169(3) 0.2827(4) 1.0088(5) 0.046(2) Uani 1 1 d . . . C92 C 0.0433(3) 0.3489(4) 1.1277(5) 0.038(2) Uani 1 1 d . . . C101 C 0.0664(3) 0.2670(4) 1.2571(5) 0.042(2) Uani 1 1 d . . . C102 C 0.1219(3) 0.1761(4) 1.2060(5) 0.042(2) Uani 1 1 d . . . C103 C 0.0418(3) 0.2001(4) 1.1352(5) 0.045(2) Uani 1 1 d . . . N1 N 0.1206(2) 0.4194(3) 0.4669(4) 0.0368(16) Uiso 1 1 d . . . C1C C 0.1313(6) 0.4569(8) 0.5365(11) 0.044(4) Uiso 0.50 1 d P . . C1C1 C 0.1296(6) 0.3769(8) 0.5311(11) 0.044(4) Uiso 0.50 1 d P . . C1D C 0.1591(6) 0.4573(8) 0.4512(11) 0.047(5) Uiso 0.50 1 d P . . C1D1 C 0.1589(7) 0.3769(10) 0.4456(13) 0.062(6) Uiso 0.50 1 d P . . C1E C 0.1140(7) 0.4620(10) 0.4011(13) 0.063(6) Uiso 0.50 1 d P . . C1E1 C 0.1080(7) 0.3826(9) 0.3970(12) 0.054(5) Uiso 0.50 1 d P . . C1F C 0.0830(6) 0.4596(8) 0.4887(11) 0.049(5) Uiso 0.50 1 d P . . C1F1 C 0.0804(7) 0.3834(9) 0.4805(13) 0.060(6) Uiso 0.50 1 d P . . C2C C 0.1436(4) 0.4124(5) 0.6098(7) 0.074(3) Uiso 1 1 d . . . C2D C 0.2019(5) 0.4157(7) 0.4297(9) 0.102(5) Uiso 1 1 d . . . C2E C 0.0989(4) 0.4238(6) 0.3238(8) 0.083(4) Uiso 1 1 d . . . C2F C 0.0391(5) 0.4235(6) 0.4979(9) 0.091(4) Uiso 1 1 d . . . N2 N 0.2500 0.0000 0.7218(7) 0.046(3) Uani 1 2 d S . . C1A C 0.2345(3) -0.0493(4) 0.7699(7) 0.057(3) Uani 1 1 d . . . C1B C 0.2120(4) 0.0237(5) 0.6712(7) 0.062(3) Uani 1 1 d . . . C2A C 0.1986(4) -0.0341(5) 0.8316(7) 0.066(3) Uani 1 1 d . . . C2B C 0.1944(4) -0.0202(5) 0.6127(8) 0.078(4) Uani 1 1 d . . . N3 N 0.0000 0.0088(5) 0.2500 0.061(3) Uiso 1 2 d S . . C1G1 C -0.0363(8) -0.0315(10) 0.2699(14) 0.070 Uiso 0.50 1 d P . . C1G2 C 0.0391(8) 0.0495(10) 0.2397(14) 0.070 Uiso 0.50 1 d P . . C1H1 C -0.0133(8) -0.0147(11) 0.0890(15) 0.070 Uiso 0.50 1 d P . . C1H2 C 0.0077(8) 0.0496(10) 0.3191(14) 0.070 Uiso 0.50 1 d P . . C2G C -0.0797(4) 0.0143(5) 0.2838(7) 0.070 Uiso 1 1 d . . . C2H C -0.0186(4) 0.0157(6) 0.1112(7) 0.070 Uiso 1 1 d . . . O110 O 0.2500 0.5000 0.0984(6) 0.034(2) Uiso 1 2 d S . . C1I C 0.2411(5) 0.4825(6) 0.1154(8) 0.078(4) Uiso 1 1 d . . . C2I C 0.2155(3) 0.5004(4) 0.2575(6) 0.047(2) Uiso 1 1 d . . . Cl1 Cl 0.0331(2) 0.4759(3) 0.6945(4) 0.166(2) Uiso 1 1 d . . . C99 C 0.0000 0.4304(11) 0.7500 0.117(8) Uiso 1 2 d S . . Cl2 Cl 0.0982(3) 0.0919(4) 0.5219(5) 0.208(3) Uiso 1 1 d . . . Cl3 Cl 0.1236(3) 0.1910(4) 0.4298(5) 0.219(3) Uiso 1 1 d . . . C98 C 0.0938(7) 0.1656(9) 0.5095(12) 0.135(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0248(4) 0.0250(4) 0.0214(4) -0.0007(3) -0.0009(3) 0.0002(3) Ge2 0.0288(4) 0.0265(4) 0.0220(4) 0.0010(3) 0.0003(3) 0.0014(3) Co1 0.0293(6) 0.0300(5) 0.0231(5) 0.0034(4) -0.0012(4) 0.0004(4) Co2 0.0317(6) 0.0293(6) 0.0254(5) -0.0025(4) -0.0030(4) -0.0030(4) Co3 0.0311(6) 0.0343(6) 0.0231(5) -0.0018(4) 0.0028(4) -0.0003(5) Co4 0.0267(5) 0.0292(6) 0.0245(5) 0.0027(4) -0.0017(4) -0.0017(4) Co5 0.0270(5) 0.0246(5) 0.0241(5) 0.0003(4) 0.0014(4) 0.0012(4) Co6 0.0269(6) 0.0290(5) 0.0226(5) -0.0005(4) -0.0025(4) 0.0015(4) Co7 0.0319(6) 0.0231(5) 0.0264(5) 0.0010(4) -0.0009(4) 0.0001(4) Co8 0.0357(6) 0.0291(6) 0.0233(5) -0.0033(4) -0.0006(4) 0.0009(4) Co9 0.0303(6) 0.0300(6) 0.0260(5) 0.0026(4) 0.0037(4) 0.0042(4) Co10 0.0408(6) 0.0340(6) 0.0249(6) 0.0059(5) 0.0054(5) 0.0054(5) O11 0.082(5) 0.031(4) 0.054(4) 0.005(3) -0.003(4) -0.003(3) O12 0.045(4) 0.076(5) 0.033(4) 0.006(3) -0.006(3) 0.000(3) O21 0.056(5) 0.093(6) 0.065(5) -0.006(4) -0.026(4) -0.019(4) O22 0.061(4) 0.048(4) 0.072(5) -0.024(4) 0.025(4) -0.005(3) O23 0.094(6) 0.028(3) 0.061(4) -0.003(3) -0.029(4) -0.012(3) O31 0.042(4) 0.060(4) 0.056(4) -0.010(3) -0.003(3) 0.013(3) O32 0.068(5) 0.040(4) 0.061(5) -0.003(3) 0.014(4) -0.015(3) O33 0.063(5) 0.073(5) 0.023(3) 0.002(3) 0.000(3) -0.003(4) O41 0.049(4) 0.050(4) 0.056(4) -0.001(3) -0.006(3) -0.019(3) O42 0.031(3) 0.071(5) 0.044(4) 0.026(3) 0.002(3) 0.009(3) O51 0.049(4) 0.042(4) 0.055(4) -0.008(3) 0.006(3) -0.018(3) O52 0.044(4) 0.038(3) 0.057(4) 0.015(3) 0.012(3) 0.011(3) O61 0.039(4) 0.123(7) 0.038(4) -0.002(4) 0.005(3) -0.024(4) O62 0.069(5) 0.041(4) 0.044(4) 0.006(3) -0.021(3) 0.004(3) O63 0.041(4) 0.047(4) 0.074(5) -0.024(3) -0.007(3) -0.004(3) O71 0.068(5) 0.041(4) 0.072(5) 0.019(4) 0.011(4) -0.011(3) O72 0.048(4) 0.061(4) 0.062(4) -0.015(4) 0.000(3) 0.020(4) O81 0.081(5) 0.071(5) 0.025(4) 0.001(3) -0.006(3) -0.004(4) O82 0.070(5) 0.036(4) 0.061(4) -0.005(3) 0.005(4) 0.009(3) O91 0.046(4) 0.065(4) 0.049(4) 0.006(3) 0.000(3) -0.009(3) O92 0.081(5) 0.059(4) 0.043(4) -0.008(3) 0.025(4) 0.021(4) O101 0.087(6) 0.079(5) 0.046(4) -0.013(4) 0.024(4) 0.014(5) O102 0.081(5) 0.050(4) 0.068(5) 0.012(4) -0.007(4) 0.025(4) O103 0.055(5) 0.058(4) 0.066(5) 0.013(4) 0.002(4) -0.014(4) C11 0.033(5) 0.049(6) 0.037(5) 0.005(4) -0.001(4) 0.002(4) C12 0.034(5) 0.044(5) 0.030(5) 0.002(4) -0.003(4) -0.002(4) C22 0.040(5) 0.041(5) 0.041(5) -0.004(4) 0.006(4) 0.003(4) C21 0.044(5) 0.043(5) 0.030(5) 0.002(4) 0.001(4) -0.006(4) C23 0.047(5) 0.039(5) 0.030(4) -0.004(4) -0.014(4) -0.001(4) C31 0.035(5) 0.039(5) 0.035(5) -0.005(4) 0.008(4) -0.007(4) C32 0.041(5) 0.046(5) 0.025(4) 0.003(4) 0.007(4) 0.001(4) C33 0.033(5) 0.039(5) 0.034(5) -0.005(4) 0.005(4) -0.006(4) C41 0.033(5) 0.050(5) 0.028(4) 0.004(4) -0.004(4) -0.006(4) C42 0.034(5) 0.041(5) 0.020(4) 0.003(3) 0.001(3) 0.001(4) C51 0.035(4) 0.032(4) 0.025(4) -0.002(3) -0.002(3) 0.006(4) C52 0.029(4) 0.040(5) 0.033(5) 0.005(4) 0.000(3) 0.003(4) C61 0.038(5) 0.058(6) 0.029(5) 0.000(4) -0.013(4) -0.002(4) C62 0.039(5) 0.039(5) 0.028(4) -0.005(4) -0.002(4) -0.003(4) C63 0.037(5) 0.035(5) 0.036(5) -0.005(4) -0.007(4) 0.008(4) C71 0.047(5) 0.036(5) 0.044(5) 0.000(4) -0.007(4) 0.002(4) C72 0.047(5) 0.032(4) 0.031(5) -0.001(4) 0.000(4) 0.000(4) C81 0.049(6) 0.039(5) 0.042(6) -0.008(4) 0.006(4) 0.005(4) C82 0.044(5) 0.036(5) 0.030(4) 0.000(4) 0.002(4) 0.004(4) C91 0.048(6) 0.048(6) 0.041(5) 0.010(4) -0.007(4) -0.007(4) C92 0.037(5) 0.043(5) 0.035(5) 0.007(4) 0.003(4) 0.000(4) C101 0.043(5) 0.043(5) 0.040(5) 0.011(4) 0.000(4) 0.001(4) C102 0.050(6) 0.042(5) 0.034(5) 0.007(4) 0.006(4) 0.011(4) C103 0.053(6) 0.044(5) 0.036(5) 0.010(4) 0.010(4) 0.001(5) N2 0.047(6) 0.025(5) 0.065(7) 0.000 0.000 0.003(5) C1A 0.061(7) 0.032(5) 0.078(8) 0.008(5) 0.004(6) -0.003(5) C1B 0.063(7) 0.051(6) 0.071(7) 0.000(5) -0.020(6) 0.005(5) C2A 0.054(7) 0.067(7) 0.077(8) 0.018(6) 0.013(6) -0.006(5) C2B 0.078(8) 0.073(8) 0.083(9) -0.013(7) -0.020(7) -0.013(7) _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 Co5 2.3643(12) . ? Ge1 Co2 2.3662(13) . ? Ge1 Co3 2.3890(12) . ? Ge1 Co1 2.3940(12) . ? Ge1 Co6 2.3951(12) . ? Ge1 Co7 2.3971(13) . ? Ge1 Co4 2.6107(13) . ? Ge1 Ge2 2.9155(11) . ? Ge2 Co10 2.3463(13) . ? Ge2 Co8 2.3765(13) . ? Ge2 Co9 2.3939(13) . ? Ge2 Co7 2.3990(13) . ? Ge2 Co6 2.4026(13) . ? Ge2 Co4 2.4055(13) . ? Ge2 Co5 2.6230(12) . ? Co1 C11 1.770(10) . ? Co1 C12 1.775(8) . ? Co1 C42 1.934(8) . ? Co1 Co4 2.5645(14) . ? Co1 Co2 2.6701(15) . ? Co1 Co5 2.7106(14) . ? Co1 Co3 2.8050(15) . ? Co2 C21 1.764(9) . ? Co2 C22 1.779(9) . ? Co2 C23 1.842(9) . ? Co2 Co7 2.6454(14) . ? Co2 Co4 2.6663(15) . ? Co2 Co3 2.6688(15) . ? Co3 C32 1.787(10) . ? Co3 C31 1.800(10) . ? Co3 C33 1.806(9) . ? Co3 C22 2.154(9) . ? Co4 C41 1.769(9) . ? Co4 C42 1.913(8) . ? Co4 C91 2.509(10) . ? Co4 Co5 2.6499(14) . ? Co4 Co9 2.6677(14) . ? Co4 Co7 2.8137(14) . ? Co5 C51 1.774(9) . ? Co5 C52 1.892(8) . ? Co5 Co9 2.5477(14) . ? Co5 Co8 2.6412(14) . ? Co5 Co6 2.8194(14) . ? Co6 C62 1.781(9) . ? Co6 C61 1.789(10) . ? Co6 C63 1.999(8) . ? Co6 Co8 2.6507(14) . ? Co6 Co7 2.8526(14) . ? Co7 C71 1.766(10) . ? Co7 C72 1.767(9) . ? Co7 C23 1.995(8) . ? Co8 C82 1.753(9) . ? Co8 C81 1.754(10) . ? Co8 C63 1.861(9) . ? Co8 Co9 2.7052(15) . ? Co8 Co10 2.7104(15) . ? Co9 C92 1.765(9) . ? Co9 C91 1.765(10) . ? Co9 C52 1.905(8) . ? Co9 Co10 2.7514(14) . ? Co10 C102 1.768(9) . ? Co10 C103 1.777(11) . ? Co10 C101 1.817(10) . ? Co10 C81 2.514(10) . ? O11 C11 1.151(11) . ? O12 C12 1.141(10) . ? O21 C21 1.134(10) . ? O22 C22 1.174(10) . ? O23 C23 1.173(10) . ? O31 C31 1.133(10) . ? O32 C32 1.137(10) . ? O33 C33 1.135(10) . ? O41 C41 1.137(10) . ? O42 C42 1.152(9) . ? O51 C51 1.129(9) . ? O52 C52 1.182(10) . ? O61 C61 1.133(11) . ? O62 C62 1.137(10) . ? O63 C63 1.171(10) . ? O71 C71 1.150(11) . ? O72 C72 1.137(10) . ? O81 C81 1.159(11) . ? O82 C82 1.136(10) . ? O91 C91 1.163(10) . ? O92 C92 1.138(10) . ? O101 C101 1.126(11) . ? O102 C102 1.151(10) . ? O103 C103 1.144(11) . ? N1 C1D 1.50(2) . ? N1 C1F1 1.51(2) . ? N1 C1C1 1.517(19) . ? N1 C1C 1.526(19) . ? N1 C1E 1.53(2) . ? N1 C1F 1.53(2) . ? N1 C1E1 1.53(2) . ? N1 C1D1 1.58(2) . ? C1C C1F 1.68(3) . ? C1C C2C 1.68(2) . ? C1C C1D 1.70(3) . ? C1C C1C1 1.89(3) . ? C1C1 C2C 1.65(2) . ? C1C1 C1D1 1.72(3) . ? C1C1 C1F1 1.74(3) . ? C1D C1E 1.63(3) . ? C1D C2D 1.67(2) . ? C1D C1D1 1.90(3) . ? C1D1 C2D 1.62(3) . ? C1D1 C1E1 1.76(3) . ? C1E C2E 1.67(3) . ? C1E C1F 1.78(3) . ? C1E C1E1 1.88(3) . ? C1E1 C2E 1.62(2) . ? C1E1 C1F1 1.67(3) . ? C1F C2F 1.59(2) . ? C1F C1F1 1.80(3) . ? C1F1 C2F 1.60(3) . ? N2 C1A 1.505(11) 2 ? N2 C1A 1.505(11) . ? N2 C1B 1.553(12) . ? N2 C1B 1.553(12) 2 ? C1A C2A 1.567(15) . ? C1B C2B 1.541(15) . ? N3 C1G1 1.49(2) 3 ? N3 C1G1 1.49(2) . ? N3 C1G2 1.54(2) . ? N3 C1G2 1.54(2) 3 ? N3 C1H2 1.55(3) . ? N3 C1H2 1.55(3) 3 ? C1G1 C2G 1.72(3) . ? C1G1 C1G2 1.92(3) 3 ? C1G2 C2G 1.54(3) 3 ? C1G2 C1H2 1.67(3) . ? C1G2 C1H2 1.75(3) 3 ? C1G2 C1G1 1.92(3) 3 ? C1H1 C2H 0.83(2) . ? C1H2 C2H 1.48(3) 3 ? C1H2 C1G2 1.75(3) 3 ? C2G C1G2 1.54(3) 3 ? C2H C1H2 1.48(3) 3 ? O110 C1I 0.574(15) 2_565 ? O110 C1I 0.574(15) . ? C1I C1I 0.99(3) 2_565 ? Cl1 C99 1.756(16) . ? C99 Cl1 1.756(16) 3_556 ? Cl2 C98 1.75(2) . ? Cl3 C98 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Co5 Ge1 Co2 124.32(5) . . ? Co5 Ge1 Co3 127.47(5) . . ? Co2 Ge1 Co3 68.28(4) . . ? Co5 Ge1 Co1 69.45(4) . . ? Co2 Ge1 Co1 68.24(4) . . ? Co3 Ge1 Co1 71.81(4) . . ? Co5 Ge1 Co6 72.65(4) . . ? Co2 Ge1 Co6 140.41(5) . . ? Co3 Ge1 Co6 133.90(5) . . ? Co1 Ge1 Co6 142.02(5) . . ? Co5 Ge1 Co7 110.60(5) . . ? Co2 Ge1 Co7 67.47(4) . . ? Co3 Ge1 Co7 119.96(5) . . ? Co1 Ge1 Co7 123.11(5) . . ? Co6 Ge1 Co7 73.06(4) . . ? Co5 Ge1 Co4 64.14(4) . . ? Co2 Ge1 Co4 64.57(4) . . ? Co3 Ge1 Co4 122.45(5) . . ? Co1 Ge1 Co4 61.47(4) . . ? Co6 Ge1 Co4 103.60(4) . . ? Co7 Ge1 Co4 68.22(4) . . ? Co5 Ge1 Ge2 58.47(3) . . ? Co2 Ge1 Ge2 102.38(4) . . ? Co3 Ge1 Ge2 170.55(4) . . ? Co1 Ge1 Ge2 106.66(4) . . ? Co6 Ge1 Ge2 52.69(3) . . ? Co7 Ge1 Ge2 52.59(3) . . ? Co4 Ge1 Ge2 51.24(3) . . ? Co10 Ge2 Co8 70.04(4) . . ? Co10 Ge2 Co9 70.95(4) . . ? Co8 Ge2 Co9 69.09(4) . . ? Co10 Ge2 Co7 136.06(5) . . ? Co8 Ge2 Co7 140.26(5) . . ? Co9 Ge2 Co7 139.18(5) . . ? Co10 Ge2 Co6 122.70(5) . . ? Co8 Ge2 Co6 67.37(4) . . ? Co9 Ge2 Co6 123.30(5) . . ? Co7 Ge2 Co6 72.90(4) . . ? Co10 Ge2 Co4 125.00(5) . . ? Co8 Ge2 Co4 122.75(5) . . ? Co9 Ge2 Co4 67.54(4) . . ? Co7 Ge2 Co4 71.70(4) . . ? Co6 Ge2 Co4 109.90(5) . . ? Co10 Ge2 Co5 121.58(5) . . ? Co8 Ge2 Co5 63.56(4) . . ? Co9 Ge2 Co5 60.83(4) . . ? Co7 Ge2 Co5 102.33(4) . . ? Co6 Ge2 Co5 68.09(4) . . ? Co4 Ge2 Co5 63.43(4) . . ? Co10 Ge2 Ge1 170.67(5) . . ? Co8 Ge2 Ge1 100.83(4) . . ? Co9 Ge2 Ge1 104.47(4) . . ? Co7 Ge2 Ge1 52.53(3) . . ? Co6 Ge2 Ge1 52.46(3) . . ? Co4 Ge2 Ge1 57.82(3) . . ? Co5 Ge2 Ge1 50.20(3) . . ? C11 Co1 C12 99.4(4) . . ? C11 Co1 C42 99.6(4) . . ? C12 Co1 C42 93.6(4) . . ? C11 Co1 Ge1 115.2(3) . . ? C12 Co1 Ge1 131.9(3) . . ? C42 Co1 Ge1 111.2(2) . . ? C11 Co1 Co4 122.6(3) . . ? C12 Co1 Co4 123.8(3) . . ? C42 Co1 Co4 47.8(2) . . ? Ge1 Co1 Co4 63.43(4) . . ? C11 Co1 Co2 168.6(3) . . ? C12 Co1 Co2 85.2(3) . . ? C42 Co1 Co2 90.5(2) . . ? Ge1 Co1 Co2 55.39(4) . . ? Co4 Co1 Co2 61.20(4) . . ? C11 Co1 Co5 73.7(3) . . ? C12 Co1 Co5 172.7(3) . . ? C42 Co1 Co5 85.4(2) . . ? Ge1 Co1 Co5 54.76(3) . . ? Co4 Co1 Co5 60.23(4) . . ? Co2 Co1 Co5 102.04(4) . . ? C11 Co1 Co3 111.6(3) . . ? C12 Co1 Co3 83.4(3) . . ? C42 Co1 Co3 148.7(3) . . ? Ge1 Co1 Co3 54.01(3) . . ? Co4 Co1 Co3 109.37(5) . . ? Co2 Co1 Co3 58.28(4) . . ? Co5 Co1 Co3 101.20(4) . . ? C21 Co2 C22 93.4(4) . . ? C21 Co2 C23 96.8(4) . . ? C22 Co2 C23 96.4(4) . . ? C21 Co2 Ge1 150.8(3) . . ? C22 Co2 Ge1 104.0(3) . . ? C23 Co2 Ge1 104.2(3) . . ? C21 Co2 Co7 134.0(3) . . ? C22 Co2 Co7 116.7(3) . . ? C23 Co2 Co7 48.9(2) . . ? Ge1 Co2 Co7 56.82(4) . . ? C21 Co2 Co4 96.4(3) . . ? C22 Co2 Co4 164.0(3) . . ? C23 Co2 Co4 95.1(3) . . ? Ge1 Co2 Co4 62.16(4) . . ? Co7 Co2 Co4 63.97(4) . . ? C21 Co2 Co3 123.5(3) . . ? C22 Co2 Co3 53.5(3) . . ? C23 Co2 Co3 127.4(3) . . ? Ge1 Co2 Co3 56.26(4) . . ? Co7 Co2 Co3 102.48(5) . . ? Co4 Co2 Co3 110.50(5) . . ? C21 Co2 Co1 96.0(3) . . ? C22 Co2 Co1 109.0(3) . . ? C23 Co2 Co1 150.8(3) . . ? Ge1 Co2 Co1 56.38(4) . . ? Co7 Co2 Co1 104.84(5) . . ? Co4 Co2 Co1 57.45(4) . . ? Co3 Co2 Co1 63.39(4) . . ? C32 Co3 C31 101.0(4) . . ? C32 Co3 C33 97.3(4) . . ? C31 Co3 C33 109.8(4) . . ? C32 Co3 C22 171.3(4) . . ? C31 Co3 C22 87.6(4) . . ? C33 Co3 C22 80.9(4) . . ? C32 Co3 Ge1 85.5(3) . . ? C31 Co3 Ge1 94.4(3) . . ? C33 Co3 Ge1 154.5(3) . . ? C22 Co3 Ge1 92.5(2) . . ? C32 Co3 Co2 132.6(3) . . ? C31 Co3 Co2 107.2(3) . . ? C33 Co3 Co2 107.6(3) . . ? C22 Co3 Co2 41.6(2) . . ? Ge1 Co3 Co2 55.45(4) . . ? C32 Co3 Co1 77.8(3) . . ? C31 Co3 Co1 148.6(3) . . ? C33 Co3 Co1 101.4(3) . . ? C22 Co3 Co1 94.1(2) . . ? Ge1 Co3 Co1 54.18(3) . . ? Co2 Co3 Co1 58.33(4) . . ? C41 Co4 C42 99.4(4) . . ? C41 Co4 Ge2 108.2(3) . . ? C42 Co4 Ge2 146.6(3) . . ? C41 Co4 C91 80.2(4) . . ? C42 Co4 C91 78.6(3) . . ? Ge2 Co4 C91 87.8(2) . . ? C41 Co4 Co1 129.2(3) . . ? C42 Co4 Co1 48.5(2) . . ? Ge2 Co4 Co1 118.41(5) . . ? C91 Co4 Co1 119.0(2) . . ? C41 Co4 Ge1 132.9(3) . . ? C42 Co4 Ge1 103.6(2) . . ? Ge2 Co4 Ge1 70.94(4) . . ? C91 Co4 Ge1 144.4(2) . . ? Co1 Co4 Ge1 55.10(3) . . ? C41 Co4 Co5 167.9(3) . . ? C42 Co4 Co5 87.6(2) . . ? Ge2 Co4 Co5 62.29(4) . . ? C91 Co4 Co5 91.7(2) . . ? Co1 Co4 Co5 62.62(4) . . ? Ge1 Co4 Co5 53.41(3) . . ? C41 Co4 Co2 86.0(3) . . ? C42 Co4 Co2 91.1(2) . . ? Ge2 Co4 Co2 108.93(5) . . ? C91 Co4 Co2 161.1(2) . . ? Co1 Co4 Co2 61.35(4) . . ? Ge1 Co4 Co2 53.27(3) . . ? Co5 Co4 Co2 103.78(5) . . ? C41 Co4 Co9 111.8(3) . . ? C42 Co4 Co9 96.6(2) . . ? Ge2 Co4 Co9 56.03(4) . . ? C91 Co4 Co9 39.7(2) . . ? Co1 Co4 Co9 110.37(5) . . ? Ge1 Co4 Co9 105.77(4) . . ? Co5 Co4 Co9 57.25(4) . . ? Co2 Co4 Co9 158.96(5) . . ? C41 Co4 Co7 87.9(3) . . ? C42 Co4 Co7 147.5(2) . . ? Ge2 Co4 Co7 54.05(3) . . ? C91 Co4 Co7 133.9(2) . . ? Co1 Co4 Co7 103.02(5) . . ? Ge1 Co4 Co7 52.29(3) . . ? Co5 Co4 Co7 91.48(4) . . ? Co2 Co4 Co7 57.65(4) . . ? Co9 Co4 Co7 110.04(5) . . ? C51 Co5 C52 97.7(4) . . ? C51 Co5 Ge1 108.2(2) . . ? C52 Co5 Ge1 144.9(3) . . ? C51 Co5 Co9 132.6(2) . . ? C52 Co5 Co9 48.1(2) . . ? Ge1 Co5 Co9 117.91(5) . . ? C51 Co5 Ge2 140.3(2) . . ? C52 Co5 Ge2 103.1(3) . . ? Ge1 Co5 Ge2 71.33(4) . . ? Co9 Co5 Ge2 55.14(3) . . ? C51 Co5 Co8 92.7(2) . . ? C52 Co5 Co8 91.9(3) . . ? Ge1 Co5 Co8 109.58(5) . . ? Co9 Co5 Co8 62.82(4) . . ? Ge2 Co5 Co8 53.67(3) . . ? C51 Co5 Co4 161.9(2) . . ? C52 Co5 Co4 85.8(3) . . ? Ge1 Co5 Co4 62.45(4) . . ? Co9 Co5 Co4 61.73(4) . . ? Ge2 Co5 Co4 54.28(3) . . ? Co8 Co5 Co4 104.99(5) . . ? C51 Co5 Co1 104.8(2) . . ? C52 Co5 Co1 95.5(3) . . ? Ge1 Co5 Co1 55.79(3) . . ? Co9 Co5 Co1 109.54(5) . . ? Ge2 Co5 Co1 106.36(4) . . ? Co8 Co5 Co1 159.91(5) . . ? Co4 Co5 Co1 57.15(4) . . ? C51 Co5 Co6 94.1(2) . . ? C52 Co5 Co6 148.2(3) . . ? Ge1 Co5 Co6 54.18(3) . . ? Co9 Co5 Co6 103.60(4) . . ? Ge2 Co5 Co6 52.24(3) . . ? Co8 Co5 Co6 57.97(4) . . ? Co4 Co5 Co6 92.00(4) . . ? Co1 Co5 Co6 109.93(4) . . ? C62 Co6 C61 99.9(4) . . ? C62 Co6 C63 95.2(4) . . ? C61 Co6 C63 90.8(4) . . ? C62 Co6 Ge1 135.7(3) . . ? C61 Co6 Ge1 84.5(3) . . ? C63 Co6 Ge1 129.0(2) . . ? C62 Co6 Ge2 96.6(3) . . ? C61 Co6 Ge2 159.2(3) . . ? C63 Co6 Ge2 100.3(3) . . ? Ge1 Co6 Ge2 74.84(4) . . ? C62 Co6 Co8 101.3(3) . . ? C61 Co6 Co8 131.7(3) . . ? C63 Co6 Co8 44.5(3) . . ? Ge1 Co6 Co8 108.31(5) . . ? Ge2 Co6 Co8 55.85(4) . . ? C62 Co6 Co5 154.0(3) . . ? C61 Co6 Co5 105.7(3) . . ? C63 Co6 Co5 80.1(2) . . ? Ge1 Co6 Co5 53.17(3) . . ? Ge2 Co6 Co5 59.67(3) . . ? Co8 Co6 Co5 57.64(4) . . ? C62 Co6 Co7 86.1(3) . . ? C61 Co6 Co7 115.1(3) . . ? C63 Co6 Co7 153.6(3) . . ? Ge1 Co6 Co7 53.50(3) . . ? Ge2 Co6 Co7 53.49(3) . . ? Co8 Co6 Co7 109.34(5) . . ? Co5 Co6 Co7 87.28(4) . . ? C71 Co7 C72 103.3(4) . . ? C71 Co7 C23 89.5(4) . . ? C72 Co7 C23 92.7(4) . . ? C71 Co7 Ge1 156.2(3) . . ? C72 Co7 Ge1 98.7(3) . . ? C23 Co7 Ge1 98.4(3) . . ? C71 Co7 Ge2 84.4(3) . . ? C72 Co7 Ge2 127.9(3) . . ? C23 Co7 Ge2 139.3(3) . . ? Ge1 Co7 Ge2 74.87(4) . . ? C71 Co7 Co2 123.8(3) . . ? C72 Co7 Co2 107.6(3) . . ? C23 Co7 Co2 44.1(3) . . ? Ge1 Co7 Co2 55.71(4) . . ? Ge2 Co7 Co2 109.81(5) . . ? C71 Co7 Co4 98.8(3) . . ? C72 Co7 Co4 157.9(3) . . ? C23 Co7 Co4 87.3(3) . . ? Ge1 Co7 Co4 59.50(3) . . ? Ge2 Co7 Co4 54.26(3) . . ? Co2 Co7 Co4 58.37(4) . . ? C71 Co7 Co6 121.6(3) . . ? C72 Co7 Co6 80.6(3) . . ? C23 Co7 Co6 148.9(3) . . ? Ge1 Co7 Co6 53.44(3) . . ? Ge2 Co7 Co6 53.61(3) . . ? Co2 Co7 Co6 109.08(5) . . ? Co4 Co7 Co6 88.00(4) . . ? C82 Co8 C81 98.4(4) . . ? C82 Co8 C63 96.6(4) . . ? C81 Co8 C63 96.9(4) . . ? C82 Co8 Ge2 140.9(3) . . ? C81 Co8 Ge2 110.1(3) . . ? C63 Co8 Ge2 105.6(3) . . ? C82 Co8 Co5 87.0(3) . . ? C81 Co8 Co5 172.6(3) . . ? C63 Co8 Co5 87.5(3) . . ? Ge2 Co8 Co5 62.77(4) . . ? C82 Co8 Co6 133.1(3) . . ? C81 Co8 Co6 114.3(3) . . ? C63 Co8 Co6 48.8(3) . . ? Ge2 Co8 Co6 56.78(4) . . ? Co5 Co8 Co6 64.39(4) . . ? C82 Co8 Co9 87.6(3) . . ? C81 Co8 Co9 117.9(3) . . ? C63 Co8 Co9 143.9(3) . . ? Ge2 Co8 Co9 55.76(4) . . ? Co5 Co8 Co9 56.90(4) . . ? Co6 Co8 Co9 104.02(5) . . ? C82 Co8 Co10 122.7(3) . . ? C81 Co8 Co10 64.4(3) . . ? C63 Co8 Co10 137.5(3) . . ? Ge2 Co8 Co10 54.46(4) . . ? Co5 Co8 Co10 108.36(5) . . ? Co6 Co8 Co10 102.04(5) . . ? Co9 Co8 Co10 61.07(4) . . ? C92 Co9 C91 99.8(4) . . ? C92 Co9 C52 94.9(4) . . ? C91 Co9 C52 99.2(4) . . ? C92 Co9 Ge2 136.2(3) . . ? C91 Co9 Ge2 109.1(3) . . ? C52 Co9 Ge2 111.6(2) . . ? C92 Co9 Co5 128.8(3) . . ? C91 Co9 Co5 117.1(3) . . ? C52 Co9 Co5 47.6(2) . . ? Ge2 Co9 Co5 64.03(4) . . ? C92 Co9 Co4 164.8(3) . . ? C91 Co9 Co4 65.3(3) . . ? C52 Co9 Co4 85.1(3) . . ? Ge2 Co9 Co4 56.44(4) . . ? Co5 Co9 Co4 61.02(4) . . ? C92 Co9 Co8 92.5(3) . . ? C91 Co9 Co8 164.1(3) . . ? C52 Co9 Co8 89.7(2) . . ? Ge2 Co9 Co8 55.15(4) . . ? Co5 Co9 Co8 60.28(4) . . ? Co4 Co9 Co8 102.75(5) . . ? C92 Co9 Co10 85.7(3) . . ? C91 Co9 Co10 111.1(3) . . ? C52 Co9 Co10 149.2(2) . . ? Ge2 Co9 Co10 53.72(4) . . ? Co5 Co9 Co10 109.90(5) . . ? Co4 Co9 Co10 102.11(5) . . ? Co8 Co9 Co10 59.56(4) . . ? C102 Co10 C103 103.4(4) . . ? C102 Co10 C101 106.1(4) . . ? C103 Co10 C101 99.1(4) . . ? C102 Co10 Ge2 94.8(3) . . ? C103 Co10 Ge2 89.0(3) . . ? C101 Co10 Ge2 155.1(3) . . ? C102 Co10 C81 85.1(4) . . ? C103 Co10 C81 171.4(4) . . ? C101 Co10 C81 79.6(4) . . ? Ge2 Co10 C81 88.9(2) . . ? C102 Co10 Co8 106.3(3) . . ? C103 Co10 Co8 134.7(3) . . ? C101 Co10 Co8 104.4(3) . . ? Ge2 Co10 Co8 55.50(4) . . ? C81 Co10 Co8 39.0(2) . . ? C102 Co10 Co9 150.1(3) . . ? C103 Co10 Co9 78.0(3) . . ? C101 Co10 Co9 103.1(3) . . ? Ge2 Co10 Co9 55.33(4) . . ? C81 Co10 Co9 94.0(2) . . ? Co8 Co10 Co9 59.37(4) . . ? O11 C11 Co1 171.7(8) . . ? O12 C12 Co1 177.1(8) . . ? O22 C22 Co2 148.0(8) . . ? O22 C22 Co3 127.1(7) . . ? Co2 C22 Co3 84.9(4) . . ? O21 C21 Co2 177.6(9) . . ? O23 C23 Co2 141.4(7) . . ? O23 C23 Co7 131.4(7) . . ? Co2 C23 Co7 87.1(4) . . ? O31 C31 Co3 179.5(9) . . ? O32 C32 Co3 173.2(8) . . ? O33 C33 Co3 179.0(9) . . ? O41 C41 Co4 177.9(8) . . ? O42 C42 Co4 141.3(7) . . ? O42 C42 Co1 135.0(6) . . ? Co4 C42 Co1 83.6(3) . . ? O51 C51 Co5 178.5(8) . . ? O52 C52 Co5 138.6(7) . . ? O52 C52 Co9 137.0(7) . . ? Co5 C52 Co9 84.3(3) . . ? O61 C61 Co6 176.7(8) . . ? O62 C62 Co6 178.8(8) . . ? O63 C63 Co8 141.1(7) . . ? O63 C63 Co6 132.2(7) . . ? Co8 C63 Co6 86.6(4) . . ? O71 C71 Co7 176.2(9) . . ? O72 C72 Co7 175.4(8) . . ? O81 C81 Co8 162.2(9) . . ? O81 C81 Co10 121.2(7) . . ? Co8 C81 Co10 76.6(3) . . ? O82 C82 Co8 178.6(9) . . ? O91 C91 Co9 162.0(9) . . ? O91 C91 Co4 123.0(7) . . ? Co9 C91 Co4 75.0(4) . . ? O92 C92 Co9 175.8(8) . . ? O101 C101 Co10 176.4(9) . . ? O102 C102 Co10 176.1(9) . . ? O103 C103 Co10 173.7(8) . . ? C1D N1 C1F1 177.0(13) . . ? C1D N1 C1C1 112.7(11) . . ? C1F1 N1 C1C1 70.2(11) . . ? C1D N1 C1C 68.4(10) . . ? C1F1 N1 C1C 112.0(12) . . ? C1C1 N1 C1C 76.6(10) . . ? C1D N1 C1E 64.9(11) . . ? C1F1 N1 C1E 112.3(13) . . ? C1C1 N1 C1E 177.1(12) . . ? C1C N1 C1E 103.4(12) . . ? C1D N1 C1F 105.0(11) . . ? C1F1 N1 C1F 72.8(11) . . ? C1C1 N1 C1F 111.3(11) . . ? C1C N1 C1F 66.8(10) . . ? C1E N1 C1F 71.2(11) . . ? C1D N1 C1E1 112.9(12) . . ? C1F1 N1 C1E1 66.5(12) . . ? C1C1 N1 C1E1 104.4(11) . . ? C1C N1 C1E1 177.6(12) . . ? C1E N1 C1E1 75.7(12) . . ? C1F N1 C1E1 110.8(12) . . ? C1D N1 C1D1 76.1(11) . . ? C1F1 N1 C1D1 106.1(13) . . ? C1C1 N1 C1D1 67.7(11) . . ? C1C N1 C1D1 113.3(12) . . ? C1E N1 C1D1 109.8(13) . . ? C1F N1 C1D1 178.8(13) . . ? C1E1 N1 C1D1 69.1(11) . . ? N1 C1C C1F 56.8(9) . . ? N1 C1C C2C 106.1(12) . . ? C1F C1C C2C 125.8(14) . . ? N1 C1C C1D 55.0(9) . . ? C1F C1C C1D 90.5(13) . . ? C2C C1C C1D 122.9(13) . . ? N1 C1C C1C1 51.5(8) . . ? C1F C1C C1C1 89.5(12) . . ? C2C C1C C1C1 54.7(9) . . ? C1D C1C C1C1 88.6(12) . . ? N1 C1C1 C2C 108.3(12) . . ? N1 C1C1 C1D1 57.8(10) . . ? C2C C1C1 C1D1 124.9(14) . . ? N1 C1C1 C1F1 54.6(10) . . ? C2C C1C1 C1F1 126.2(14) . . ? C1D1 C1C1 C1F1 90.8(14) . . ? N1 C1C1 C1C 51.9(8) . . ? C2C C1C1 C1C 56.4(9) . . ? C1D1 C1C1 C1C 91.7(13) . . ? C1F1 C1C1 C1C 87.8(12) . . ? N1 C1D C1E 58.6(11) . . ? N1 C1D C2D 107.4(13) . . ? C1E C1D C2D 125.4(15) . . ? N1 C1D C1C 56.6(9) . . ? C1E C1D C1C 92.4(14) . . ? C2D C1D C1C 125.3(14) . . ? N1 C1D C1D1 53.9(9) . . ? C1E C1D C1D1 92.2(14) . . ? C2D C1D C1D1 53.6(10) . . ? C1C C1D C1D1 92.1(13) . . ? N1 C1D1 C2D 106.0(14) . . ? N1 C1D1 C1C1 54.5(10) . . ? C2D C1D1 C1C1 124.1(16) . . ? N1 C1D1 C1E1 54.3(10) . . ? C2D C1D1 C1E1 125.8(16) . . ? C1C1 C1D1 C1E1 87.4(14) . . ? N1 C1D1 C1D 50.0(9) . . ? C2D C1D1 C1D 56.0(11) . . ? C1C1 C1D1 C1D 87.6(13) . . ? C1E1 C1D1 C1D 87.2(13) . . ? N1 C1E C1D 56.5(11) . . ? N1 C1E C2E 105.9(14) . . ? C1D C1E C2E 128.2(17) . . ? N1 C1E C1F 54.4(10) . . ? C1D C1E C1F 89.5(14) . . ? C2E C1E C1F 120.9(15) . . ? N1 C1E C1E1 52.2(10) . . ? C1D C1E C1E1 91.9(14) . . ? C2E C1E C1E1 53.7(10) . . ? C1F C1E C1E1 87.0(13) . . ? N1 C1E1 C2E 108.6(14) . . ? N1 C1E1 C1F1 55.9(11) . . ? C2E C1E1 C1F1 125.7(16) . . ? N1 C1E1 C1D1 56.6(10) . . ? C2E C1E1 C1D1 124.5(15) . . ? C1F1 C1E1 C1D1 91.8(15) . . ? N1 C1E1 C1E 52.1(10) . . ? C2E C1E1 C1E 56.6(11) . . ? C1F1 C1E1 C1E 90.4(14) . . ? C1D1 C1E1 C1E 88.4(14) . . ? N1 C1F C2F 108.6(13) . . ? N1 C1F C1C 56.4(9) . . ? C2F C1F C1C 131.4(15) . . ? N1 C1F C1E 54.4(10) . . ? C2F C1F C1E 123.0(15) . . ? C1C C1F C1E 87.5(13) . . ? N1 C1F C1F1 52.9(10) . . ? C2F C1F C1F1 55.8(10) . . ? C1C C1F C1F1 92.2(13) . . ? C1E C1F C1F1 89.3(14) . . ? N1 C1F1 C2F 109.5(15) . . ? N1 C1F1 C1E1 57.5(11) . . ? C2F C1F1 C1E1 124.3(17) . . ? N1 C1F1 C1C1 55.2(10) . . ? C2F C1F1 C1C1 129.2(16) . . ? C1E1 C1F1 C1C1 90.1(14) . . ? N1 C1F1 C1F 54.3(10) . . ? C2F C1F1 C1F 55.3(11) . . ? C1E1 C1F1 C1F 93.2(14) . . ? C1C1 C1F1 C1F 90.5(14) . . ? C1C1 C2C C1C 68.9(10) . . ? C1D1 C2D C1D 70.4(12) . . ? C1E1 C2E C1E 69.7(12) . . ? C1F C2F C1F1 68.9(12) . . ? C1A N2 C1A 113.0(11) 2 . ? C1A N2 C1B 105.5(6) 2 . ? C1A N2 C1B 110.8(6) . . ? C1A N2 C1B 110.8(6) 2 2 ? C1A N2 C1B 105.5(6) . 2 ? C1B N2 C1B 111.5(11) . 2 ? N2 C1A C2A 114.6(8) . . ? C2B C1B N2 112.6(8) . . ? C1G1 N3 C1G1 101(2) 3 . ? C1G1 N3 C1G2 78.4(12) 3 . ? C1G1 N3 C1G2 173.1(14) . . ? C1G1 N3 C1G2 173.1(14) 3 3 ? C1G1 N3 C1G2 78.4(12) . 3 ? C1G2 N3 C1G2 103(2) . 3 ? C1G1 N3 C1H2 117.4(13) 3 . ? C1G1 N3 C1H2 109.2(13) . . ? C1G2 N3 C1H2 65.5(13) . . ? C1G2 N3 C1H2 68.9(13) 3 . ? C1G1 N3 C1H2 109.2(13) 3 3 ? C1G1 N3 C1H2 117.4(13) . 3 ? C1G2 N3 C1H2 68.9(13) . 3 ? C1G2 N3 C1H2 65.5(13) 3 3 ? C1H2 N3 C1H2 103(2) . 3 ? N3 C1G1 C2G 101.5(14) . . ? N3 C1G1 C1G2 51.8(11) . 3 ? C2G C1G1 C1G2 49.8(10) . 3 ? C2G C1G2 N3 108.3(16) 3 . ? C2G C1G2 C1H2 132.4(19) 3 . ? N3 C1G2 C1H2 57.6(12) . . ? C2G C1G2 C1H2 120.0(18) 3 3 ? N3 C1G2 C1H2 55.9(12) . 3 ? C1H2 C1G2 C1H2 90.7(17) . 3 ? C2G C1G2 C1G1 58.5(12) 3 3 ? N3 C1G2 C1G1 49.8(11) . 3 ? C1H2 C1G2 C1G1 92.7(16) . 3 ? C1H2 C1G2 C1G1 85.1(15) 3 3 ? C2H C1H2 N3 109.0(16) 3 . ? C2H C1H2 C1G2 122.5(19) 3 . ? N3 C1H2 C1G2 56.9(12) . . ? C2H C1H2 C1G2 130.8(19) 3 3 ? N3 C1H2 C1G2 55.2(11) . 3 ? C1G2 C1H2 C1G2 89.3(17) . 3 ? C1G2 C2G C1G1 71.7(13) 3 . ? C1H1 C2H C1H2 143(3) . 3 ? C1I O110 C1I 118(4) 2_565 . ? O110 C1I C1I 31(2) . 2_565 ? Cl1 C99 Cl1 104.6(14) . 3_556 ? Cl2 C98 Cl3 113.2(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.477 _refine_diff_density_min -1.729 _refine_diff_density_rms 0.159