# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1a _database_code_depnum_ccdc_archive 'CCDC 862922' #TrackingRef '9060_web_deposit_cif_file_0_MikhailV.Barybin_ #1326663422.1aCIF-final.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cp2Co]2[{(OC)5V}2{1,4-diisocyanodurene}]' _chemical_melting_point ? _chemical_formula_moiety 'C22 H12 N2 O10 V2, 2(C10 H10 Co)' _chemical_formula_sum 'C42 H32 Co2 N2 O10 V2' _chemical_formula_weight 944.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n _symmetry_space_group_name_Hall '-P 4bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 23.7192(14) _cell_length_b 23.7192(14) _cell_length_c 7.1617(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4029.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8659 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.97 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'SADABS, 2000' _exptl_special_details ; ? ; _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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 41416 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 30.10 _reflns_number_total 5907 _reflns_number_gt 4501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections except 2 which were flagged by the user for being in the beamstop. 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^)+(0.0734P)^2^+0.3571P] 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 5907 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 V V 0.017425(15) 0.656540(16) -0.11471(5) 0.02424(11) Uani 1 1 d . . . O10 O -0.09720(9) 0.59451(10) -0.1053(3) 0.0510(6) Uani 1 1 d . . . O11 O 0.04046(8) 0.60436(7) -0.5060(2) 0.0365(4) Uani 1 1 d . . . O12 O -0.03400(10) 0.75882(8) -0.3258(3) 0.0469(5) Uani 1 1 d . . . O13 O -0.00919(8) 0.70748(8) 0.2749(2) 0.0369(4) Uani 1 1 d . . . O14 O 0.06033(10) 0.54904(9) 0.0881(3) 0.0524(6) Uani 1 1 d . . . N1 N 0.14136(8) 0.70984(9) -0.1177(3) 0.0309(4) Uani 1 1 d . . . C1 C 0.09572(10) 0.69084(10) -0.1158(3) 0.0285(5) Uani 1 1 d . . . C2 C 0.19623(9) 0.73017(10) -0.1196(3) 0.0246(4) Uani 1 1 d . . . C3 C 0.24050(9) 0.69110(10) -0.1193(3) 0.0247(4) Uani 1 1 d . . . C4 C 0.20431(9) 0.78866(10) -0.1214(3) 0.0250(4) Uani 1 1 d . . . C5 C 0.22921(12) 0.62836(10) -0.1170(4) 0.0355(6) Uani 1 1 d . . . H5A H 0.2493 0.6111 -0.0120 0.053 Uiso 1 1 calc R . . H5B H 0.2423 0.6116 -0.2343 0.053 Uiso 1 1 calc R . . H5C H 0.1886 0.6217 -0.1031 0.053 Uiso 1 1 calc R . . C6 C 0.15541(11) 0.82863(11) -0.1231(4) 0.0350(5) Uani 1 1 d . . . H6A H 0.1613 0.8572 -0.2201 0.053 Uiso 1 1 calc R . . H6B H 0.1523 0.8471 -0.0011 0.053 Uiso 1 1 calc R . . H6C H 0.1206 0.8078 -0.1493 0.053 Uiso 1 1 calc R . . C10 C -0.05427(11) 0.61905(12) -0.1113(3) 0.0342(5) Uani 1 1 d . . . C11 C 0.03314(9) 0.62357(10) -0.3613(3) 0.0276(5) Uani 1 1 d . . . C12 C -0.01413(11) 0.72160(10) -0.2453(3) 0.0318(5) Uani 1 1 d . . . C13 C 0.00153(10) 0.68893(10) 0.1315(3) 0.0285(5) Uani 1 1 d . . . C14 C 0.04622(11) 0.58943(10) 0.0131(3) 0.0327(5) Uani 1 1 d . . . Co Co -0.069274(13) 0.856530(13) 0.09322(5) 0.02765(10) Uani 1 1 d . . . C21 C -0.02153(12) 0.92004(12) 0.1954(5) 0.0454(7) Uani 1 1 d . . . H21 H -0.0336 0.9486 0.2795 0.054 Uiso 1 1 calc R . . C22 C 0.00165(11) 0.86676(13) 0.2462(4) 0.0439(7) Uani 1 1 d . . . H22 H 0.0077 0.8533 0.3695 0.053 Uiso 1 1 calc R . . C23 C 0.01397(10) 0.83761(11) 0.0785(4) 0.0343(6) Uani 1 1 d . . . H23 H 0.0298 0.8009 0.0691 0.041 Uiso 1 1 calc R . . C24 C -0.00142(10) 0.87282(11) -0.0724(4) 0.0343(5) Uani 1 1 d . . . H24 H 0.0025 0.8639 -0.2010 0.041 Uiso 1 1 calc R . . C25 C -0.02351(11) 0.92313(11) 0.0000(4) 0.0400(6) Uani 1 1 d . . . H25 H -0.0374 0.9540 -0.0710 0.048 Uiso 1 1 calc R . . C31 C -0.14588(11) 0.86004(12) 0.2193(4) 0.0426(6) Uani 1 1 d . . . H31 H -0.1569 0.8850 0.3162 0.051 Uiso 1 1 calc R . . C32 C -0.12098(11) 0.80602(12) 0.2437(4) 0.0435(7) Uani 1 1 d . . . H32 H -0.1123 0.7886 0.3596 0.052 Uiso 1 1 calc R . . C33 C -0.11152(11) 0.78286(11) 0.0640(4) 0.0374(6) Uani 1 1 d . . . H33 H -0.0953 0.7470 0.0385 0.045 Uiso 1 1 calc R . . C34 C -0.13037(11) 0.82229(11) -0.0713(4) 0.0358(5) Uani 1 1 d . . . H34 H -0.1291 0.8175 -0.2030 0.043 Uiso 1 1 calc R . . C35 C -0.15135(10) 0.87009(11) 0.0245(4) 0.0384(6) Uani 1 1 d . . . H35 H -0.1664 0.9031 -0.0316 0.046 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 V 0.02166(18) 0.02598(19) 0.0251(2) 0.00002(14) -0.00084(14) -0.00037(14) O10 0.0400(11) 0.0750(15) 0.0382(11) 0.0002(10) -0.0028(9) -0.0231(10) O11 0.0435(10) 0.0350(9) 0.0311(10) -0.0023(8) 0.0021(8) 0.0049(8) O12 0.0712(14) 0.0359(10) 0.0336(10) -0.0030(8) -0.0073(10) 0.0183(10) O13 0.0460(10) 0.0377(9) 0.0269(9) -0.0018(7) 0.0003(8) 0.0039(8) O14 0.0753(15) 0.0475(12) 0.0344(11) 0.0067(9) 0.0024(10) 0.0227(11) N1 0.0268(9) 0.0402(11) 0.0256(10) -0.0016(8) 0.0011(8) -0.0074(8) C1 0.0287(11) 0.0320(11) 0.0248(11) -0.0017(9) 0.0004(9) -0.0003(9) C2 0.0225(10) 0.0348(11) 0.0165(10) -0.0017(8) 0.0017(8) -0.0069(8) C3 0.0290(11) 0.0305(11) 0.0148(9) -0.0011(8) -0.0002(8) -0.0066(9) C4 0.0265(10) 0.0332(11) 0.0153(10) -0.0003(8) 0.0012(8) -0.0010(9) C5 0.0411(14) 0.0289(12) 0.0366(14) -0.0034(10) -0.0007(11) -0.0070(10) C6 0.0317(12) 0.0395(13) 0.0339(13) -0.0007(10) 0.0034(10) 0.0031(10) C10 0.0336(12) 0.0440(14) 0.0252(12) 0.0003(10) -0.0015(10) -0.0039(10) C11 0.0245(10) 0.0256(10) 0.0326(13) 0.0032(9) -0.0026(9) -0.0001(8) C12 0.0376(13) 0.0315(12) 0.0264(12) -0.0070(9) -0.0014(10) 0.0021(10) C13 0.0257(10) 0.0276(11) 0.0323(12) 0.0047(9) -0.0041(9) -0.0006(9) C14 0.0361(13) 0.0342(12) 0.0279(12) -0.0005(10) 0.0035(10) 0.0036(10) Co 0.02586(16) 0.02602(16) 0.03107(19) 0.00203(12) 0.00272(12) 0.00465(12) C21 0.0386(14) 0.0413(15) 0.0561(19) -0.0182(13) 0.0028(13) -0.0018(12) C22 0.0361(14) 0.0588(18) 0.0367(15) 0.0001(13) -0.0072(11) -0.0003(12) C23 0.0223(10) 0.0322(12) 0.0484(16) 0.0032(11) 0.0029(10) 0.0032(9) C24 0.0289(11) 0.0355(12) 0.0385(14) 0.0030(11) 0.0069(10) -0.0042(10) C25 0.0341(13) 0.0280(12) 0.0578(19) 0.0059(12) -0.0004(12) -0.0018(10) C31 0.0295(12) 0.0485(15) 0.0498(17) -0.0046(13) 0.0107(12) 0.0046(11) C32 0.0349(13) 0.0466(15) 0.0489(17) 0.0149(13) 0.0116(12) 0.0018(11) C33 0.0315(12) 0.0285(12) 0.0522(16) 0.0052(11) 0.0058(11) 0.0010(9) C34 0.0330(12) 0.0344(13) 0.0399(14) 0.0016(11) -0.0028(11) -0.0008(10) C35 0.0275(12) 0.0352(13) 0.0525(17) 0.0025(12) -0.0024(11) 0.0054(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 V C10 1.919(3) . ? V C12 1.953(3) . ? V C14 1.959(3) . ? V C13 1.960(3) . ? V C11 1.967(3) . ? V C1 2.027(2) . ? O10 C10 1.174(3) . ? O11 C11 1.145(3) . ? O12 C12 1.155(3) . ? O13 C13 1.146(3) . ? O14 C14 1.148(3) . ? N1 C1 1.173(3) . ? N1 C2 1.388(3) . ? C2 C4 1.401(3) . ? C2 C3 1.401(3) . ? C3 C4 1.394(3) 2_565 ? C3 C5 1.512(3) . ? C4 C3 1.394(3) 2_565 ? C4 C6 1.498(3) . ? Co C21 2.022(3) . ? Co C22 2.022(3) . ? Co C32 2.025(3) . ? Co C33 2.025(3) . ? Co C23 2.028(2) . ? Co C25 2.030(3) . ? Co C31 2.031(3) . ? Co C35 2.034(3) . ? Co C24 2.036(2) . ? Co C34 2.037(3) . ? C21 C25 1.402(4) . ? C21 C22 1.425(4) . ? C22 C23 1.416(4) . ? C23 C24 1.414(4) . ? C24 C25 1.403(4) . ? C31 C35 1.421(4) . ? C31 C32 1.422(4) . ? C32 C33 1.417(4) . ? C33 C34 1.419(4) . ? C34 C35 1.416(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 V C12 91.87(11) . . ? C10 V C14 85.79(11) . . ? C12 V C14 177.55(11) . . ? C10 V C13 89.99(10) . . ? C12 V C13 92.71(10) . . ? C14 V C13 88.02(10) . . ? C10 V C11 89.71(10) . . ? C12 V C11 87.53(10) . . ? C14 V C11 91.73(10) . . ? C13 V C11 179.63(10) . . ? C10 V C1 176.02(11) . . ? C12 V C1 91.84(10) . . ? C14 V C1 90.49(10) . . ? C13 V C1 91.27(10) . . ? C11 V C1 89.01(9) . . ? C1 N1 C2 177.7(3) . . ? N1 C1 V 178.9(2) . . ? N1 C2 C4 118.2(2) . . ? N1 C2 C3 118.2(2) . . ? C4 C2 C3 123.56(19) . . ? C4 C3 C2 118.4(2) 2_565 . ? C4 C3 C5 120.3(2) 2_565 . ? C2 C3 C5 121.2(2) . . ? C3 C4 C2 118.0(2) 2_565 . ? C3 C4 C6 120.6(2) 2_565 . ? C2 C4 C6 121.4(2) . . ? O10 C10 V 177.4(2) . . ? O11 C11 V 177.8(2) . . ? O12 C12 V 177.6(2) . . ? O13 C13 V 178.2(2) . . ? O14 C14 V 176.5(2) . . ? C21 Co C22 41.28(12) . . ? C21 Co C32 125.98(14) . . ? C22 Co C32 106.65(13) . . ? C21 Co C33 163.23(13) . . ? C22 Co C33 124.83(12) . . ? C32 Co C33 40.96(12) . . ? C21 Co C23 68.79(11) . . ? C22 Co C23 40.94(11) . . ? C32 Co C23 119.11(11) . . ? C33 Co C23 106.59(10) . . ? C21 Co C25 40.49(13) . . ? C22 Co C25 68.89(12) . . ? C32 Co C25 163.61(12) . . ? C33 Co C25 154.46(12) . . ? C23 Co C25 68.55(10) . . ? C21 Co C31 108.05(12) . . ? C22 Co C31 119.91(13) . . ? C32 Co C31 41.04(11) . . ? C33 Co C31 68.81(11) . . ? C23 Co C31 154.63(12) . . ? C25 Co C31 126.36(12) . . ? C21 Co C35 120.40(11) . . ? C22 Co C35 155.31(12) . . ? C32 Co C35 69.06(12) . . ? C33 Co C35 68.77(11) . . ? C23 Co C35 162.68(12) . . ? C25 Co C35 108.02(11) . . ? C31 Co C35 40.93(12) . . ? C21 Co C24 68.08(12) . . ? C22 Co C24 68.60(12) . . ? C32 Co C24 154.28(11) . . ? C33 Co C24 119.65(11) . . ? C23 Co C24 40.71(10) . . ? C25 Co C24 40.36(11) . . ? C31 Co C24 163.42(11) . . ? C35 Co C24 125.85(11) . . ? C21 Co C34 154.83(12) . . ? C22 Co C34 162.41(12) . . ? C32 Co C34 68.97(12) . . ? C33 Co C34 40.90(11) . . ? C23 Co C34 125.07(11) . . ? C25 Co C34 120.04(11) . . ? C31 Co C34 68.71(12) . . ? C35 Co C34 40.70(11) . . ? C24 Co C34 107.52(11) . . ? C25 C21 C22 108.3(2) . . ? C25 C21 Co 70.06(15) . . ? C22 C21 Co 69.38(16) . . ? C23 C22 C21 107.2(3) . . ? C23 C22 Co 69.73(15) . . ? C21 C22 Co 69.34(16) . . ? C24 C23 C22 107.8(2) . . ? C24 C23 Co 69.97(14) . . ? C22 C23 Co 69.33(14) . . ? C25 C24 C23 108.5(2) . . ? C25 C24 Co 69.57(15) . . ? C23 C24 Co 69.31(14) . . ? C21 C25 C24 108.2(2) . . ? C21 C25 Co 69.45(16) . . ? C24 C25 Co 70.07(14) . . ? C35 C31 C32 108.1(2) . . ? C35 C31 Co 69.64(15) . . ? C32 C31 Co 69.27(15) . . ? C33 C32 C31 107.7(3) . . ? C33 C32 Co 69.52(15) . . ? C31 C32 Co 69.69(15) . . ? C32 C33 C34 108.3(2) . . ? C32 C33 Co 69.52(16) . . ? C34 C33 Co 69.99(15) . . ? C35 C34 C33 107.9(3) . . ? C35 C34 Co 69.53(15) . . ? C33 C34 Co 69.11(15) . . ? C34 C35 C31 108.0(2) . . ? C34 C35 Co 69.77(14) . . ? C31 C35 Co 69.42(14) . . ? 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 N1 C2 C3 C4 179.93(19) . . . 2_565 ? C4 C2 C3 C4 -0.1(3) . . . 2_565 ? N1 C2 C3 C5 0.0(3) . . . . ? C4 C2 C3 C5 179.9(2) . . . . ? N1 C2 C4 C3 178.66(19) . . . 2_565 ? C3 C2 C4 C3 -1.3(3) . . . 2_565 ? N1 C2 C4 C6 -0.5(3) . . . . ? C3 C2 C4 C6 179.5(2) . . . . ? C22 Co C21 C25 119.6(2) . . . . ? C32 Co C21 C25 -167.31(15) . . . . ? C33 Co C21 C25 158.3(3) . . . . ? C23 Co C21 C25 81.40(17) . . . . ? C31 Co C21 C25 -125.36(17) . . . . ? C35 Co C21 C25 -82.25(19) . . . . ? C24 Co C21 C25 37.47(15) . . . . ? C34 Co C21 C25 -47.2(3) . . . . ? C32 Co C21 C22 73.1(2) . . . . ? C33 Co C21 C22 38.7(5) . . . . ? C23 Co C21 C22 -38.17(17) . . . . ? C25 Co C21 C22 -119.6(2) . . . . ? C31 Co C21 C22 115.08(18) . . . . ? C35 Co C21 C22 158.19(17) . . . . ? C24 Co C21 C22 -82.09(18) . . . . ? C34 Co C21 C22 -166.7(2) . . . . ? C25 C21 C22 C23 0.3(3) . . . . ? Co C21 C22 C23 59.71(18) . . . . ? C25 C21 C22 Co -59.46(19) . . . . ? C21 Co C22 C23 -118.5(2) . . . . ? C32 Co C22 C23 115.48(17) . . . . ? C33 Co C22 C23 74.3(2) . . . . ? C25 Co C22 C23 -81.20(17) . . . . ? C31 Co C22 C23 158.07(16) . . . . ? C35 Co C22 C23 -168.6(2) . . . . ? C24 Co C22 C23 -37.75(15) . . . . ? C34 Co C22 C23 42.7(5) . . . . ? C32 Co C22 C21 -126.07(18) . . . . ? C33 Co C22 C21 -167.29(17) . . . . ? C23 Co C22 C21 118.5(2) . . . . ? C25 Co C22 C21 37.26(17) . . . . ? C31 Co C22 C21 -83.5(2) . . . . ? C35 Co C22 C21 -50.1(4) . . . . ? C24 Co C22 C21 80.71(18) . . . . ? C34 Co C22 C21 161.2(4) . . . . ? C21 C22 C23 C24 0.1(3) . . . . ? Co C22 C23 C24 59.60(17) . . . . ? C21 C22 C23 Co -59.46(18) . . . . ? C21 Co C23 C24 -80.61(18) . . . . ? C22 Co C23 C24 -119.1(2) . . . . ? C32 Co C23 C24 159.04(17) . . . . ? C33 Co C23 C24 116.44(16) . . . . ? C25 Co C23 C24 -37.00(16) . . . . ? C31 Co C23 C24 -168.2(2) . . . . ? C35 Co C23 C24 44.7(4) . . . . ? C34 Co C23 C24 75.42(19) . . . . ? C21 Co C23 C22 38.47(18) . . . . ? C32 Co C23 C22 -81.9(2) . . . . ? C33 Co C23 C22 -124.48(18) . . . . ? C25 Co C23 C22 82.08(19) . . . . ? C31 Co C23 C22 -49.1(3) . . . . ? C35 Co C23 C22 163.8(3) . . . . ? C24 Co C23 C22 119.1(2) . . . . ? C34 Co C23 C22 -165.50(17) . . . . ? C22 C23 C24 C25 -0.5(3) . . . . ? Co C23 C24 C25 58.71(18) . . . . ? C22 C23 C24 Co -59.20(17) . . . . ? C21 Co C24 C25 -37.59(17) . . . . ? C22 Co C24 C25 -82.16(19) . . . . ? C32 Co C24 C25 -166.2(3) . . . . ? C33 Co C24 C25 158.97(17) . . . . ? C23 Co C24 C25 -120.1(2) . . . . ? C31 Co C24 C25 42.0(5) . . . . ? C35 Co C24 C25 74.9(2) . . . . ? C34 Co C24 C25 116.05(17) . . . . ? C21 Co C24 C23 82.52(18) . . . . ? C22 Co C24 C23 37.95(16) . . . . ? C32 Co C24 C23 -46.1(3) . . . . ? C33 Co C24 C23 -80.91(18) . . . . ? C25 Co C24 C23 120.1(2) . . . . ? C31 Co C24 C23 162.1(4) . . . . ? C35 Co C24 C23 -165.01(16) . . . . ? C34 Co C24 C23 -123.84(16) . . . . ? C22 C21 C25 C24 -0.6(3) . . . . ? Co C21 C25 C24 -59.58(18) . . . . ? C22 C21 C25 Co 59.03(19) . . . . ? C23 C24 C25 C21 0.6(3) . . . . ? Co C24 C25 C21 59.20(18) . . . . ? C23 C24 C25 Co -58.56(17) . . . . ? C22 Co C25 C21 -37.96(17) . . . . ? C32 Co C25 C21 39.1(5) . . . . ? C33 Co C25 C21 -165.7(2) . . . . ? C23 Co C25 C21 -82.04(17) . . . . ? C31 Co C25 C21 74.3(2) . . . . ? C35 Co C25 C21 116.01(17) . . . . ? C24 Co C25 C21 -119.4(2) . . . . ? C34 Co C25 C21 158.89(16) . . . . ? C21 Co C25 C24 119.4(2) . . . . ? C22 Co C25 C24 81.40(18) . . . . ? C32 Co C25 C24 158.4(4) . . . . ? C33 Co C25 C24 -46.3(3) . . . . ? C23 Co C25 C24 37.32(16) . . . . ? C31 Co C25 C24 -166.29(17) . . . . ? C35 Co C25 C24 -124.63(17) . . . . ? C34 Co C25 C24 -81.75(18) . . . . ? C21 Co C31 C35 115.88(18) . . . . ? C22 Co C31 C35 159.46(16) . . . . ? C32 Co C31 C35 -119.6(2) . . . . ? C33 Co C31 C35 -81.62(17) . . . . ? C23 Co C31 C35 -165.7(2) . . . . ? C25 Co C31 C35 74.8(2) . . . . ? C24 Co C31 C35 42.2(5) . . . . ? C34 Co C31 C35 -37.58(15) . . . . ? C21 Co C31 C32 -124.52(19) . . . . ? C22 Co C31 C32 -80.9(2) . . . . ? C33 Co C31 C32 37.98(18) . . . . ? C23 Co C31 C32 -46.1(3) . . . . ? C25 Co C31 C32 -165.64(18) . . . . ? C35 Co C31 C32 119.6(2) . . . . ? C24 Co C31 C32 161.8(4) . . . . ? C34 Co C31 C32 82.01(19) . . . . ? C35 C31 C32 C33 -0.4(3) . . . . ? Co C31 C32 C33 -59.38(18) . . . . ? C35 C31 C32 Co 59.03(18) . . . . ? C21 Co C32 C33 -165.61(16) . . . . ? C22 Co C32 C33 -124.39(17) . . . . ? C23 Co C32 C33 -81.77(19) . . . . ? C25 Co C32 C33 164.0(4) . . . . ? C31 Co C32 C33 118.9(2) . . . . ? C35 Co C32 C33 81.33(18) . . . . ? C24 Co C32 C33 -49.2(3) . . . . ? C34 Co C32 C33 37.60(16) . . . . ? C21 Co C32 C31 75.5(2) . . . . ? C22 Co C32 C31 116.69(19) . . . . ? C33 Co C32 C31 -118.9(2) . . . . ? C23 Co C32 C31 159.31(17) . . . . ? C25 Co C32 C31 45.1(5) . . . . ? C35 Co C32 C31 -37.59(17) . . . . ? C24 Co C32 C31 -168.2(2) . . . . ? C34 Co C32 C31 -81.32(19) . . . . ? C31 C32 C33 C34 0.1(3) . . . . ? Co C32 C33 C34 -59.42(18) . . . . ? C31 C32 C33 Co 59.49(18) . . . . ? C21 Co C33 C32 44.2(4) . . . . ? C22 Co C33 C32 74.40(19) . . . . ? C23 Co C33 C32 115.55(17) . . . . ? C25 Co C33 C32 -169.6(2) . . . . ? C31 Co C33 C32 -38.05(17) . . . . ? C35 Co C33 C32 -82.11(18) . . . . ? C24 Co C33 C32 157.77(16) . . . . ? C34 Co C33 C32 -119.6(2) . . . . ? C21 Co C33 C34 163.8(3) . . . . ? C22 Co C33 C34 -166.02(16) . . . . ? C32 Co C33 C34 119.6(2) . . . . ? C23 Co C33 C34 -124.87(16) . . . . ? C25 Co C33 C34 -50.0(3) . . . . ? C31 Co C33 C34 81.53(17) . . . . ? C35 Co C33 C34 37.47(16) . . . . ? C24 Co C33 C34 -82.65(18) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? Co C33 C34 C35 -58.88(17) . . . . ? C32 C33 C34 Co 59.13(19) . . . . ? C21 Co C34 C35 -49.5(3) . . . . ? C22 Co C34 C35 160.6(4) . . . . ? C32 Co C34 C35 81.95(17) . . . . ? C33 Co C34 C35 119.6(2) . . . . ? C23 Co C34 C35 -166.53(16) . . . . ? C25 Co C34 C35 -82.85(19) . . . . ? C31 Co C34 C35 37.79(17) . . . . ? C24 Co C34 C35 -125.08(16) . . . . ? C21 Co C34 C33 -169.1(2) . . . . ? C22 Co C34 C33 41.0(5) . . . . ? C32 Co C34 C33 -37.65(16) . . . . ? C23 Co C34 C33 73.88(19) . . . . ? C25 Co C34 C33 157.56(16) . . . . ? C31 Co C34 C33 -81.80(17) . . . . ? C35 Co C34 C33 -119.6(2) . . . . ? C24 Co C34 C33 115.33(17) . . . . ? C33 C34 C35 C31 -0.5(3) . . . . ? Co C34 C35 C31 -59.08(18) . . . . ? C33 C34 C35 Co 58.62(17) . . . . ? C32 C31 C35 C34 0.5(3) . . . . ? Co C31 C35 C34 59.30(18) . . . . ? C32 C31 C35 Co -58.80(18) . . . . ? C21 Co C35 C34 157.99(17) . . . . ? C22 Co C35 C34 -166.1(3) . . . . ? C32 Co C35 C34 -81.70(17) . . . . ? C33 Co C35 C34 -37.65(16) . . . . ? C23 Co C35 C34 39.8(4) . . . . ? C25 Co C35 C34 115.42(17) . . . . ? C31 Co C35 C34 -119.4(2) . . . . ? C24 Co C35 C34 74.32(19) . . . . ? C21 Co C35 C31 -82.6(2) . . . . ? C22 Co C35 C31 -46.7(3) . . . . ? C32 Co C35 C31 37.68(17) . . . . ? C33 Co C35 C31 81.73(18) . . . . ? C23 Co C35 C31 159.2(3) . . . . ? C25 Co C35 C31 -125.21(17) . . . . ? C24 Co C35 C31 -166.31(16) . . . . ? C34 Co C35 C31 119.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.245 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.114