# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Guillem Aromi' _publ_contact_author_address ; Departament de Quimica Inorganica Universitat de Barcelona Diagonal 647 Barcelona Catalunya 08028 SPAIN ; _publ_contact_author_email GUILLEM.AROMI@QI.UB.ES _publ_section_title ; Di- and Trinuclear CoII Complexes of a Bis-beta-Diketone Ligand with Variable Conformation: Structure and Magnetic Studies ; loop_ _publ_author_name 'Guillem Aromi' 'Joan Cano' 'Joan Ribas' 'Helen Stoeckli-Evans' 'Simon J. Teat' # Attachment '[Co2(HL)2(bpy)2]newcif.cif' data_ga054 _database_code_depnum_ccdc_archive 'CCDC 298734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H64 Co2 N4 O12' _chemical_formula_weight 1343.18 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0139(4) _cell_length_b 16.3755(5) _cell_length_c 15.3571(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.636(2) _cell_angle_gamma 90.00 _cell_volume 3226.56(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8976 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 29.04 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6898 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 22659 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 29.42 _reflns_number_total 8953 _reflns_number_gt 6846 _reflns_threshold_expression I>2\s(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 and local programs' _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. All non-hydrogens were refined anistropically. The solvent molecules were refined with geometrical and displacement parameters retrains. From the bond distances in the disordered acetone solvent molecule it appears that there is positional disorder of the methyls and carbonyl. Since this solvent molecule is no chemical interest it was decide to leave it as it is. Hydrogens where place in calculated positions were possible. The hydroxyl H and the methyl Hs on the ligand were found in the difference map. It was not possible to find the methyl hydrogens on the acetone in the rotational difference map (Hfix 137 in shelx), and since they cannot be placed they were omitted from the refinement. ; _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^)+(0.0761P)^2^+1.0516P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8953 _refine_ls_number_parameters 462 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.056 _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 Co1 Co -0.067333(19) 0.290746(15) 0.309795(16) 0.02424(8) Uani 1 1 d . . . O1 O 0.04915(11) 0.22477(9) 0.26835(9) 0.0302(3) Uani 1 1 d . . . O2 O 0.04847(10) 0.37602(8) 0.34953(9) 0.0291(3) Uani 1 1 d . . . O3 O 0.05386(10) 0.51444(8) 0.41632(9) 0.0289(3) Uani 1 1 d . . . H3O H 0.0281 0.4735 0.3878 0.043 Uiso 1 1 calc R . . O4 O 0.16293(11) 0.63685(9) 0.63021(9) 0.0286(3) Uani 1 1 d . . . O5 O 0.04649(13) 0.77837(9) 0.57879(9) 0.0338(3) Uani 1 1 d . . . C1 C 0.20588(16) 0.15122(13) 0.29316(12) 0.0312(4) Uani 1 1 d . . . C2 C 0.15489(18) 0.07656(14) 0.28759(15) 0.0391(5) Uani 1 1 d . . . H2 H 0.0823 0.0747 0.2891 0.047 Uiso 1 1 calc R . . C3 C 0.2087(2) 0.00472(15) 0.27979(18) 0.0500(6) Uani 1 1 d . . . H3 H 0.1736 -0.0463 0.2774 0.060 Uiso 1 1 calc R . . C4 C 0.3136(2) 0.00766(17) 0.27546(18) 0.0498(6) Uani 1 1 d . . . H4 H 0.3506 -0.0415 0.2696 0.060 Uiso 1 1 calc R . . C5 C 0.3653(2) 0.08176(17) 0.27964(17) 0.0465(6) Uani 1 1 d . . . H5 H 0.4373 0.0834 0.2755 0.056 Uiso 1 1 calc R . . C6 C 0.31234(18) 0.15346(15) 0.28982(15) 0.0388(5) Uani 1 1 d . . . H6 H 0.3484 0.2041 0.2945 0.047 Uiso 1 1 calc R . . C7 C 0.14385(15) 0.22652(12) 0.30436(12) 0.0279(4) Uani 1 1 d . . . C8 C 0.19485(15) 0.29087(12) 0.35542(13) 0.0282(4) Uani 1 1 d . . . H8 H 0.2674 0.2852 0.3765 0.034 Uiso 1 1 calc R . . C9 C 0.14622(14) 0.36211(11) 0.37707(12) 0.0246(3) Uani 1 1 d . . . C10 C 0.20398(14) 0.42546(11) 0.43534(11) 0.0242(3) Uani 1 1 d . . . C11 C 0.30687(14) 0.41263(12) 0.47779(13) 0.0267(4) Uani 1 1 d . . . H11 H 0.3426 0.3652 0.4634 0.032 Uiso 1 1 calc R . . C12 C 0.35808(14) 0.46633(12) 0.53964(12) 0.0277(4) Uani 1 1 d . . . C13 C 0.30483(15) 0.53554(12) 0.55934(12) 0.0274(4) Uani 1 1 d . . . H13 H 0.3385 0.5724 0.6028 0.033 Uiso 1 1 calc R . . C14 C 0.20385(14) 0.55282(11) 0.51770(12) 0.0253(4) Uani 1 1 d . . . C15 C 0.15270(14) 0.49765(11) 0.45464(12) 0.0240(3) Uani 1 1 d . . . C16 C 0.46670(16) 0.44762(15) 0.58811(15) 0.0362(5) Uani 1 1 d . . . H16A H 0.4622 0.4109 0.6377 0.054 Uiso 1 1 calc R . . H16B H 0.5010 0.4985 0.6104 0.054 Uiso 1 1 calc R . . H16C H 0.5072 0.4213 0.5476 0.054 Uiso 1 1 calc R . . C17 C 0.15113(14) 0.62663(11) 0.54695(12) 0.0261(4) Uani 1 1 d . . . C18 C 0.10017(16) 0.68065(12) 0.48280(13) 0.0298(4) Uani 1 1 d . . . H18 H 0.0950 0.6654 0.4225 0.036 Uiso 1 1 calc R . . C19 C 0.05659(15) 0.75516(12) 0.50165(13) 0.0284(4) Uani 1 1 d . . . C20 C 0.01815(17) 0.81473(13) 0.42906(13) 0.0319(4) Uani 1 1 d . . . C21 C 0.0220(2) 0.80038(14) 0.34031(15) 0.0406(5) Uani 1 1 d . . . H21 H 0.0532 0.7516 0.3236 0.049 Uiso 1 1 calc R . . C22 C -0.0189(2) 0.85608(16) 0.27607(16) 0.0478(6) Uani 1 1 d . . . H22 H -0.0162 0.8451 0.2158 0.057 Uiso 1 1 calc R . . C23 C -0.0638(2) 0.92769(16) 0.29914(16) 0.0493(6) Uani 1 1 d . . . H23 H -0.0915 0.9660 0.2550 0.059 Uiso 1 1 calc R . . C24 C -0.0678(3) 0.94295(17) 0.38666(18) 0.0562(7) Uani 1 1 d . . . H24 H -0.0988 0.9919 0.4030 0.067 Uiso 1 1 calc R . . C25 C -0.0268(2) 0.88690(15) 0.45128(15) 0.0456(6) Uani 1 1 d . . . H25 H -0.0296 0.8982 0.5115 0.055 Uiso 1 1 calc R . . N1 N -0.17722(13) 0.20956(10) 0.23988(11) 0.0285(3) Uani 1 1 d . . . N2 N -0.11815(12) 0.35225(10) 0.18814(10) 0.0273(3) Uani 1 1 d . . . C26 C -0.20424(18) 0.13793(13) 0.27015(15) 0.0369(5) Uani 1 1 d . . . H26 H -0.1675 0.1189 0.3251 0.044 Uiso 1 1 calc R . . C27 C -0.2833(2) 0.08975(15) 0.22539(18) 0.0441(6) Uani 1 1 d . . . H27 H -0.2997 0.0385 0.2487 0.053 Uiso 1 1 calc R . . C28 C -0.33764(19) 0.11781(16) 0.14629(18) 0.0440(6) Uani 1 1 d . . . H28 H -0.3942 0.0872 0.1152 0.053 Uiso 1 1 calc R . . C29 C -0.30880(17) 0.19103(15) 0.11277(15) 0.0380(5) Uani 1 1 d . . . H29 H -0.3442 0.2108 0.0577 0.046 Uiso 1 1 calc R . . C30 C -0.22757(15) 0.23519(13) 0.16049(13) 0.0292(4) Uani 1 1 d . . . C31 C -0.18835(16) 0.31277(13) 0.12883(13) 0.0295(4) Uani 1 1 d . . . C32 C -0.2190(2) 0.34310(16) 0.04379(15) 0.0466(6) Uani 1 1 d . . . H32 H -0.2684 0.3141 0.0026 0.056 Uiso 1 1 calc R . . C33 C -0.1775(3) 0.41523(18) 0.01969(16) 0.0541(7) Uani 1 1 d . . . H33 H -0.1976 0.4363 -0.0383 0.065 Uiso 1 1 calc R . . C34 C -0.1066(2) 0.45633(16) 0.08025(16) 0.0458(6) Uani 1 1 d . . . H34 H -0.0769 0.5064 0.0654 0.055 Uiso 1 1 calc R . . C35 C -0.07964(17) 0.42261(13) 0.16399(14) 0.0352(4) Uani 1 1 d . . . H35 H -0.0312 0.4512 0.2063 0.042 Uiso 1 1 calc R . . O1S O -0.5196(2) 0.2699(2) 0.4316(2) 0.0443(7) Uani 0.60 1 d PDU A 1 C1S C -0.3558(11) 0.2070(11) 0.4137(8) 0.062(3) Uani 0.60 1 d PDU A 1 C2S C -0.4283(5) 0.2397(3) 0.4716(3) 0.0577(12) Uani 0.60 1 d PDU A 1 C3S C -0.3900(7) 0.2415(5) 0.5670(4) 0.096(2) Uani 0.60 1 d PDU A 1 O1S' O -0.3269(7) 0.1906(6) 0.5896(5) 0.106(2) Uani 0.40 1 d PDU B 2 C1S' C -0.3351(16) 0.1936(17) 0.4255(10) 0.058(4) Uani 0.40 1 d PDU B 2 C2S' C -0.3842(4) 0.2072(4) 0.5050(4) 0.0322(11) Uani 0.40 1 d PDU B 2 C3S' C -0.4852(6) 0.2483(5) 0.4889(7) 0.061(2) Uani 0.40 1 d PDU B 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 Co1 0.02471(13) 0.02292(13) 0.02245(13) -0.00155(9) -0.00371(9) 0.00137(9) O1 0.0278(7) 0.0324(7) 0.0271(7) -0.0059(5) -0.0045(5) 0.0043(5) O2 0.0238(6) 0.0250(6) 0.0348(7) -0.0036(5) -0.0062(5) 0.0033(5) O3 0.0238(6) 0.0257(7) 0.0326(7) -0.0048(5) -0.0084(5) 0.0036(5) O4 0.0279(6) 0.0316(7) 0.0235(6) -0.0023(5) -0.0041(5) 0.0033(5) O5 0.0459(8) 0.0278(7) 0.0258(7) 0.0007(5) 0.0005(6) 0.0078(6) C1 0.0344(10) 0.0335(10) 0.0229(8) -0.0062(8) -0.0029(7) 0.0081(8) C2 0.0355(11) 0.0353(11) 0.0414(12) -0.0127(9) -0.0086(9) 0.0048(9) C3 0.0474(13) 0.0348(12) 0.0605(16) -0.0194(11) -0.0120(11) 0.0071(10) C4 0.0476(13) 0.0456(14) 0.0514(14) -0.0232(11) -0.0060(11) 0.0183(11) C5 0.0399(12) 0.0519(15) 0.0477(13) -0.0118(11) 0.0072(10) 0.0140(11) C6 0.0371(11) 0.0408(12) 0.0388(11) -0.0050(9) 0.0069(9) 0.0080(9) C7 0.0309(9) 0.0302(9) 0.0211(8) -0.0012(7) 0.0004(7) 0.0054(7) C8 0.0246(8) 0.0295(9) 0.0282(9) -0.0032(8) -0.0027(7) 0.0033(7) C9 0.0246(8) 0.0250(9) 0.0218(8) 0.0008(7) -0.0030(6) 0.0010(7) C10 0.0239(8) 0.0247(9) 0.0219(8) 0.0001(7) -0.0019(6) 0.0002(6) C11 0.0235(8) 0.0269(9) 0.0280(9) 0.0000(7) -0.0009(7) 0.0029(7) C12 0.0227(8) 0.0324(10) 0.0253(9) 0.0008(7) -0.0037(7) 0.0007(7) C13 0.0271(9) 0.0285(9) 0.0242(8) -0.0016(7) -0.0025(7) -0.0020(7) C14 0.0261(8) 0.0242(8) 0.0240(8) -0.0002(7) -0.0008(7) 0.0006(7) C15 0.0230(8) 0.0250(9) 0.0222(8) 0.0018(7) -0.0014(6) 0.0015(7) C16 0.0242(9) 0.0433(12) 0.0369(11) -0.0023(9) -0.0068(8) 0.0035(8) C17 0.0247(8) 0.0234(8) 0.0280(9) -0.0026(7) -0.0022(7) -0.0015(7) C18 0.0373(10) 0.0260(9) 0.0233(8) -0.0016(7) -0.0028(7) 0.0018(8) C19 0.0318(9) 0.0240(9) 0.0268(9) 0.0004(7) -0.0020(7) -0.0003(7) C20 0.0379(10) 0.0269(9) 0.0282(9) 0.0031(8) -0.0028(8) 0.0010(8) C21 0.0565(14) 0.0324(11) 0.0319(10) 0.0045(9) 0.0043(10) 0.0069(10) C22 0.0688(17) 0.0440(13) 0.0283(11) 0.0077(10) 0.0015(11) 0.0035(12) C23 0.0669(17) 0.0382(13) 0.0387(12) 0.0138(10) -0.0030(12) 0.0065(11) C24 0.087(2) 0.0356(13) 0.0438(13) 0.0075(11) 0.0037(13) 0.0224(13) C25 0.0697(17) 0.0338(12) 0.0307(11) 0.0036(9) 0.0011(11) 0.0134(11) N1 0.0294(8) 0.0256(8) 0.0295(8) -0.0033(6) 0.0017(6) -0.0009(6) N2 0.0264(7) 0.0278(8) 0.0254(7) -0.0020(6) -0.0025(6) 0.0021(6) C26 0.0423(11) 0.0296(10) 0.0386(11) -0.0021(9) 0.0060(9) -0.0038(9) C27 0.0479(13) 0.0342(11) 0.0536(14) -0.0089(10) 0.0181(11) -0.0117(10) C28 0.0354(11) 0.0448(13) 0.0525(14) -0.0218(11) 0.0093(10) -0.0118(10) C29 0.0325(10) 0.0425(12) 0.0361(11) -0.0150(9) -0.0030(8) -0.0029(9) C30 0.0266(9) 0.0302(9) 0.0292(9) -0.0093(8) -0.0001(7) 0.0018(7) C31 0.0314(9) 0.0297(9) 0.0253(9) -0.0061(7) -0.0017(7) 0.0026(7) C32 0.0581(15) 0.0485(14) 0.0271(10) -0.0038(10) -0.0105(10) -0.0040(11) C33 0.0780(19) 0.0527(15) 0.0270(11) 0.0079(11) -0.0045(11) -0.0027(14) C34 0.0596(15) 0.0385(12) 0.0373(12) 0.0079(10) 0.0021(11) -0.0030(11) C35 0.0378(11) 0.0314(10) 0.0337(10) 0.0006(8) -0.0017(8) -0.0027(8) O1S 0.0391(15) 0.0574(18) 0.0354(14) -0.0002(13) 0.0036(12) 0.0196(13) C1S 0.051(6) 0.057(5) 0.083(6) -0.018(4) 0.028(5) -0.001(4) C2S 0.065(3) 0.052(3) 0.057(3) -0.015(2) 0.014(3) -0.016(3) C3S 0.117(6) 0.110(6) 0.059(4) 0.012(4) 0.008(4) 0.039(5) O1S' 0.107(6) 0.141(7) 0.066(4) 0.018(4) 0.002(4) 0.021(5) C1S' 0.046(7) 0.080(11) 0.049(5) -0.029(6) 0.012(4) 0.002(6) C2S' 0.026(2) 0.039(3) 0.031(3) -0.002(2) 0.0019(19) 0.008(2) C3S' 0.047(4) 0.048(4) 0.100(6) -0.022(4) 0.049(4) -0.007(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 Co1 O1 2.0478(14) . ? Co1 O2 2.0702(14) . ? Co1 O4 2.0460(14) 3_566 ? Co1 O5 2.0315(14) 3_566 ? Co1 N1 2.1098(16) . ? Co1 N2 2.1279(16) . ? O1 C7 1.264(2) . ? O2 C9 1.292(2) . ? O3 C15 1.350(2) . ? O4 Co1 2.0460(14) 3_566 ? O4 C17 1.273(2) . ? O5 Co1 2.0315(14) 3_566 ? O5 C19 1.272(2) . ? C1 C2 1.387(3) . ? C1 C6 1.395(3) . ? C1 C7 1.499(3) . ? C2 C3 1.385(3) . ? C3 C4 1.378(4) . ? C4 C5 1.384(4) . ? C5 C6 1.383(3) . ? C7 C8 1.411(3) . ? C8 C9 1.394(3) . ? C9 C10 1.489(2) . ? C10 C11 1.404(2) . ? C10 C15 1.413(3) . ? C11 C12 1.381(3) . ? C12 C13 1.388(3) . ? C12 C16 1.515(3) . ? C13 C14 1.391(2) . ? C14 C15 1.407(3) . ? C14 C17 1.496(3) . ? C17 C18 1.405(3) . ? C18 C19 1.396(3) . ? C19 C20 1.502(3) . ? C20 C21 1.392(3) . ? C20 C25 1.386(3) . ? C21 C22 1.383(3) . ? C22 C23 1.382(4) . ? C23 C24 1.377(4) . ? C24 C25 1.391(3) . ? N1 C26 1.331(3) . ? N1 C30 1.351(3) . ? N2 C31 1.343(2) . ? N2 C35 1.334(3) . ? C26 C27 1.385(3) . ? C27 C28 1.378(4) . ? C28 C29 1.381(4) . ? C29 C30 1.385(3) . ? C30 C31 1.481(3) . ? C31 C32 1.392(3) . ? C32 C33 1.375(4) . ? C33 C34 1.371(4) . ? C34 C35 1.390(3) . ? O1S C2S 1.337(7) . ? C1S C2S 1.500(9) . ? C2S C3S 1.466(8) . ? O1S' C2S' 1.412(8) . ? C1S' C2S' 1.486(11) . ? C2S' C3S' 1.461(8) . ? 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 O1 Co1 O2 84.68(6) . . ? O1 Co1 O4 169.50(5) . 3_566 ? O1 Co1 O5 88.07(6) . 3_566 ? O1 Co1 N1 89.05(6) . . ? O1 Co1 N2 96.56(6) . . ? O2 Co1 O4 86.78(6) . 3_566 ? O2 Co1 O5 98.02(6) . 3_566 ? O2 Co1 N1 166.66(6) . . ? O2 Co1 N2 92.49(6) . . ? O4 Co1 O5 87.08(6) 3_566 3_566 ? O4 Co1 N1 100.54(6) 3_566 . ? O4 Co1 N2 89.89(6) 3_566 . ? O5 Co1 N1 93.51(6) 3_566 . ? O5 Co1 N2 168.87(7) 3_566 . ? N1 Co1 N2 76.52(6) . . ? Co1 O1 C7 124.78(12) . . ? Co1 O2 C9 127.30(12) . . ? Co1 O4 C17 123.25(12) 3_566 . ? Co1 O5 C19 126.73(13) 3_566 . ? C2 C1 C6 119.3(2) . . ? C2 C1 C7 118.08(19) . . ? C6 C1 C7 122.7(2) . . ? C1 C2 C3 120.7(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C5 120.4(2) . . ? C4 C5 C6 120.1(2) . . ? C1 C6 C5 119.9(2) . . ? O1 C7 C1 115.81(17) . . ? O1 C7 C8 126.41(18) . . ? C1 C7 C8 117.75(17) . . ? C7 C8 C9 124.57(17) . . ? O2 C9 C8 122.07(17) . . ? O2 C9 C10 116.39(16) . . ? C8 C9 C10 121.52(16) . . ? C9 C10 C11 121.42(16) . . ? C9 C10 C15 120.02(16) . . ? C11 C10 C15 118.36(16) . . ? C10 C11 C12 122.48(18) . . ? C11 C12 C13 117.96(17) . . ? C11 C12 C16 120.81(18) . . ? C13 C12 C16 121.13(18) . . ? C12 C13 C14 122.25(17) . . ? C13 C14 C15 119.17(17) . . ? C13 C14 C17 118.15(16) . . ? C15 C14 C17 122.52(16) . . ? O3 C15 C10 121.86(16) . . ? O3 C15 C14 118.39(16) . . ? C10 C15 C14 119.72(16) . . ? O4 C17 C14 115.07(16) . . ? O4 C17 C18 125.80(18) . . ? C14 C17 C18 118.99(17) . . ? C17 C18 C19 124.42(18) . . ? O5 C19 C18 124.28(18) . . ? O5 C19 C20 115.06(17) . . ? C18 C19 C20 120.65(18) . . ? C19 C20 C21 123.69(19) . . ? C19 C20 C25 118.20(19) . . ? C21 C20 C25 118.08(19) . . ? C20 C21 C22 121.0(2) . . ? C21 C22 C23 120.4(2) . . ? C22 C23 C24 119.4(2) . . ? C23 C24 C25 120.3(2) . . ? C20 C25 C24 120.9(2) . . ? Co1 N1 C26 125.03(15) . . ? Co1 N1 C30 116.66(13) . . ? C26 N1 C30 118.20(18) . . ? Co1 N2 C31 116.35(13) . . ? Co1 N2 C35 125.24(13) . . ? C31 N2 C35 118.15(17) . . ? N1 C26 C27 123.2(2) . . ? C26 C27 C28 118.5(2) . . ? C27 C28 C29 119.1(2) . . ? C28 C29 C30 119.1(2) . . ? N1 C30 C29 121.8(2) . . ? N1 C30 C31 114.90(16) . . ? C29 C30 C31 123.26(19) . . ? N2 C31 C30 115.01(17) . . ? N2 C31 C32 121.4(2) . . ? C30 C31 C32 123.61(19) . . ? C31 C32 C33 119.7(2) . . ? C32 C33 C34 119.3(2) . . ? C33 C34 C35 118.0(2) . . ? N2 C35 C34 123.5(2) . . ? O1S C2S C1S 117.3(7) . . ? O1S C2S C3S 125.4(6) . . ? C1S C2S C3S 117.2(8) . . ? O1S' C2S' C1S' 119.6(9) . . ? O1S' C2S' C3S' 124.5(6) . . ? C1S' C2S' C3S' 115.4(9) . . ? 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 O2 Co1 O1 C7 31.15(16) . . . . ? O4 Co1 O1 C7 -4.5(4) 3_566 . . . ? O5 Co1 O1 C7 -67.09(16) 3_566 . . . ? N1 Co1 O1 C7 -160.63(16) . . . . ? N2 Co1 O1 C7 123.06(16) . . . . ? O1 Co1 O2 C9 -31.59(15) . . . . ? O4 Co1 O2 C9 142.30(16) 3_566 . . . ? O5 Co1 O2 C9 55.70(16) 3_566 . . . ? N1 Co1 O2 C9 -93.9(3) . . . . ? N2 Co1 O2 C9 -127.96(16) . . . . ? C6 C1 C2 C3 0.7(3) . . . . ? C7 C1 C2 C3 -178.1(2) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 C6 1.2(4) . . . . ? C4 C5 C6 C1 -2.0(4) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? C7 C1 C6 C5 179.8(2) . . . . ? Co1 O1 C7 C1 153.54(13) . . . . ? Co1 O1 C7 C8 -24.5(3) . . . . ? C2 C1 C7 O1 -32.0(3) . . . . ? C2 C1 C7 C8 146.2(2) . . . . ? C6 C1 C7 O1 149.2(2) . . . . ? C6 C1 C7 C8 -32.6(3) . . . . ? O1 C7 C8 C9 2.8(3) . . . . ? C1 C7 C8 C9 -175.25(18) . . . . ? Co1 O2 C9 C8 23.2(3) . . . . ? Co1 O2 C9 C10 -155.27(13) . . . . ? C7 C8 C9 O2 -1.8(3) . . . . ? C7 C8 C9 C10 176.65(18) . . . . ? O2 C9 C10 C11 172.21(17) . . . . ? O2 C9 C10 C15 -2.7(3) . . . . ? C8 C9 C10 C11 -6.3(3) . . . . ? C8 C9 C10 C15 178.85(18) . . . . ? C9 C10 C11 C12 -172.62(18) . . . . ? C15 C10 C11 C12 2.3(3) . . . . ? C10 C11 C12 C13 -0.4(3) . . . . ? C10 C11 C12 C16 176.15(19) . . . . ? C11 C12 C13 C14 -1.5(3) . . . . ? C16 C12 C13 C14 -178.01(19) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C12 C13 C14 C17 176.84(18) . . . . ? C13 C14 C15 O3 178.52(17) . . . . ? C13 C14 C15 C10 0.7(3) . . . . ? C17 C14 C15 O3 3.2(3) . . . . ? C17 C14 C15 C10 -174.64(17) . . . . ? C9 C10 C15 O3 -5.2(3) . . . . ? C9 C10 C15 C14 172.61(17) . . . . ? C11 C10 C15 O3 179.82(17) . . . . ? C11 C10 C15 C14 -2.4(3) . . . . ? Co1 O4 C17 C14 -160.80(12) 3_566 . . . ? Co1 O4 C17 C18 23.7(3) 3_566 . . . ? C13 C14 C17 O4 -43.3(2) . . . . ? C13 C14 C17 C18 132.5(2) . . . . ? C15 C14 C17 O4 132.01(19) . . . . ? C15 C14 C17 C18 -52.2(3) . . . . ? O4 C17 C18 C19 1.5(3) . . . . ? C14 C17 C18 C19 -173.82(19) . . . . ? Co1 O5 C19 C18 -10.7(3) 3_566 . . . ? Co1 O5 C19 C20 169.64(14) 3_566 . . . ? C17 C18 C19 O5 -9.0(3) . . . . ? C17 C18 C19 C20 170.62(19) . . . . ? O5 C19 C20 C21 -179.7(2) . . . . ? O5 C19 C20 C25 -1.9(3) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? C18 C19 C20 C25 178.4(2) . . . . ? C19 C20 C21 C22 177.1(2) . . . . ? C25 C20 C21 C22 -0.8(4) . . . . ? C20 C21 C22 C23 0.6(4) . . . . ? C21 C22 C23 C24 -0.3(4) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C19 C20 C25 C24 -177.3(3) . . . . ? C21 C20 C25 C24 0.7(4) . . . . ? C23 C24 C25 C20 -0.4(5) . . . . ? O1 Co1 N1 C26 83.38(17) . . . . ? O1 Co1 N1 C30 -100.53(14) . . . . ? O2 Co1 N1 C26 145.2(2) . . . . ? O2 Co1 N1 C30 -38.7(3) . . . . ? O4 Co1 N1 C26 -92.31(17) 3_566 . . . ? O4 Co1 N1 C30 83.78(14) 3_566 . . . ? O5 Co1 N1 C26 -4.63(17) 3_566 . . . ? O5 Co1 N1 C30 171.46(14) 3_566 . . . ? N2 Co1 N1 C26 -179.64(18) . . . . ? N2 Co1 N1 C30 -3.55(14) . . . . ? O1 Co1 N2 C31 86.10(15) . . . . ? O1 Co1 N2 C35 -87.97(17) . . . . ? O2 Co1 N2 C31 171.03(14) . . . . ? O2 Co1 N2 C35 -3.05(17) . . . . ? O4 Co1 N2 C31 -102.20(14) 3_566 . . . ? O4 Co1 N2 C35 83.73(17) 3_566 . . . ? O5 Co1 N2 C31 -28.1(4) 3_566 . . . ? O5 Co1 N2 C35 157.9(3) 3_566 . . . ? N1 Co1 N2 C31 -1.33(14) . . . . ? N1 Co1 N2 C35 -175.40(18) . . . . ? Co1 N1 C26 C27 174.10(17) . . . . ? C30 N1 C26 C27 -1.9(3) . . . . ? N1 C26 C27 C28 -0.9(4) . . . . ? C26 C27 C28 C29 2.6(4) . . . . ? C27 C28 C29 C30 -1.4(3) . . . . ? Co1 N1 C30 C29 -173.21(16) . . . . ? Co1 N1 C30 C31 7.5(2) . . . . ? C26 N1 C30 C29 3.2(3) . . . . ? C26 N1 C30 C31 -176.17(18) . . . . ? C28 C29 C30 N1 -1.5(3) . . . . ? C28 C29 C30 C31 177.8(2) . . . . ? Co1 N2 C31 C30 5.5(2) . . . . ? Co1 N2 C31 C32 -173.25(18) . . . . ? C35 N2 C31 C30 -179.95(18) . . . . ? C35 N2 C31 C32 1.3(3) . . . . ? N1 C30 C31 N2 -8.5(3) . . . . ? N1 C30 C31 C32 170.2(2) . . . . ? C29 C30 C31 N2 172.15(19) . . . . ? C29 C30 C31 C32 -9.1(3) . . . . ? N2 C31 C32 C33 -0.5(4) . . . . ? C30 C31 C32 C33 -179.1(2) . . . . ? C31 C32 C33 C34 -0.3(4) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? Co1 N2 C35 C34 172.59(19) . . . . ? C31 N2 C35 C34 -1.4(3) . . . . ? C33 C34 C35 N2 0.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O2 0.84 1.74 2.4842(19) 147.1 . _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.876 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.077 # Attachment '[Co2(HL)2(py)4].CIF' data_ga038 _database_code_depnum_ccdc_archive 'CCDC 298735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H82 Co2 N6 O10' _chemical_formula_weight 1573.52 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1277(9) _cell_length_b 11.9911(9) _cell_length_c 15.5385(12) _cell_angle_alpha 88.681(6) _cell_angle_beta 78.050(6) _cell_angle_gamma 79.383(6) _cell_volume 1993.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 25258 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 29.58 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'STOE IPDS-2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24519 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.52 _reflns_number_total 10827 _reflns_number_gt 8159 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-Area V1.17 (STOE & Cie GmbH, 2002)' _computing_cell_refinement 'X-Area V1.17 (STOE & Cie GmbH, 2002)' _computing_data_reduction 'X-RED32 V1.04 (STOE & Cie GmbH, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0722P)^2^+0.1910P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0147(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10827 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 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 Co1 Co 0.26327(2) 0.05980(2) 0.297860(16) 0.02573(8) Uani 1 1 d . . . O1 O 0.34724(12) 0.19729(11) 0.27214(9) 0.0309(3) Uani 1 1 d . . . O2 O 0.20778(12) 0.11879(10) 0.42563(8) 0.0293(3) Uani 1 1 d . . . O3 O 0.05395(13) 0.06470(11) 0.55404(9) 0.0329(3) Uani 1 1 d . . . H3 H 0.111(3) 0.061(2) 0.502(2) 0.052(7) Uiso 1 1 d . . . O4 O -0.17289(11) 0.07098(10) 0.66473(8) 0.0275(2) Uani 1 1 d . . . O5 O -0.30472(11) 0.00671(11) 0.82640(8) 0.0288(3) Uani 1 1 d . . . N1 N 0.09388(15) 0.15778(13) 0.26638(11) 0.0309(3) Uani 1 1 d . . . N2 N 0.43843(14) -0.03450(13) 0.32026(10) 0.0301(3) Uani 1 1 d . . . C1 C 0.37629(17) 0.38582(15) 0.27385(12) 0.0304(4) Uani 1 1 d . . . C2 C 0.48578(19) 0.36023(18) 0.20982(14) 0.0378(4) Uani 1 1 d . . . H2A H 0.5222 0.2833 0.1947 0.045 Uiso 1 1 calc R . . C3 C 0.5418(2) 0.4468(2) 0.16801(16) 0.0473(5) Uani 1 1 d . . . H3A H 0.6173 0.4288 0.1252 0.057 Uiso 1 1 calc R . . C4 C 0.4884(2) 0.5592(2) 0.18829(17) 0.0501(6) Uani 1 1 d . . . H4A H 0.5262 0.6183 0.1589 0.060 Uiso 1 1 calc R . . C5 C 0.3800(3) 0.58481(19) 0.25143(18) 0.0521(6) Uani 1 1 d . . . H5A H 0.3427 0.6618 0.2654 0.062 Uiso 1 1 calc R . . C6 C 0.3248(2) 0.49864(17) 0.29478(15) 0.0417(5) Uani 1 1 d . . . H6A H 0.2511 0.5172 0.3391 0.050 Uiso 1 1 calc R . . C7 C 0.31917(16) 0.28909(15) 0.31635(12) 0.0275(3) Uani 1 1 d . . . C8 C 0.24301(17) 0.30651(15) 0.40102(12) 0.0306(4) Uani 1 1 d . . . H8 H 0.227(2) 0.384(2) 0.4269(16) 0.034(6) Uiso 1 1 d . . . C9 C 0.19007(15) 0.22290(14) 0.45156(11) 0.0259(3) Uani 1 1 d . . . C10 C 0.10905(16) 0.25113(14) 0.54032(11) 0.0258(3) Uani 1 1 d . . . C11 C 0.09711(17) 0.35683(15) 0.58091(12) 0.0305(4) Uani 1 1 d . . . H11A H 0.1412 0.4116 0.5506 0.037 Uiso 1 1 calc R . . C12 C 0.02329(19) 0.38449(15) 0.66378(13) 0.0332(4) Uani 1 1 d . . . C13 C -0.04325(17) 0.30417(15) 0.70581(12) 0.0310(4) Uani 1 1 d . . . H13A H -0.0949 0.3222 0.7623 0.037 Uiso 1 1 calc R . . C14 C -0.03703(16) 0.19872(14) 0.66832(12) 0.0268(3) Uani 1 1 d . . . C15 C 0.04238(16) 0.17007(14) 0.58587(11) 0.0261(3) Uani 1 1 d . . . C16 C 0.0151(2) 0.49782(18) 0.70710(15) 0.0461(5) Uani 1 1 d . . . H16C H -0.0505 0.5065 0.7606 0.069 Uiso 1 1 calc R . . H16B H -0.0048 0.5588 0.6664 0.069 Uiso 1 1 calc R . . H16A H 0.0954 0.5017 0.7224 0.069 Uiso 1 1 calc R . . C17 C -0.12043(16) 0.12081(14) 0.71340(11) 0.0261(3) Uani 1 1 d . . . C18 C -0.14143(17) 0.11365(16) 0.80587(12) 0.0298(3) Uani 1 1 d . . . H18 H -0.095(2) 0.158(2) 0.8393(16) 0.034(6) Uiso 1 1 d . . . C19 C -0.23321(16) 0.06047(14) 0.85653(11) 0.0260(3) Uani 1 1 d . . . C20 C -0.25524(16) 0.06735(14) 0.95495(12) 0.0278(3) Uani 1 1 d . . . C21 C -0.15865(18) 0.06660(17) 0.99948(13) 0.0347(4) Uani 1 1 d . . . H21A H -0.0762 0.0668 0.9672 0.042 Uiso 1 1 calc R . . C22 C -0.1821(2) 0.06557(19) 1.09055(14) 0.0394(4) Uani 1 1 d . . . H22A H -0.1153 0.0628 1.1204 0.047 Uiso 1 1 calc R . . C23 C -0.3021(2) 0.06857(18) 1.13813(13) 0.0398(4) Uani 1 1 d . . . H23A H -0.3178 0.0683 1.2006 0.048 Uiso 1 1 calc R . . C24 C -0.3996(2) 0.07194(18) 1.09464(13) 0.0388(4) Uani 1 1 d . . . H24A H -0.4825 0.0752 1.1272 0.047 Uiso 1 1 calc R . . C25 C -0.37563(17) 0.07052(16) 1.00350(13) 0.0329(4) Uani 1 1 d . . . H25A H -0.4424 0.0717 0.9738 0.039 Uiso 1 1 calc R . . C26 C -0.02105(18) 0.15923(16) 0.31444(13) 0.0342(4) Uani 1 1 d . . . H26A H -0.0299 0.1196 0.3684 0.041 Uiso 1 1 calc R . . C27 C -0.12744(19) 0.21605(18) 0.28869(15) 0.0398(4) Uani 1 1 d . . . H27A H -0.2076 0.2161 0.3247 0.048 Uiso 1 1 calc R . . C28 C -0.1155(2) 0.27246(18) 0.21029(16) 0.0426(5) Uani 1 1 d . . . H28A H -0.1872 0.3116 0.1910 0.051 Uiso 1 1 calc R . . C29 C 0.0027(2) 0.27112(18) 0.16010(15) 0.0413(4) Uani 1 1 d . . . H29A H 0.0138 0.3093 0.1056 0.050 Uiso 1 1 calc R . . C30 C 0.10371(19) 0.21378(17) 0.19041(13) 0.0358(4) Uani 1 1 d . . . H30A H 0.1848 0.2138 0.1558 0.043 Uiso 1 1 calc R . . C31 C 0.50687(19) 0.00766(18) 0.36849(14) 0.0370(4) Uani 1 1 d . . . H31A H 0.4734 0.0785 0.3981 0.044 Uiso 1 1 calc R . . C32 C 0.6246(2) -0.0479(2) 0.37706(16) 0.0472(5) Uani 1 1 d . . . H32A H 0.6708 -0.0157 0.4118 0.057 Uiso 1 1 calc R . . C33 C 0.6730(2) -0.1503(2) 0.33433(17) 0.0508(6) Uani 1 1 d . . . H33A H 0.7541 -0.1893 0.3381 0.061 Uiso 1 1 calc R . . C34 C 0.6026(2) -0.1958(2) 0.28581(16) 0.0475(5) Uani 1 1 d . . . H34A H 0.6333 -0.2673 0.2568 0.057 Uiso 1 1 calc R . . C35 C 0.48637(19) -0.13495(17) 0.28030(14) 0.0371(4) Uani 1 1 d . . . H35A H 0.4382 -0.1661 0.2464 0.045 Uiso 1 1 calc R . . C41 C 0.7894(2) 0.5173(2) -0.00349(17) 0.0533(6) Uani 1 1 d . . . C42 C 0.8440(2) 0.5564(2) 0.05821(18) 0.0521(6) Uani 1 1 d . . . H42A H 0.9015 0.5049 0.0841 0.063 Uiso 1 1 calc R . . C43 C 0.8168(3) 0.6694(3) 0.0834(2) 0.0703(8) Uani 1 1 d . . . H43A H 0.8557 0.6964 0.1257 0.084 Uiso 1 1 calc R . . C44 C 0.7297(4) 0.7441(3) 0.0447(3) 0.0848(13) Uani 1 1 d . . . H44A H 0.7090 0.8224 0.0605 0.102 Uiso 1 1 calc R . . C45 C 0.6762(3) 0.7022(4) -0.0152(3) 0.0847(12) Uani 1 1 d . . . H45A H 0.6170 0.7520 -0.0408 0.102 Uiso 1 1 calc R . . C46 C 0.7049(3) 0.5913(4) -0.0393(2) 0.0768(10) Uani 1 1 d . . . H46A H 0.6660 0.5645 -0.0816 0.092 Uiso 1 1 calc R . . C47 C 0.8179(4) 0.3945(3) -0.0321(2) 0.0788(9) Uani 1 1 d . . . H47C H 0.7513 0.3781 -0.0597 0.118 Uiso 1 1 calc R . . H47B H 0.8233 0.3463 0.0192 0.118 Uiso 1 1 calc R . . H47A H 0.8978 0.3793 -0.0745 0.118 Uiso 1 1 calc R . . N3 N 0.7309(2) 0.42702(19) 0.45450(19) 0.0667(7) Uani 1 1 d . . . C36 C 0.7763(2) 0.3405(3) 0.4988(2) 0.0591(7) Uani 1 1 d . . . H36A H 0.8532 0.3421 0.5159 0.071 Uiso 1 1 calc R . . C37 C 0.7219(3) 0.2495(2) 0.52190(18) 0.0597(7) Uani 1 1 d . . . H37A H 0.7598 0.1893 0.5538 0.072 Uiso 1 1 calc R . . C38 C 0.6130(3) 0.2460(3) 0.49860(18) 0.0612(7) Uani 1 1 d . . . H38A H 0.5718 0.1837 0.5153 0.073 Uiso 1 1 calc R . . C39 C 0.5614(2) 0.3315(3) 0.45116(19) 0.0618(7) Uani 1 1 d . . . H39A H 0.4852 0.3299 0.4332 0.074 Uiso 1 1 calc R . . C40 C 0.6245(3) 0.4212(3) 0.4299(2) 0.0649(8) Uani 1 1 d . . . H40A H 0.5902 0.4813 0.3962 0.078 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 Co1 0.02776(12) 0.02459(12) 0.02479(12) -0.00005(8) -0.00005(8) -0.01070(8) O1 0.0355(6) 0.0266(6) 0.0300(6) -0.0008(5) 0.0023(5) -0.0143(5) O2 0.0362(6) 0.0248(6) 0.0259(6) -0.0011(5) 0.0013(5) -0.0118(5) O3 0.0419(7) 0.0252(6) 0.0296(7) -0.0038(5) 0.0068(6) -0.0161(5) O4 0.0306(6) 0.0273(6) 0.0266(6) 0.0007(5) -0.0023(5) -0.0141(5) O5 0.0290(6) 0.0320(6) 0.0258(6) -0.0007(5) -0.0012(5) -0.0116(5) N1 0.0342(7) 0.0270(7) 0.0310(8) 0.0018(6) -0.0026(6) -0.0089(6) N2 0.0302(7) 0.0319(7) 0.0293(7) 0.0005(6) -0.0038(6) -0.0110(6) C1 0.0346(8) 0.0291(8) 0.0291(9) 0.0045(7) -0.0025(7) -0.0148(7) C2 0.0384(10) 0.0336(9) 0.0392(10) 0.0030(8) 0.0038(8) -0.0146(8) C3 0.0449(11) 0.0465(12) 0.0465(12) 0.0054(10) 0.0105(9) -0.0212(9) C4 0.0595(13) 0.0414(11) 0.0504(13) 0.0109(10) 0.0026(11) -0.0292(10) C5 0.0644(14) 0.0310(10) 0.0554(14) 0.0053(10) 0.0084(11) -0.0190(10) C6 0.0490(11) 0.0302(9) 0.0411(11) 0.0019(8) 0.0075(9) -0.0143(8) C7 0.0289(8) 0.0259(7) 0.0287(8) 0.0028(6) -0.0028(6) -0.0113(6) C8 0.0357(9) 0.0267(8) 0.0284(9) 0.0007(7) 0.0007(7) -0.0118(7) C9 0.0270(7) 0.0259(7) 0.0253(8) 0.0012(6) -0.0023(6) -0.0102(6) C10 0.0287(7) 0.0252(7) 0.0245(8) 0.0015(6) -0.0036(6) -0.0099(6) C11 0.0371(9) 0.0256(8) 0.0299(9) 0.0018(7) -0.0010(7) -0.0151(7) C12 0.0421(9) 0.0260(8) 0.0315(9) -0.0024(7) 0.0003(7) -0.0152(7) C13 0.0363(9) 0.0286(8) 0.0271(8) -0.0024(7) 0.0023(7) -0.0129(7) C14 0.0290(8) 0.0254(7) 0.0268(8) 0.0012(6) -0.0033(6) -0.0105(6) C15 0.0300(8) 0.0234(7) 0.0265(8) 0.0002(6) -0.0049(6) -0.0103(6) C16 0.0639(14) 0.0326(10) 0.0400(11) -0.0095(8) 0.0076(10) -0.0243(9) C17 0.0273(7) 0.0232(7) 0.0272(8) -0.0001(6) -0.0010(6) -0.0086(6) C18 0.0314(8) 0.0321(8) 0.0270(8) 0.0010(7) -0.0021(7) -0.0129(7) C19 0.0278(7) 0.0233(7) 0.0264(8) 0.0005(6) -0.0025(6) -0.0069(6) C20 0.0317(8) 0.0241(7) 0.0267(8) -0.0005(6) -0.0012(6) -0.0083(6) C21 0.0339(9) 0.0399(10) 0.0301(9) -0.0001(8) -0.0037(7) -0.0095(7) C22 0.0446(11) 0.0448(11) 0.0301(9) -0.0017(8) -0.0081(8) -0.0104(9) C23 0.0515(12) 0.0402(10) 0.0257(9) -0.0007(8) -0.0002(8) -0.0123(9) C24 0.0393(10) 0.0435(11) 0.0305(9) -0.0019(8) 0.0056(8) -0.0134(8) C25 0.0326(9) 0.0360(9) 0.0297(9) 0.0001(7) -0.0012(7) -0.0115(7) C26 0.0365(9) 0.0306(9) 0.0340(9) 0.0001(7) -0.0007(7) -0.0096(7) C27 0.0341(9) 0.0389(10) 0.0451(11) -0.0044(9) -0.0033(8) -0.0078(8) C28 0.0448(11) 0.0360(10) 0.0488(12) -0.0012(9) -0.0166(9) -0.0043(8) C29 0.0524(12) 0.0348(10) 0.0381(11) 0.0053(8) -0.0124(9) -0.0086(9) C30 0.0410(10) 0.0320(9) 0.0336(10) 0.0035(8) -0.0029(8) -0.0108(7) C31 0.0391(10) 0.0403(10) 0.0342(10) -0.0013(8) -0.0074(8) -0.0137(8) C32 0.0427(11) 0.0605(14) 0.0446(12) 0.0022(11) -0.0184(10) -0.0148(10) C33 0.0388(11) 0.0614(15) 0.0512(13) 0.0030(11) -0.0152(10) -0.0004(10) C34 0.0464(12) 0.0464(12) 0.0461(13) -0.0061(10) -0.0118(10) 0.0043(9) C35 0.0397(10) 0.0341(9) 0.0385(10) -0.0029(8) -0.0102(8) -0.0065(8) C41 0.0508(13) 0.0621(15) 0.0429(13) 0.0080(11) 0.0039(10) -0.0165(11) C42 0.0476(12) 0.0493(13) 0.0523(14) 0.0049(11) -0.0015(10) -0.0013(10) C43 0.0636(17) 0.0653(18) 0.075(2) -0.0119(15) 0.0104(15) -0.0199(14) C44 0.083(2) 0.0422(14) 0.098(3) 0.0117(16) 0.041(2) 0.0018(14) C45 0.069(2) 0.092(3) 0.070(2) 0.037(2) 0.0130(17) 0.0123(18) C46 0.0549(16) 0.116(3) 0.0511(16) 0.0238(18) -0.0001(13) -0.0094(17) C47 0.083(2) 0.084(2) 0.066(2) -0.0126(18) -0.0007(17) -0.0233(18) N3 0.0665(14) 0.0430(11) 0.0816(17) -0.0082(11) 0.0189(13) -0.0248(10) C36 0.0456(12) 0.0674(17) 0.0652(17) -0.0217(14) -0.0142(12) -0.0071(12) C37 0.0852(19) 0.0515(14) 0.0419(13) 0.0013(11) -0.0182(13) -0.0055(13) C38 0.0812(19) 0.0617(16) 0.0425(13) -0.0010(12) 0.0047(13) -0.0373(14) C39 0.0412(12) 0.094(2) 0.0524(15) -0.0088(15) -0.0081(11) -0.0192(13) C40 0.0703(18) 0.0551(15) 0.0539(15) 0.0107(13) 0.0004(13) 0.0123(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.0263(12) 2_556 ? Co1 O1 2.0332(12) . ? Co1 O5 2.0355(13) 2_556 ? Co1 O2 2.0542(13) . ? Co1 N2 2.1563(16) . ? Co1 N1 2.1707(16) . ? O1 C7 1.265(2) . ? O2 C9 1.288(2) . ? O3 C15 1.342(2) . ? O3 H3 0.92(3) . ? O4 C17 1.266(2) . ? O4 Co1 2.0263(12) 2_556 ? O5 C19 1.275(2) . ? O5 Co1 2.0355(13) 2_556 ? N1 C26 1.338(2) . ? N1 C30 1.339(2) . ? N2 C35 1.335(3) . ? N2 C31 1.339(2) . ? C1 C6 1.386(3) . ? C1 C2 1.394(3) . ? C1 C7 1.499(2) . ? C2 C3 1.389(3) . ? C2 H2A 0.9500 . ? C3 C4 1.384(4) . ? C3 H3A 0.9500 . ? C4 C5 1.379(3) . ? C4 H4A 0.9500 . ? C5 C6 1.389(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.407(3) . ? C8 C9 1.399(2) . ? C8 H8 1.00(2) . ? C9 C10 1.491(2) . ? C10 C11 1.401(2) . ? C10 C15 1.419(2) . ? C11 C12 1.387(3) . ? C11 H11A 0.9500 . ? C12 C13 1.391(2) . ? C12 C16 1.510(3) . ? C13 C14 1.389(2) . ? C13 H13A 0.9500 . ? C14 C15 1.407(2) . ? C14 C17 1.498(2) . ? C16 H16C 0.9800 . ? C16 H16B 0.9800 . ? C16 H16A 0.9800 . ? C17 C18 1.410(2) . ? C18 C19 1.398(2) . ? C18 H18 1.02(2) . ? C19 C20 1.500(2) . ? C20 C25 1.389(2) . ? C20 C21 1.392(3) . ? C21 C22 1.385(3) . ? C21 H21A 0.9500 . ? C22 C23 1.381(3) . ? C22 H22A 0.9500 . ? C23 C24 1.387(3) . ? C23 H23A 0.9500 . ? C24 C25 1.386(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.383(3) . ? C26 H26A 0.9500 . ? C27 C28 1.374(3) . ? C27 H27A 0.9500 . ? C28 C29 1.381(3) . ? C28 H28A 0.9500 . ? C29 C30 1.370(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.387(3) . ? C31 H31A 0.9500 . ? C32 C33 1.372(4) . ? C32 H32A 0.9500 . ? C33 C34 1.379(4) . ? C33 H33A 0.9500 . ? C34 C35 1.381(3) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C41 C46 1.367(4) . ? C41 C42 1.369(4) . ? C41 C47 1.505(5) . ? C42 C43 1.381(4) . ? C42 H42A 0.9500 . ? C43 C44 1.414(5) . ? C43 H43A 0.9500 . ? C44 C45 1.354(6) . ? C44 H44A 0.9500 . ? C45 C46 1.352(6) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 H47C 0.9800 . ? C47 H47B 0.9800 . ? C47 H47A 0.9800 . ? N3 C36 1.313(4) . ? N3 C40 1.331(4) . ? C36 C37 1.350(4) . ? C36 H36A 0.9500 . ? C37 C38 1.343(4) . ? C37 H37A 0.9500 . ? C38 C39 1.359(4) . ? C38 H38A 0.9500 . ? C39 C40 1.388(4) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? 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 O4 Co1 O1 174.52(5) 2_556 . ? O4 Co1 O5 87.28(5) 2_556 2_556 ? O1 Co1 O5 98.15(5) . 2_556 ? O4 Co1 O2 87.76(5) 2_556 . ? O1 Co1 O2 86.79(5) . . ? O5 Co1 O2 174.64(5) 2_556 . ? O4 Co1 N2 92.68(5) 2_556 . ? O1 Co1 N2 88.10(6) . . ? O5 Co1 N2 89.43(6) 2_556 . ? O2 Co1 N2 92.83(6) . . ? O4 Co1 N1 89.95(5) 2_556 . ? O1 Co1 N1 89.57(6) . . ? O5 Co1 N1 87.69(6) 2_556 . ? O2 Co1 N1 90.28(6) . . ? N2 Co1 N1 176.00(6) . . ? C7 O1 Co1 126.16(11) . . ? C9 O2 Co1 126.34(11) . . ? C15 O3 H3 105.3(18) . . ? C17 O4 Co1 124.99(11) . 2_556 ? C19 O5 Co1 123.27(11) . 2_556 ? C26 N1 C30 117.49(17) . . ? C26 N1 Co1 124.40(13) . . ? C30 N1 Co1 117.91(13) . . ? C35 N2 C31 117.69(17) . . ? C35 N2 Co1 119.94(13) . . ? C31 N2 Co1 122.20(14) . . ? C6 C1 C2 118.91(16) . . ? C6 C1 C7 123.10(17) . . ? C2 C1 C7 117.99(17) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 119.49(19) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C1 C6 C5 120.5(2) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? O1 C7 C8 125.99(15) . . ? O1 C7 C1 115.66(15) . . ? C8 C7 C1 118.33(16) . . ? C9 C8 C7 125.10(17) . . ? C9 C8 H8 118.0(14) . . ? C7 C8 H8 116.9(14) . . ? O2 C9 C8 123.16(16) . . ? O2 C9 C10 116.18(14) . . ? C8 C9 C10 120.65(15) . . ? C11 C10 C15 118.44(15) . . ? C11 C10 C9 121.44(14) . . ? C15 C10 C9 120.12(15) . . ? C12 C11 C10 122.41(15) . . ? C12 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? C11 C12 C13 117.73(17) . . ? C11 C12 C16 121.29(16) . . ? C13 C12 C16 120.97(17) . . ? C14 C13 C12 122.53(17) . . ? C14 C13 H13A 118.7 . . ? C12 C13 H13A 118.7 . . ? C13 C14 C15 119.05(15) . . ? C13 C14 C17 119.60(15) . . ? C15 C14 C17 121.24(15) . . ? O3 C15 C14 117.93(14) . . ? O3 C15 C10 122.32(15) . . ? C14 C15 C10 119.74(15) . . ? C12 C16 H16C 109.5 . . ? C12 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C12 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? O4 C17 C18 124.82(15) . . ? O4 C17 C14 116.30(15) . . ? C18 C17 C14 118.74(15) . . ? C19 C18 C17 124.04(16) . . ? C19 C18 H18 116.6(13) . . ? C17 C18 H18 118.9(13) . . ? O5 C19 C18 125.50(16) . . ? O5 C19 C20 115.03(14) . . ? C18 C19 C20 119.46(15) . . ? C25 C20 C21 118.82(17) . . ? C25 C20 C19 118.80(16) . . ? C21 C20 C19 122.34(16) . . ? C22 C21 C20 120.33(18) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C21 120.33(19) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 119.91(19) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 119.69(18) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C20 120.88(18) . . ? C24 C25 H25A 119.6 . . ? C20 C25 H25A 119.6 . . ? N1 C26 C27 122.61(18) . . ? N1 C26 H26A 118.7 . . ? C27 C26 H26A 118.7 . . ? C28 C27 C26 119.1(2) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 118.7(2) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C30 C29 C28 118.8(2) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? N1 C30 C29 123.29(19) . . ? N1 C30 H30A 118.4 . . ? C29 C30 H30A 118.4 . . ? N2 C31 C32 122.7(2) . . ? N2 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? C33 C32 C31 118.7(2) . . ? C33 C32 H32A 120.7 . . ? C31 C32 H32A 120.7 . . ? C32 C33 C34 119.3(2) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? C33 C34 C35 118.5(2) . . ? C33 C34 H34A 120.7 . . ? C35 C34 H34A 120.7 . . ? N2 C35 C34 123.1(2) . . ? N2 C35 H35A 118.4 . . ? C34 C35 H35A 118.4 . . ? C46 C41 C42 119.2(3) . . ? C46 C41 C47 118.8(3) . . ? C42 C41 C47 122.0(3) . . ? C41 C42 C43 121.1(3) . . ? C41 C42 H42A 119.4 . . ? C43 C42 H42A 119.4 . . ? C42 C43 C44 118.3(3) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? C45 C44 C43 119.0(3) . . ? C45 C44 H44A 120.5 . . ? C43 C44 H44A 120.5 . . ? C46 C45 C44 121.6(3) . . ? C46 C45 H45A 119.2 . . ? C44 C45 H45A 119.2 . . ? C45 C46 C41 120.7(4) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C41 C47 H47C 109.5 . . ? C41 C47 H47B 109.5 . . ? H47C C47 H47B 109.5 . . ? C41 C47 H47A 109.5 . . ? H47C C47 H47A 109.5 . . ? H47B C47 H47A 109.5 . . ? C36 N3 C40 116.2(2) . . ? N3 C36 C37 124.8(3) . . ? N3 C36 H36A 117.6 . . ? C37 C36 H36A 117.6 . . ? C38 C37 C36 118.4(3) . . ? C38 C37 H37A 120.8 . . ? C36 C37 H37A 120.8 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 C40 117.4(3) . . ? C38 C39 H39A 121.3 . . ? C40 C39 H39A 121.3 . . ? N3 C40 C39 123.0(3) . . ? N3 C40 H40A 118.5 . . ? C39 C40 H40A 118.5 . . ? 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 O4 Co1 O1 C7 -17.6(6) 2_556 . . . ? O5 Co1 O1 C7 154.95(14) 2_556 . . . ? O2 Co1 O1 C7 -22.96(15) . . . . ? N2 Co1 O1 C7 -115.90(15) . . . . ? N1 Co1 O1 C7 67.35(15) . . . . ? O4 Co1 O2 C9 -152.64(14) 2_556 . . . ? O1 Co1 O2 C9 26.85(14) . . . . ? O5 Co1 O2 C9 -130.4(5) 2_556 . . . ? N2 Co1 O2 C9 114.79(14) . . . . ? N1 Co1 O2 C9 -62.70(14) . . . . ? O4 Co1 N1 C26 39.68(16) 2_556 . . . ? O1 Co1 N1 C26 -134.86(16) . . . . ? O5 Co1 N1 C26 126.96(16) 2_556 . . . ? O2 Co1 N1 C26 -48.08(16) . . . . ? N2 Co1 N1 C26 170.7(8) . . . . ? O4 Co1 N1 C30 -135.01(15) 2_556 . . . ? O1 Co1 N1 C30 50.45(15) . . . . ? O5 Co1 N1 C30 -47.73(14) 2_556 . . . ? O2 Co1 N1 C30 137.23(14) . . . . ? N2 Co1 N1 C30 -4.0(9) . . . . ? O4 Co1 N2 C35 55.58(15) 2_556 . . . ? O1 Co1 N2 C35 -129.85(15) . . . . ? O5 Co1 N2 C35 -31.67(15) 2_556 . . . ? O2 Co1 N2 C35 143.46(15) . . . . ? N1 Co1 N2 C35 -75.4(9) . . . . ? O4 Co1 N2 C31 -129.35(15) 2_556 . . . ? O1 Co1 N2 C31 45.22(15) . . . . ? O5 Co1 N2 C31 143.40(15) 2_556 . . . ? O2 Co1 N2 C31 -41.47(15) . . . . ? N1 Co1 N2 C31 99.7(9) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? C7 C1 C2 C3 179.5(2) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C2 C1 C6 C5 1.3(3) . . . . ? C7 C1 C6 C5 -178.2(2) . . . . ? C4 C5 C6 C1 -1.5(4) . . . . ? Co1 O1 C7 C8 13.9(3) . . . . ? Co1 O1 C7 C1 -167.74(11) . . . . ? C6 C1 C7 O1 156.0(2) . . . . ? C2 C1 C7 O1 -23.4(3) . . . . ? C6 C1 C7 C8 -25.5(3) . . . . ? C2 C1 C7 C8 155.06(19) . . . . ? O1 C7 C8 C9 2.8(3) . . . . ? C1 C7 C8 C9 -175.51(17) . . . . ? Co1 O2 C9 C8 -21.2(2) . . . . ? Co1 O2 C9 C10 159.10(11) . . . . ? C7 C8 C9 O2 1.2(3) . . . . ? C7 C8 C9 C10 -179.14(17) . . . . ? O2 C9 C10 C11 170.83(16) . . . . ? C8 C9 C10 C11 -8.9(3) . . . . ? O2 C9 C10 C15 -8.8(2) . . . . ? C8 C9 C10 C15 171.45(16) . . . . ? C15 C10 C11 C12 0.3(3) . . . . ? C9 C10 C11 C12 -179.34(17) . . . . ? C10 C11 C12 C13 -1.9(3) . . . . ? C10 C11 C12 C16 178.17(19) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C16 C12 C13 C14 -179.4(2) . . . . ? C12 C13 C14 C15 2.0(3) . . . . ? C12 C13 C14 C17 -174.17(17) . . . . ? C13 C14 C15 O3 175.08(16) . . . . ? C17 C14 C15 O3 -8.8(2) . . . . ? C13 C14 C15 C10 -3.5(3) . . . . ? C17 C14 C15 C10 172.60(15) . . . . ? C11 C10 C15 O3 -176.16(16) . . . . ? C9 C10 C15 O3 3.5(3) . . . . ? C11 C10 C15 C14 2.4(2) . . . . ? C9 C10 C15 C14 -177.93(15) . . . . ? Co1 O4 C17 C18 -16.4(2) 2_556 . . . ? Co1 O4 C17 C14 167.89(11) 2_556 . . . ? C13 C14 C17 O4 136.22(18) . . . . ? C15 C14 C17 O4 -39.9(2) . . . . ? C13 C14 C17 C18 -39.7(2) . . . . ? C15 C14 C17 C18 144.17(17) . . . . ? O4 C17 C18 C19 -7.3(3) . . . . ? C14 C17 C18 C19 168.26(17) . . . . ? Co1 O5 C19 C18 22.0(2) 2_556 . . . ? Co1 O5 C19 C20 -159.63(11) 2_556 . . . ? C17 C18 C19 O5 4.0(3) . . . . ? C17 C18 C19 C20 -174.30(16) . . . . ? O5 C19 C20 C25 -31.7(2) . . . . ? C18 C19 C20 C25 146.83(18) . . . . ? O5 C19 C20 C21 146.01(17) . . . . ? C18 C19 C20 C21 -35.5(3) . . . . ? C25 C20 C21 C22 1.9(3) . . . . ? C19 C20 C21 C22 -175.73(18) . . . . ? C20 C21 C22 C23 -1.9(3) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 1.0(3) . . . . ? C23 C24 C25 C20 -0.9(3) . . . . ? C21 C20 C25 C24 -0.5(3) . . . . ? C19 C20 C25 C24 177.19(18) . . . . ? C30 N1 C26 C27 -0.3(3) . . . . ? Co1 N1 C26 C27 -175.03(15) . . . . ? N1 C26 C27 C28 0.7(3) . . . . ? C26 C27 C28 C29 -0.5(3) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? C26 N1 C30 C29 -0.3(3) . . . . ? Co1 N1 C30 C29 174.75(16) . . . . ? C28 C29 C30 N1 0.5(3) . . . . ? C35 N2 C31 C32 0.9(3) . . . . ? Co1 N2 C31 C32 -174.23(16) . . . . ? N2 C31 C32 C33 0.0(3) . . . . ? C31 C32 C33 C34 -1.3(4) . . . . ? C32 C33 C34 C35 1.5(4) . . . . ? C31 N2 C35 C34 -0.7(3) . . . . ? Co1 N2 C35 C34 174.59(17) . . . . ? C33 C34 C35 N2 -0.5(4) . . . . ? C46 C41 C42 C43 -1.3(4) . . . . ? C47 C41 C42 C43 179.8(3) . . . . ? C41 C42 C43 C44 0.8(4) . . . . ? C42 C43 C44 C45 0.1(4) . . . . ? C43 C44 C45 C46 -0.6(5) . . . . ? C44 C45 C46 C41 0.2(5) . . . . ? C42 C41 C46 C45 0.8(4) . . . . ? C47 C41 C46 C45 179.7(3) . . . . ? C40 N3 C36 C37 -1.4(4) . . . . ? N3 C36 C37 C38 -0.3(5) . . . . ? C36 C37 C38 C39 1.5(4) . . . . ? C37 C38 C39 C40 -1.1(4) . . . . ? C36 N3 C40 C39 1.8(4) . . . . ? C38 C39 C40 N3 -0.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.92(3) 1.66(3) 2.5034(17) 152(3) . _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 29.52 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.486 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.061 # Attachment '[Co3(HL)3].CIF' data_ga102 _database_code_depnum_ccdc_archive 'CCDC 298736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H54 Co3 O15' _chemical_formula_weight 1371.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.979(4) _cell_length_b 15.001(4) _cell_length_c 16.832(8) _cell_angle_alpha 110.075(9) _cell_angle_beta 106.062(9) _cell_angle_gamma 106.923(7) _cell_volume 3085.7(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5230 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.56 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6897 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEXII CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 24618 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.76 _reflns_number_total 11869 _reflns_number_gt 9942 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _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 and local programs' _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. A number of crystals of this material were tried all of which produced diffraction patterns with reflections that did not index to this cell and could not be indexed to another cell. It is believe that this is due to some form of twinning, that could not be resolved. The unit cell have metric symmetry C-monoclinic but with an R(int) of 23.3%. However, in the triclinic system R(int) is 4.7%. The structure solved and refined in P-1, PLATON was use to check for high symmetry but could not find any. The twin law (0 1 0 1 0 0 -1 -1 -1) was used successfullly to account for the C-monoclinic character of the twinning, 2-fold rotation about the monoclinic unique axis. It is feel that the final R1 on this data is high than because there is another component of twinning that could not be modelling (the additional reflections). Hydrogen where place geometrically where possible. It was not possible to find the methyl or hydroxyl hydrogens in the difference map and so they were omitted from the refinement as it was not possible to place them geometrically. The disordered phenyl group was modelled with displacement parameter restrains. All non-hydrogens were refined anisotropically except the low occupancy Co. While this is not an ideal refinement it does show the geometry of the compound. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11869 _refine_ls_number_parameters 897 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.1250 _refine_ls_wR_factor_ref 0.3908 _refine_ls_wR_factor_gt 0.3631 _refine_ls_goodness_of_fit_ref 1.735 _refine_ls_restrained_S_all 1.723 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.76106(9) 0.75278(9) 0.42901(8) 0.0270(3) Uani 1 1 d . . . Co2 Co 0.77706(9) 0.59875(9) 0.28506(8) 0.0249(3) Uani 0.95 1 d P . . Co2' Co 0.7887(17) 0.4816(18) 0.1775(14) 0.022(4) Uiso 0.05 1 d P . . Co3 Co 0.80562(9) 0.33176(9) 0.03788(8) 0.0256(3) Uani 1 1 d . . . O1 O 0.6785(5) 0.8331(5) 0.4026(5) 0.0347(15) Uani 1 1 d . A . O2 O 0.6559(5) 0.6301(5) 0.2994(4) 0.0294(13) Uani 1 1 d . A . O3 O 0.6848(5) 0.5303(5) 0.1430(4) 0.0292(13) Uani 1 1 d . A . O4 O 0.6862(5) 0.3796(5) 0.0283(5) 0.0310(14) Uani 1 1 d . A . O5 O 0.6968(5) 0.1839(5) -0.0390(5) 0.0324(14) Uani 1 1 d . A . C1 C 0.556(2) 0.886(2) 0.3292(19) 0.042(4) Uani 0.50 1 d PU A -1 C2 C 0.6200(18) 0.9907(18) 0.3898(16) 0.043(3) Uani 0.50 1 d PU A -1 H2 H 0.6879 1.0102 0.4312 0.052 Uiso 0.50 1 calc PR A -1 C3 C 0.5863(19) 1.0682(18) 0.3910(16) 0.044(4) Uani 0.50 1 d PU A -1 H3 H 0.6324 1.1405 0.4268 0.053 Uiso 0.50 1 calc PR A -1 C4 C 0.4800(18) 1.0352(18) 0.3367(17) 0.046(3) Uani 0.50 1 d PU A -1 H4 H 0.4530 1.0859 0.3413 0.055 Uiso 0.50 1 calc PR A -1 C5 C 0.415(3) 0.929(2) 0.277(2) 0.044(4) Uani 0.50 1 d PU A -1 H5 H 0.3454 0.9084 0.2394 0.053 Uiso 0.50 1 calc PR A -1 C6 C 0.451(2) 0.856(2) 0.272(3) 0.041(4) Uani 0.50 1 d PU A -1 H6 H 0.4072 0.7842 0.2301 0.049 Uiso 0.50 1 calc PR A -1 C1A C 0.544(2) 0.877(2) 0.3519(19) 0.040(4) Uani 0.50 1 d PU A -2 C2A C 0.5690(18) 0.9475(18) 0.4432(16) 0.044(3) Uani 0.50 1 d PU A -2 H2A H 0.6182 0.9492 0.4941 0.053 Uiso 0.50 1 calc PR A -2 C3A C 0.5239(19) 1.0127(19) 0.4592(17) 0.048(4) Uani 0.50 1 d PU A -2 H3A H 0.5403 1.0592 0.5215 0.058 Uiso 0.50 1 calc PR A -2 C4A C 0.4515(19) 1.0131(19) 0.3839(18) 0.048(3) Uani 0.50 1 d PU A -2 H4A H 0.4161 1.0559 0.3961 0.058 Uiso 0.50 1 calc PR A -2 C5A C 0.433(3) 0.951(2) 0.293(3) 0.046(4) Uani 0.50 1 d PU A -2 H5A H 0.3926 0.9574 0.2426 0.055 Uiso 0.50 1 calc PR A -2 C6A C 0.478(2) 0.876(3) 0.280(3) 0.044(4) Uani 0.50 1 d PU A -2 H6A H 0.4608 0.8259 0.2182 0.053 Uiso 0.50 1 calc PR A -2 C7 C 0.5965(8) 0.8042(8) 0.3339(7) 0.039(2) Uani 1 1 d . . . C8 C 0.5464(8) 0.7057(8) 0.2513(7) 0.037(2) Uani 1 1 d . A . H8 H 0.4859 0.6936 0.2034 0.045 Uiso 1 1 calc R . . C9 C 0.5795(7) 0.6269(7) 0.2360(6) 0.0295(18) Uani 1 1 d . . . C10 C 0.5236(7) 0.5276(7) 0.1473(6) 0.0283(18) Uani 1 1 d . A . C11 C 0.4166(8) 0.4771(8) 0.1029(7) 0.035(2) Uani 1 1 d . . . H11 H 0.3782 0.5107 0.1266 0.042 Uiso 1 1 calc R A . C12 C 0.3650(7) 0.3805(8) 0.0261(7) 0.037(2) Uani 1 1 d . A . C13 C 0.4215(7) 0.3306(7) -0.0068(6) 0.0313(19) Uani 1 1 d . . . H13 H 0.3859 0.2628 -0.0589 0.038 Uiso 1 1 calc R A . C14 C 0.5299(7) 0.3771(7) 0.0344(6) 0.0281(18) Uani 1 1 d . A . C15 C 0.5790(7) 0.4788(7) 0.1087(7) 0.0306(19) Uani 1 1 d . . . C16 C 0.2481(8) 0.3265(9) -0.0211(10) 0.058(4) Uani 1 1 d . . . C17 C 0.5910(7) 0.3201(7) 0.0042(6) 0.0273(17) Uani 1 1 d . . . C18 C 0.5480(7) 0.2124(7) -0.0382(7) 0.0321(19) Uani 1 1 d . A . H18 H 0.4762 0.1773 -0.0571 0.039 Uiso 1 1 calc R . . C19 C 0.6011(7) 0.1482(8) -0.0566(7) 0.033(2) Uani 1 1 d . . . C20 C 0.5466(8) 0.0353(8) -0.0933(7) 0.037(2) Uani 1 1 d . A . C21 C 0.4386(9) -0.0195(9) -0.1477(9) 0.049(3) Uani 1 1 d . . . H21 H 0.4000 0.0173 -0.1627 0.059 Uiso 1 1 calc R A . C22 C 0.3894(10) -0.1270(9) -0.1787(11) 0.058(4) Uani 1 1 d . A . H22 H 0.3170 -0.1628 -0.2136 0.070 Uiso 1 1 calc R . . C23 C 0.4443(11) -0.1824(9) -0.1598(10) 0.056(3) Uani 1 1 d . . . H23 H 0.4095 -0.2555 -0.1801 0.067 Uiso 1 1 calc R A . C24 C 0.5493(11) -0.1316(9) -0.1113(10) 0.053(3) Uani 1 1 d . A . H24 H 0.5873 -0.1705 -0.1009 0.064 Uiso 1 1 calc R . . C25 C 0.6006(9) -0.0238(9) -0.0773(9) 0.046(3) Uani 1 1 d . . . H25 H 0.6731 0.0104 -0.0428 0.055 Uiso 1 1 calc R A . O1' O 0.8908(5) 0.8705(5) 0.5383(5) 0.0325(14) Uani 1 1 d . . . O2' O 0.8458(5) 0.7631(5) 0.3485(4) 0.0273(13) Uani 1 1 d . . . O3' O 0.9002(5) 0.6091(5) 0.2506(5) 0.0303(13) Uani 1 1 d . . . O4' O 0.9039(5) 0.4891(5) 0.1149(5) 0.0308(14) Uani 1 1 d . . . O5' O 0.8212(5) 0.3495(5) -0.0717(4) 0.0295(13) Uani 1 1 d . . . C1' C 1.0635(8) 0.9524(7) 0.6418(7) 0.0317(19) Uani 1 1 d . . . C2' C 1.0396(8) 0.9265(8) 0.7073(7) 0.035(2) Uani 1 1 d . . . H2' H 0.9720 0.8786 0.6908 0.043 Uiso 1 1 calc R . . C3' C 1.1140(9) 0.9704(9) 0.7962(8) 0.040(2) Uani 1 1 d . . . H3' H 1.0979 0.9504 0.8400 0.049 Uiso 1 1 calc R . . C4' C 1.2123(9) 1.0436(8) 0.8230(7) 0.041(2) Uani 1 1 d . . . H4' H 1.2632 1.0736 0.8846 0.049 Uiso 1 1 calc R . . C5' C 1.2351(9) 1.0725(9) 0.7578(8) 0.043(2) Uani 1 1 d . . . H5' H 1.3011 1.1245 0.7756 0.052 Uiso 1 1 calc R . . C6' C 1.1618(8) 1.0257(8) 0.6679(7) 0.035(2) Uani 1 1 d . . . H6' H 1.1784 1.0435 0.6232 0.042 Uiso 1 1 calc R . . C7' C 0.9818(7) 0.9000(7) 0.5454(7) 0.0291(18) Uani 1 1 d . . . C8' C 1.0106(7) 0.8830(7) 0.4691(7) 0.0286(18) Uani 1 1 d . . . H8' H 1.0803 0.9210 0.4824 0.034 Uiso 1 1 calc R . . C9' C 0.9435(7) 0.8149(7) 0.3776(7) 0.0284(18) Uani 1 1 d . . . C10' C 0.9846(7) 0.7941(7) 0.3036(6) 0.0278(18) Uani 1 1 d . . . C11' C 1.0503(7) 0.8753(7) 0.2968(7) 0.032(2) Uani 1 1 d . . . H11' H 1.0762 0.9453 0.3438 0.038 Uiso 1 1 calc R . . C12' C 1.0793(8) 0.8568(8) 0.2230(7) 0.036(2) Uani 1 1 d . . . C13' C 1.0384(7) 0.7531(7) 0.1526(7) 0.0300(18) Uani 1 1 d . . . H13' H 1.0539 0.7395 0.0998 0.036 Uiso 1 1 calc R . . C14' C 0.9752(7) 0.6704(7) 0.1600(7) 0.0293(18) Uani 1 1 d . . . C15' C 0.9521(7) 0.6901(7) 0.2368(7) 0.0314(19) Uani 1 1 d . . . C16' C 1.1502(9) 0.9467(9) 0.2163(8) 0.046(3) Uani 1 1 d . . . C17' C 0.9277(7) 0.5584(7) 0.0857(6) 0.0287(18) Uani 1 1 d . . . C18' C 0.9071(8) 0.5355(7) -0.0056(6) 0.0306(19) Uani 1 1 d . . . H18' H 0.9326 0.5915 -0.0194 0.037 Uiso 1 1 calc R . . C19' C 0.8490(7) 0.4314(7) -0.0807(6) 0.0292(19) Uani 1 1 d . . . C20' C 0.8186(8) 0.4159(8) -0.1796(6) 0.033(2) Uani 1 1 d . . . C21' C 0.8342(10) 0.4954(9) -0.2033(8) 0.050(3) Uani 1 1 d . . . H21' H 0.8706 0.5663 -0.1559 0.060 Uiso 1 1 calc R . . C22' C 0.7968(13) 0.4734(10) -0.2976(8) 0.063(4) Uani 1 1 d . . . H22' H 0.8077 0.5295 -0.3135 0.075 Uiso 1 1 calc R . . C23' C 0.7455(11) 0.3732(11) -0.3656(8) 0.055(3) Uani 1 1 d . . . H23' H 0.7191 0.3588 -0.4290 0.066 Uiso 1 1 calc R . . C24' C 0.7317(14) 0.2940(11) -0.3434(9) 0.072(5) Uani 1 1 d . . . H24' H 0.6969 0.2236 -0.3917 0.086 Uiso 1 1 calc R . . C25' C 0.7675(13) 0.3129(9) -0.2510(8) 0.060(4) Uani 1 1 d . . . H25' H 0.7571 0.2559 -0.2366 0.072 Uiso 1 1 calc R . . O1" O 0.6927(5) 0.7163(5) 0.5103(5) 0.0335(14) Uani 1 1 d . . . O2" O 0.8101(5) 0.6351(5) 0.4238(4) 0.0296(13) Uani 1 1 d . . . O3" O 0.7572(5) 0.4501(5) 0.2693(5) 0.0310(14) Uani 1 1 d . . . O4" O 0.8045(5) 0.3402(5) 0.1630(4) 0.0285(13) Uani 1 1 d . . . O5" O 0.9158(5) 0.2769(5) 0.0630(5) 0.0323(14) Uani 1 1 d . . . C1" C 0.6160(8) 0.6291(8) 0.5839(7) 0.038(2) Uani 1 1 d . . . C2" C 0.5670(10) 0.6957(11) 0.5993(9) 0.051(3) Uani 1 1 d . . . H2" H 0.5730 0.7446 0.5748 0.061 Uiso 1 1 calc R . . C3" C 0.5096(11) 0.6894(12) 0.6506(10) 0.058(3) Uani 1 1 d . . . H3" H 0.4782 0.7361 0.6631 0.070 Uiso 1 1 calc R . . C4" C 0.4972(10) 0.6164(11) 0.6842(10) 0.059(3) Uani 1 1 d . . . H4" H 0.4569 0.6130 0.7189 0.070 Uiso 1 1 calc R . . C5" C 0.5426(11) 0.5493(11) 0.6677(9) 0.055(3) Uani 1 1 d . . . H5" H 0.5335 0.4983 0.6897 0.066 Uiso 1 1 calc R . . C6" C 0.6030(11) 0.5568(10) 0.6174(8) 0.050(3) Uani 1 1 d . . . H6" H 0.6356 0.5110 0.6065 0.060 Uiso 1 1 calc R . . C7" C 0.6838(7) 0.6424(7) 0.5324(6) 0.0305(19) Uani 1 1 d . . . C8" C 0.7278(9) 0.5707(8) 0.5078(7) 0.037(2) Uani 1 1 d . . . H8" H 0.7184 0.5205 0.5307 0.045 Uiso 1 1 calc R . . C9" C 0.7823(7) 0.5669(7) 0.4545(6) 0.0289(18) Uani 1 1 d . . . C10" C 0.8164(7) 0.4800(7) 0.4276(7) 0.0280(18) Uani 1 1 d . . . C11" C 0.8587(7) 0.4505(8) 0.4931(7) 0.0312(19) Uani 1 1 d . . . H11" H 0.8628 0.4832 0.5542 0.037 Uiso 1 1 calc R . . C12" C 0.8955(8) 0.3733(8) 0.4712(7) 0.037(2) Uani 1 1 d . . . C13" C 0.8964(7) 0.3337(8) 0.3845(7) 0.034(2) Uani 1 1 d . . . H13" H 0.9258 0.2853 0.3703 0.041 Uiso 1 1 calc R . . C14" C 0.8560(8) 0.3620(7) 0.3170(6) 0.0308(18) Uani 1 1 d . . . C15" C 0.8087(7) 0.4314(8) 0.3385(7) 0.0317(19) Uani 1 1 d . . . C16" C 0.9375(11) 0.3409(11) 0.5435(8) 0.048(3) Uani 1 1 d . . . C17" C 0.8667(7) 0.3280(7) 0.2281(7) 0.0286(18) Uani 1 1 d . . . C18" C 0.9357(8) 0.2890(7) 0.2127(7) 0.035(2) Uani 1 1 d . . . H18" H 0.9739 0.2774 0.2605 0.042 Uiso 1 1 calc R . . C19" C 0.9551(7) 0.2644(7) 0.1325(7) 0.0297(18) Uani 1 1 d . . . C20" C 1.0327(8) 0.2190(7) 0.1264(7) 0.034(2) Uani 1 1 d . . . C21" C 1.1094(8) 0.2312(9) 0.2034(8) 0.040(2) Uani 1 1 d . . . H21" H 1.1149 0.2691 0.2642 0.048 Uiso 1 1 calc R . . C22" C 1.1781(9) 0.1881(9) 0.1920(10) 0.053(3) Uani 1 1 d . . . H22" H 1.2303 0.1968 0.2452 0.063 Uiso 1 1 calc R . . C23" C 1.1723(10) 0.1333(10) 0.1054(10) 0.054(3) Uani 1 1 d . . . H23" H 1.2194 0.1036 0.0983 0.065 Uiso 1 1 calc R . . C24" C 1.0979(12) 0.1218(12) 0.0294(10) 0.060(4) Uani 1 1 d . . . H24" H 1.0933 0.0838 -0.0309 0.072 Uiso 1 1 calc R . . C25" C 1.0289(11) 0.1646(11) 0.0387(9) 0.051(3) Uani 1 1 d . . . H25" H 0.9785 0.1570 -0.0150 0.061 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 Co1 0.0240(6) 0.0244(6) 0.0402(6) 0.0184(5) 0.0172(5) 0.0122(5) Co2 0.0225(6) 0.0226(6) 0.0383(6) 0.0188(5) 0.0156(5) 0.0121(5) Co3 0.0236(6) 0.0219(6) 0.0378(6) 0.0175(5) 0.0151(5) 0.0114(5) O1 0.029(3) 0.030(3) 0.049(4) 0.021(3) 0.015(3) 0.016(3) O2 0.030(3) 0.030(3) 0.039(3) 0.020(3) 0.019(3) 0.018(3) O3 0.021(3) 0.026(3) 0.038(3) 0.015(3) 0.012(2) 0.008(2) O4 0.023(3) 0.027(3) 0.046(3) 0.018(3) 0.017(3) 0.011(2) O5 0.031(3) 0.026(3) 0.047(3) 0.018(3) 0.020(3) 0.015(3) C1 0.041(6) 0.042(6) 0.058(7) 0.027(6) 0.027(6) 0.026(5) C2 0.041(6) 0.041(5) 0.060(6) 0.028(5) 0.025(5) 0.027(5) C3 0.050(7) 0.037(6) 0.059(7) 0.029(6) 0.027(6) 0.024(6) C4 0.048(6) 0.040(6) 0.063(7) 0.028(5) 0.022(5) 0.034(5) C5 0.044(6) 0.042(6) 0.063(6) 0.028(5) 0.025(5) 0.031(5) C6 0.041(7) 0.042(6) 0.059(6) 0.029(5) 0.027(6) 0.028(5) C1A 0.040(6) 0.042(6) 0.058(6) 0.029(5) 0.025(5) 0.028(5) C2A 0.041(6) 0.047(6) 0.059(6) 0.026(5) 0.027(5) 0.028(5) C3A 0.043(7) 0.046(7) 0.064(7) 0.024(6) 0.024(6) 0.027(6) C4A 0.047(6) 0.043(6) 0.067(7) 0.030(5) 0.022(5) 0.031(5) C5A 0.046(6) 0.042(6) 0.063(6) 0.031(5) 0.021(5) 0.030(5) C6A 0.044(7) 0.043(6) 0.059(6) 0.029(5) 0.023(6) 0.028(5) C7 0.036(5) 0.035(5) 0.050(5) 0.019(4) 0.015(4) 0.024(4) C8 0.033(5) 0.040(5) 0.052(6) 0.027(5) 0.022(4) 0.022(4) C9 0.022(4) 0.031(4) 0.038(4) 0.019(4) 0.010(3) 0.013(4) C10 0.027(4) 0.027(4) 0.040(4) 0.021(4) 0.014(4) 0.016(4) C11 0.032(5) 0.039(5) 0.042(5) 0.023(4) 0.016(4) 0.021(4) C12 0.016(4) 0.038(5) 0.056(6) 0.025(5) 0.012(4) 0.012(4) C13 0.025(4) 0.029(4) 0.037(4) 0.015(4) 0.009(4) 0.013(4) C14 0.019(4) 0.029(4) 0.041(4) 0.020(4) 0.013(3) 0.011(3) C15 0.022(4) 0.032(4) 0.052(5) 0.027(4) 0.019(4) 0.015(4) C16 0.023(5) 0.039(6) 0.077(8) 0.005(6) 0.007(5) 0.010(4) C17 0.024(4) 0.028(4) 0.037(4) 0.019(4) 0.014(3) 0.014(3) C18 0.022(4) 0.026(4) 0.053(5) 0.023(4) 0.016(4) 0.009(3) C19 0.026(4) 0.033(5) 0.041(5) 0.016(4) 0.016(4) 0.015(4) C20 0.029(5) 0.029(5) 0.048(5) 0.015(4) 0.018(4) 0.010(4) C21 0.032(5) 0.031(5) 0.072(7) 0.020(5) 0.020(5) 0.006(4) C22 0.042(6) 0.030(5) 0.097(10) 0.022(6) 0.041(7) 0.006(5) C23 0.059(8) 0.025(5) 0.078(8) 0.020(5) 0.040(7) 0.004(5) C24 0.054(7) 0.033(5) 0.091(9) 0.039(6) 0.039(7) 0.019(5) C25 0.040(6) 0.032(5) 0.073(7) 0.026(5) 0.032(5) 0.016(4) O1' 0.032(3) 0.024(3) 0.043(3) 0.014(3) 0.019(3) 0.012(3) O2' 0.023(3) 0.024(3) 0.037(3) 0.015(3) 0.015(2) 0.010(2) O3' 0.025(3) 0.028(3) 0.042(3) 0.018(3) 0.015(3) 0.011(3) O4' 0.030(3) 0.023(3) 0.046(3) 0.020(3) 0.017(3) 0.014(3) O5' 0.026(3) 0.025(3) 0.040(3) 0.017(3) 0.014(3) 0.012(2) C1' 0.035(5) 0.028(4) 0.043(5) 0.021(4) 0.022(4) 0.017(4) C2' 0.040(5) 0.031(5) 0.038(5) 0.019(4) 0.018(4) 0.015(4) C3' 0.045(6) 0.038(5) 0.048(6) 0.025(5) 0.025(5) 0.017(5) C4' 0.043(6) 0.035(5) 0.032(5) 0.013(4) 0.008(4) 0.012(4) C5' 0.035(5) 0.039(5) 0.049(6) 0.022(5) 0.019(5) 0.005(4) C6' 0.034(5) 0.034(5) 0.039(5) 0.022(4) 0.014(4) 0.012(4) C7' 0.029(4) 0.022(4) 0.044(5) 0.021(4) 0.018(4) 0.012(3) C8' 0.024(4) 0.019(4) 0.047(5) 0.019(4) 0.017(4) 0.008(3) C9' 0.030(4) 0.024(4) 0.047(5) 0.024(4) 0.022(4) 0.018(4) C10' 0.024(4) 0.024(4) 0.042(5) 0.020(4) 0.013(4) 0.013(3) C11' 0.030(5) 0.024(4) 0.041(5) 0.014(4) 0.016(4) 0.014(4) C12' 0.040(5) 0.031(5) 0.039(5) 0.019(4) 0.017(4) 0.013(4) C13' 0.030(4) 0.026(4) 0.042(5) 0.020(4) 0.022(4) 0.011(4) C14' 0.023(4) 0.025(4) 0.046(5) 0.020(4) 0.017(4) 0.011(3) C15' 0.031(5) 0.028(4) 0.043(5) 0.023(4) 0.015(4) 0.014(4) C16' 0.043(6) 0.033(5) 0.057(6) 0.021(5) 0.026(5) 0.005(4) C17' 0.028(4) 0.019(4) 0.043(5) 0.018(4) 0.014(4) 0.010(3) C18' 0.034(5) 0.025(4) 0.041(5) 0.020(4) 0.020(4) 0.014(4) C19' 0.025(4) 0.031(4) 0.042(5) 0.022(4) 0.014(4) 0.017(4) C20' 0.034(5) 0.030(5) 0.035(4) 0.019(4) 0.012(4) 0.013(4) C21' 0.057(7) 0.030(5) 0.046(6) 0.022(5) 0.017(5) -0.002(5) C22' 0.081(10) 0.043(6) 0.044(6) 0.026(5) 0.015(6) 0.003(6) C23' 0.062(8) 0.054(7) 0.035(5) 0.021(5) 0.012(5) 0.016(6) C24' 0.096(12) 0.044(7) 0.039(6) 0.016(5) 0.003(7) 0.010(7) C25' 0.089(10) 0.028(5) 0.048(6) 0.024(5) 0.015(6) 0.013(6) O1" 0.033(3) 0.034(3) 0.046(3) 0.022(3) 0.025(3) 0.016(3) O2" 0.032(3) 0.027(3) 0.041(3) 0.020(3) 0.019(3) 0.017(3) O3" 0.033(3) 0.028(3) 0.043(3) 0.025(3) 0.017(3) 0.016(3) O4" 0.027(3) 0.030(3) 0.039(3) 0.021(3) 0.015(3) 0.017(3) O5" 0.030(3) 0.032(3) 0.044(3) 0.023(3) 0.017(3) 0.017(3) C1" 0.034(5) 0.039(5) 0.044(5) 0.020(4) 0.025(4) 0.013(4) C2" 0.047(6) 0.064(8) 0.066(7) 0.037(6) 0.043(6) 0.028(6) C3" 0.058(8) 0.070(9) 0.079(9) 0.042(7) 0.052(7) 0.035(7) C4" 0.046(7) 0.063(8) 0.067(8) 0.026(7) 0.038(6) 0.015(6) C5" 0.059(8) 0.055(7) 0.055(7) 0.030(6) 0.035(6) 0.012(6) C6" 0.064(8) 0.050(7) 0.051(6) 0.027(5) 0.041(6) 0.022(6) C7" 0.024(4) 0.030(4) 0.039(5) 0.020(4) 0.019(4) 0.004(4) C8" 0.050(6) 0.036(5) 0.037(5) 0.022(4) 0.022(4) 0.023(5) C9" 0.034(5) 0.023(4) 0.034(4) 0.018(4) 0.014(4) 0.012(4) C10" 0.023(4) 0.027(4) 0.046(5) 0.025(4) 0.019(4) 0.011(3) C11" 0.029(4) 0.033(5) 0.045(5) 0.029(4) 0.018(4) 0.016(4) C12" 0.042(5) 0.038(5) 0.052(6) 0.033(5) 0.024(5) 0.026(5) C13" 0.026(4) 0.034(5) 0.057(6) 0.030(4) 0.021(4) 0.018(4) C14" 0.033(5) 0.030(4) 0.038(4) 0.021(4) 0.017(4) 0.017(4) C15" 0.026(4) 0.035(5) 0.053(5) 0.034(4) 0.020(4) 0.018(4) C16" 0.059(7) 0.061(7) 0.060(7) 0.048(6) 0.034(6) 0.040(6) C17" 0.024(4) 0.020(4) 0.045(5) 0.019(4) 0.015(4) 0.009(3) C18" 0.036(5) 0.030(4) 0.049(5) 0.024(4) 0.019(4) 0.019(4) C19" 0.026(4) 0.020(4) 0.051(5) 0.021(4) 0.018(4) 0.012(3) C20" 0.033(5) 0.029(4) 0.050(5) 0.024(4) 0.020(4) 0.018(4) C21" 0.033(5) 0.039(5) 0.053(6) 0.024(5) 0.018(4) 0.019(4) C22" 0.033(5) 0.040(6) 0.086(9) 0.032(6) 0.018(6) 0.019(5) C23" 0.047(7) 0.051(7) 0.094(9) 0.043(7) 0.042(7) 0.034(6) C24" 0.067(8) 0.074(9) 0.067(8) 0.033(7) 0.042(7) 0.052(8) C25" 0.059(7) 0.060(7) 0.062(7) 0.039(6) 0.032(6) 0.041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.8404(17) . ? Co1 O1 2.027(6) . ? Co1 O2 2.069(6) . ? Co1 O1' 2.018(7) . ? Co1 O2' 2.110(6) . ? Co1 O1" 2.045(7) . ? Co1 O2" 2.086(6) . ? Co2 Co2' 2.14(2) . ? Co2 O2 2.058(6) . ? Co2 O3 2.084(6) . ? Co2 O2' 2.094(6) . ? Co2 O3' 2.062(7) . ? Co2 O2" 2.080(7) . ? Co2 O3" 2.072(6) . ? Co2' Co3 2.77(2) . ? Co2' O3 1.94(2) . ? Co2' O4 2.21(2) . ? Co2' O3' 1.83(2) . ? Co2' O4' 2.25(2) . ? Co2' O3" 1.90(2) . ? Co2' O4" 2.14(2) . ? Co3 O4 2.100(6) . ? Co3 O5 2.003(7) . ? Co3 O4' 2.059(7) . ? Co3 O5' 2.017(7) . ? Co3 O4" 2.070(7) . ? Co3 O5" 2.056(6) . ? O1 C7 1.262(12) . ? O2 C9 1.307(11) . ? O3 C15 1.385(11) . ? O4 C17 1.298(11) . ? O5 C19 1.280(12) . ? C1 C2 1.38(4) . ? C1 C6 1.43(4) . ? C1 C7 1.53(3) . ? C2 C3 1.39(3) . ? C3 C4 1.43(3) . ? C4 C5 1.39(4) . ? C5 C6 1.34(4) . ? C1A C2A 1.40(4) . ? C1A C6A 1.33(5) . ? C1A C7 1.52(3) . ? C2A C3A 1.34(3) . ? C3A C4A 1.43(3) . ? C4A C5A 1.38(4) . ? C5A C6A 1.47(4) . ? C7 C8 1.430(14) . ? C8 C9 1.384(12) . ? C9 C10 1.485(13) . ? C10 C11 1.394(14) . ? C10 C15 1.403(12) . ? C11 C12 1.369(15) . ? C12 C13 1.388(13) . ? C12 C16 1.522(13) . ? C13 C14 1.409(12) . ? C14 C15 1.400(13) . ? C14 C17 1.497(11) . ? C17 C18 1.373(13) . ? C18 C19 1.426(12) . ? C19 C20 1.454(14) . ? C20 C21 1.422(15) . ? C20 C25 1.405(15) . ? C21 C22 1.390(16) . ? C22 C23 1.38(2) . ? C23 C24 1.37(2) . ? C24 C25 1.390(16) . ? O1' C7' 1.260(12) . ? O2' C9' 1.291(11) . ? O3' C15' 1.370(13) . ? O4' C17' 1.298(12) . ? O5' C19' 1.253(12) . ? C1' C2' 1.388(15) . ? C1' C6' 1.391(15) . ? C1' C7' 1.488(13) . ? C2' C3' 1.373(15) . ? C3' C4' 1.388(17) . ? C4' C5' 1.398(17) . ? C5' C6' 1.375(15) . ? C7' C8' 1.432(13) . ? C8' C9' 1.375(14) . ? C9' C10' 1.516(13) . ? C10' C11' 1.387(15) . ? C10' C15' 1.409(12) . ? C11' C12' 1.394(14) . ? C12' C13' 1.406(13) . ? C12' C16' 1.515(16) . ? C13' C14' 1.392(14) . ? C14' C15' 1.387(14) . ? C14' C17' 1.504(12) . ? C17' C18' 1.374(14) . ? C18' C19' 1.427(13) . ? C19' C20' 1.511(13) . ? C20' C21' 1.362(16) . ? C20' C25' 1.394(15) . ? C21' C22' 1.408(17) . ? C22' C23' 1.349(18) . ? C23' C24' 1.34(2) . ? C24' C25' 1.391(18) . ? O1" C7" 1.269(12) . ? O2" C9" 1.312(12) . ? O3" C15" 1.373(11) . ? O4" C17" 1.331(11) . ? O5" C19" 1.258(12) . ? C1" C2" 1.400(16) . ? C1" C6" 1.376(18) . ? C1" C7" 1.521(13) . ? C2" C3" 1.383(16) . ? C3" C4" 1.39(2) . ? C4" C5" 1.37(2) . ? C5" C6" 1.406(17) . ? C7" C8" 1.421(13) . ? C8" C9" 1.368(14) . ? C9" C10" 1.509(11) . ? C10" C11" 1.387(13) . ? C10" C15" 1.379(14) . ? C11" C12" 1.403(12) . ? C12" C13" 1.381(15) . ? C12" C16" 1.508(14) . ? C13" C14" 1.392(13) . ? C14" C15" 1.424(11) . ? C14" C17" 1.476(13) . ? C17" C18" 1.370(12) . ? C18" C19" 1.408(14) . ? C19" C20" 1.517(11) . ? C20" C21" 1.388(14) . ? C20" C25" 1.395(16) . ? C21" C22" 1.388(14) . ? C22" C23" 1.37(2) . ? C23" C24" 1.36(2) . ? C24" C25" 1.382(15) . ? 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 Co2 Co1 O1 122.2(2) . . ? Co2 Co1 O2 46.35(17) . . ? Co2 Co1 O1' 119.00(18) . . ? Co2 Co1 O2' 47.27(16) . . ? Co2 Co1 O1" 122.20(19) . . ? Co2 Co1 O2" 46.92(18) . . ? O1 Co1 O2 86.3(3) . . ? O1 Co1 O1' 100.7(3) . . ? O1 Co1 O2' 102.0(3) . . ? O1 Co1 O1" 92.0(3) . . ? O1 Co1 O2" 164.0(3) . . ? O2 Co1 O1' 164.0(3) . . ? O2 Co1 O2' 78.7(3) . . ? O2 Co1 O1" 99.9(3) . . ? O2 Co1 O2" 78.0(2) . . ? O1' Co1 O2' 85.8(3) . . ? O1' Co1 O1" 94.2(3) . . ? O1' Co1 O2" 95.3(3) . . ? O2' Co1 O1" 165.7(2) . . ? O2' Co1 O2" 78.4(2) . . ? O1" Co1 O2" 87.4(3) . . ? Co1 Co2 Co2' 179.3(7) . . ? Co1 Co2 O2 46.68(18) . . ? Co1 Co2 O3 125.78(17) . . ? Co1 Co2 O2' 47.73(17) . . ? Co1 Co2 O3' 128.72(18) . . ? Co1 Co2 O2" 47.10(16) . . ? Co1 Co2 O3" 125.66(19) . . ? Co2' Co2 O2 133.3(6) . . ? Co2' Co2 O3 54.6(6) . . ? Co2' Co2 O2' 132.9(7) . . ? Co2' Co2 O3' 51.7(7) . . ? Co2' Co2 O2" 132.3(6) . . ? Co2' Co2 O3" 53.6(7) . . ? O2 Co2 O3 83.9(2) . . ? O2 Co2 O2' 79.3(2) . . ? O2 Co2 O3' 157.5(3) . . ? O2 Co2 O2" 78.4(2) . . ? O2 Co2 O3" 111.9(3) . . ? O3 Co2 O2' 113.2(3) . . ? O3 Co2 O3' 87.1(3) . . ? O3 Co2 O2" 156.4(3) . . ? O3 Co2 O3" 88.3(3) . . ? O2' Co2 O3' 85.4(2) . . ? O2' Co2 O2" 78.9(3) . . ? O2' Co2 O3" 157.2(3) . . ? O3' Co2 O2" 114.8(3) . . ? O3' Co2 O3" 88.3(3) . . ? O2" Co2 O3" 84.0(3) . . ? Co2 Co2' Co3 179.2(13) . . ? Co2 Co2' O3 61.3(6) . . ? Co2 Co2' O4 131.9(10) . . ? Co2 Co2' O3' 62.1(6) . . ? Co2 Co2' O4' 132.3(12) . . ? Co2 Co2' O3" 61.5(6) . . ? Co2 Co2' O4" 132.8(11) . . ? Co3 Co2' O3 118.7(9) . . ? Co3 Co2' O4 48.3(4) . . ? Co3 Co2' O3' 117.2(10) . . ? Co3 Co2' O4' 47.0(4) . . ? Co3 Co2' O3" 119.2(10) . . ? Co3 Co2' O4" 47.8(4) . . ? O3 Co2' O4 71.4(7) . . ? O3 Co2' O3' 98.7(10) . . ? O3 Co2' O4' 120.2(11) . . ? O3 Co2' O3" 98.0(10) . . ? O3 Co2' O4" 140.9(13) . . ? O4 Co2' O3' 138.0(13) . . ? O4 Co2' O4' 79.1(7) . . ? O4 Co2' O3" 120.4(12) . . ? O4 Co2' O4" 80.8(7) . . ? O3' Co2' O4' 71.2(9) . . ? O3' Co2' O3" 101.1(10) . . ? O3' Co2' O4" 120.3(11) . . ? O4' Co2' O3" 141.5(11) . . ? O4' Co2' O4" 79.1(7) . . ? O3" Co2' O4" 72.8(8) . . ? Co2' Co3 O4 51.7(5) . . ? Co2' Co3 O5 122.2(5) . . ? Co2' Co3 O4' 53.2(5) . . ? Co2' Co3 O5' 122.5(5) . . ? Co2' Co3 O4" 50.0(5) . . ? Co2' Co3 O5" 123.2(5) . . ? O4 Co3 O5 87.3(2) . . ? O4 Co3 O4' 86.1(2) . . ? O4 Co3 O5' 93.7(3) . . ? O4 Co3 O4" 85.0(2) . . ? O4 Co3 O5" 170.1(3) . . ? O5 Co3 O4' 173.4(2) . . ? O5 Co3 O5' 94.9(3) . . ? O5 Co3 O4" 94.5(3) . . ? O5 Co3 O5" 90.0(3) . . ? O4' Co3 O5' 85.2(3) . . ? O4' Co3 O4" 85.3(3) . . ? O4' Co3 O5" 96.6(3) . . ? O5' Co3 O4" 170.5(3) . . ? O5' Co3 O5" 96.0(3) . . ? O4" Co3 O5" 85.8(3) . . ? Co1 O1 C7 130.1(6) . . ? Co1 O2 Co2 87.0(3) . . ? Co1 O2 C9 129.4(6) . . ? Co2 O2 C9 127.6(6) . . ? Co2 O3 Co2' 64.1(6) . . ? Co2 O3 C15 120.7(6) . . ? Co2' O3 C15 129.7(9) . . ? Co2' O4 Co3 80.1(6) . . ? Co2' O4 C17 119.1(8) . . ? Co3 O4 C17 125.8(5) . . ? Co3 O5 C19 129.1(6) . . ? C2 C1 C6 119(3) . . ? C2 C1 C7 119(2) . . ? C6 C1 C7 122(3) . . ? C1 C2 C3 121(2) . . ? C2 C3 C4 118(2) . . ? C3 C4 C5 120(2) . . ? C4 C5 C6 120(3) . . ? C1 C6 C5 120(3) . . ? C2A C1A C6A 121(3) . . ? C2A C1A C7 120(2) . . ? C6A C1A C7 119(2) . . ? C1A C2A C3A 120(2) . . ? C2A C3A C4A 121(2) . . ? C3A C4A C5A 120(2) . . ? C4A C5A C6A 117(3) . . ? C1A C6A C5A 121(3) . . ? O1 C7 C1 118.3(14) . . ? O1 C7 C1A 113.4(13) . . ? O1 C7 C8 125.3(8) . . ? C1 C7 C1A 19.2(13) . . ? C1 C7 C8 115.5(13) . . ? C1A C7 C8 120.6(14) . . ? C7 C8 C9 124.8(9) . . ? O2 C9 C8 123.4(8) . . ? O2 C9 C10 115.2(7) . . ? C8 C9 C10 121.2(8) . . ? C9 C10 C11 122.2(8) . . ? C9 C10 C15 119.7(8) . . ? C11 C10 C15 118.1(8) . . ? C10 C11 C12 122.2(8) . . ? C11 C12 C13 118.6(8) . . ? C11 C12 C16 121.3(9) . . ? C13 C12 C16 120.0(9) . . ? C12 C13 C14 122.3(8) . . ? C13 C14 C15 116.8(8) . . ? C13 C14 C17 122.5(8) . . ? C15 C14 C17 120.7(8) . . ? O3 C15 C10 120.8(8) . . ? O3 C15 C14 117.5(7) . . ? C10 C15 C14 121.7(8) . . ? O4 C17 C14 115.2(8) . . ? O4 C17 C18 124.7(8) . . ? C14 C17 C18 119.9(8) . . ? C17 C18 C19 126.1(9) . . ? O5 C19 C18 124.1(9) . . ? O5 C19 C20 116.4(8) . . ? C18 C19 C20 119.4(8) . . ? C19 C20 C21 122.0(9) . . ? C19 C20 C25 120.3(9) . . ? C21 C20 C25 117.7(10) . . ? C20 C21 C22 119.9(11) . . ? C21 C22 C23 121.0(12) . . ? C22 C23 C24 119.8(11) . . ? C23 C24 C25 120.6(12) . . ? C20 C25 C24 120.9(11) . . ? Co1 O1' C7' 128.7(6) . . ? Co1 O2' Co2 85.0(2) . . ? Co1 O2' C9' 127.9(6) . . ? Co2 O2' C9' 120.9(5) . . ? Co2 O3' Co2' 66.3(7) . . ? Co2 O3' C15' 123.7(5) . . ? Co2' O3' C15' 135.8(9) . . ? Co2' O4' Co3 79.8(6) . . ? Co2' O4' C17' 119.8(8) . . ? Co3 O4' C17' 128.4(6) . . ? Co3 O5' C19' 129.4(6) . . ? C2' C1' C6' 119.5(9) . . ? C2' C1' C7' 118.0(9) . . ? C6' C1' C7' 122.5(9) . . ? C1' C2' C3' 119.8(10) . . ? C2' C3' C4' 121.1(10) . . ? C3' C4' C5' 118.9(10) . . ? C4' C5' C6' 119.9(10) . . ? C1' C6' C5' 120.6(10) . . ? O1' C7' C1' 115.7(8) . . ? O1' C7' C8' 125.3(9) . . ? C1' C7' C8' 119.0(8) . . ? C7' C8' C9' 124.0(9) . . ? O2' C9' C8' 124.9(8) . . ? O2' C9' C10' 115.6(8) . . ? C8' C9' C10' 119.5(8) . . ? C9' C10' C11' 121.7(8) . . ? C9' C10' C15' 119.7(9) . . ? C11' C10' C15' 118.5(9) . . ? C10' C11' C12' 121.8(8) . . ? C11' C12' C13' 118.6(10) . . ? C11' C12' C16' 121.0(9) . . ? C13' C12' C16' 120.3(9) . . ? C12' C13' C14' 120.2(9) . . ? C13' C14' C15' 120.1(8) . . ? C13' C14' C17' 122.3(9) . . ? C15' C14' C17' 117.6(8) . . ? O3' C15' C10' 118.9(9) . . ? O3' C15' C14' 120.7(8) . . ? C10' C15' C14' 120.4(9) . . ? O4' C17' C14' 114.4(8) . . ? O4' C17' C18' 124.8(8) . . ? C14' C17' C18' 120.7(9) . . ? C17' C18' C19' 123.1(9) . . ? O5' C19' C18' 125.1(9) . . ? O5' C19' C20' 116.0(8) . . ? C18' C19' C20' 119.0(9) . . ? C19' C20' C21' 124.3(9) . . ? C19' C20' C25' 117.4(9) . . ? C21' C20' C25' 118.2(10) . . ? C20' C21' C22' 120.5(10) . . ? C21' C22' C23' 120.3(12) . . ? C22' C23' C24' 120.0(12) . . ? C23' C24' C25' 121.2(12) . . ? C20' C25' C24' 119.9(11) . . ? Co1 O1" C7" 129.3(6) . . ? Co1 O2" Co2 86.0(2) . . ? Co1 O2" C9" 126.4(6) . . ? Co2 O2" C9" 125.4(5) . . ? Co2 O3" Co2' 64.9(7) . . ? Co2 O3" C15" 123.8(6) . . ? Co2' O3" C15" 133.5(9) . . ? Co2' O4" Co3 82.2(6) . . ? Co2' O4" C17" 126.6(8) . . ? Co3 O4" C17" 130.3(6) . . ? Co3 O5" C19" 128.4(6) . . ? C2" C1" C6" 119.2(10) . . ? C2" C1" C7" 117.8(10) . . ? C6" C1" C7" 123.0(9) . . ? C1" C2" C3" 119.0(13) . . ? C2" C3" C4" 121.4(12) . . ? C3" C4" C5" 120.1(11) . . ? C4" C5" C6" 119.0(13) . . ? C1" C6" C5" 121.3(12) . . ? O1" C7" C1" 115.6(8) . . ? O1" C7" C8" 124.4(8) . . ? C1" C7" C8" 119.8(9) . . ? C7" C8" C9" 126.4(9) . . ? O2" C9" C8" 125.2(8) . . ? O2" C9" C10" 114.7(8) . . ? C8" C9" C10" 120.1(9) . . ? C9" C10" C11" 120.3(8) . . ? C9" C10" C15" 120.3(8) . . ? C11" C10" C15" 119.4(8) . . ? C10" C11" C12" 121.5(9) . . ? C11" C12" C13" 117.8(9) . . ? C11" C12" C16" 119.8(9) . . ? C13" C12" C16" 122.3(8) . . ? C12" C13" C14" 122.5(8) . . ? C13" C14" C15" 117.7(8) . . ? C13" C14" C17" 122.2(8) . . ? C15" C14" C17" 120.0(8) . . ? O3" C15" C10" 120.9(7) . . ? O3" C15" C14" 118.7(8) . . ? C10" C15" C14" 120.3(8) . . ? O4" C17" C14" 114.6(7) . . ? O4" C17" C18" 121.6(9) . . ? C14" C17" C18" 123.8(9) . . ? C17" C18" C19" 125.9(9) . . ? O5" C19" C18" 127.3(8) . . ? O5" C19" C20" 114.1(8) . . ? C18" C19" C20" 118.6(8) . . ? C19" C20" C21" 123.7(9) . . ? C19" C20" C25" 118.3(9) . . ? C21" C20" C25" 117.9(9) . . ? C20" C21" C22" 120.1(11) . . ? C21" C22" C23" 121.3(11) . . ? C22" C23" C24" 119.0(10) . . ? C23" C24" C25" 121.0(12) . . ? C20" C25" C24" 120.6(11) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.877 _refine_diff_density_min -1.983 _refine_diff_density_rms 0.168