# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Key Lab for Polyoxometalate Science Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_phone +86-431-5098620 _publ_contact_author_fax +86-431-5098620 _publ_author_name 'Jian-Fang Ma' #=========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 783322' #TrackingRef '- crystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H57.50 Ca0.20 Co4 N8 O19' _chemical_formula_sum 'C76 H57.50 Ca0.20 Co4 N8 O19' _chemical_formula_weight 1630.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-p 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.414(5) _cell_length_b 15.591(5) _cell_length_c 16.260(5) _cell_angle_alpha 90 _cell_angle_beta 117.953(5) _cell_angle_gamma 90 _cell_volume 3451.7(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6161 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 67.12 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1667 _exptl_absorpt_coefficient_mu 8.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25910 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 67.12 _reflns_number_total 6161 _reflns_number_gt 4168 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^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 6161 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 C1 C 0.9407(4) 0.0963(4) 0.5717(5) 0.0587(19) Uani 1 1 d . . . H1 H 0.9229 0.1533 0.5563 0.070 Uiso 1 1 calc R . . C2 C 1.0336(4) 0.0657(5) 0.6144(5) 0.067(2) Uani 1 1 d . . . H2 H 1.0906 0.0977 0.6323 0.080 Uiso 1 1 calc R . . C3 C 0.9335(4) -0.0377(4) 0.5884(4) 0.0384(12) Uani 1 1 d . . . H3 H 0.9093 -0.0929 0.5858 0.046 Uiso 1 1 calc R . . C4 C 1.1099(4) -0.0777(4) 0.6750(4) 0.0514(16) Uani 1 1 d . . . H4A H 1.1667 -0.0577 0.6697 0.062 Uiso 1 1 calc R . . H4B H 1.0922 -0.1340 0.6466 0.062 Uiso 1 1 calc R . . C5 C 1.1352(4) -0.0838(4) 0.7764(4) 0.0405(13) Uani 1 1 d . . . C6 C 1.0891(4) -0.1437(4) 0.8056(5) 0.0535(16) Uani 1 1 d . . . H6 H 1.0440 -0.1818 0.7629 0.064 Uiso 1 1 calc R . . C7 C 1.1099(5) -0.1469(4) 0.8971(5) 0.0586(17) Uani 1 1 d . . . H7 H 1.0780 -0.1869 0.9158 0.070 Uiso 1 1 calc R . . C8 C 1.1774(5) -0.0920(4) 0.9620(4) 0.0541(16) Uani 1 1 d . . . H8 H 1.1910 -0.0953 1.0241 0.065 Uiso 1 1 calc R . . C9 C 1.2244(4) -0.0324(4) 0.9345(4) 0.0494(15) Uani 1 1 d . . . C10 C 1.2028(4) -0.0298(4) 0.8411(4) 0.0438(13) Uani 1 1 d . . . H10 H 1.2351 0.0097 0.8223 0.053 Uiso 1 1 calc R . . C11 C 1.2986(6) 0.0325(5) 0.9999(4) 0.069(2) Uani 1 1 d . . . H11A H 1.3576 0.0293 0.9928 0.083 Uiso 1 1 calc R . . H11B H 1.2715 0.0897 0.9817 0.083 Uiso 1 1 calc R . . C12 C 1.4008(4) -0.0256(4) 1.1616(4) 0.0461(14) Uani 1 1 d . . . H12 H 1.4479 -0.0528 1.1503 0.055 Uiso 1 1 calc R . . C13 C 1.3195(5) 0.0201(4) 1.2295(4) 0.0498(15) Uani 1 1 d . . . H13 H 1.3002 0.0305 1.2749 0.060 Uiso 1 1 calc R . . C14 C 1.2730(5) 0.0484(5) 1.1411(5) 0.0626(19) Uani 1 1 d . . . H14 H 1.2161 0.0814 1.1145 0.075 Uiso 1 1 calc R . . C15 C 0.6782(3) 0.1331(3) 0.6227(3) 0.0277(10) Uani 1 1 d . . . C16 C 0.7195(3) 0.1855(3) 0.7101(3) 0.0285(10) Uani 1 1 d . . . C17 C 0.6608(4) 0.2463(3) 0.7206(3) 0.0358(12) Uani 1 1 d . . . H17 H 0.5946 0.2491 0.6773 0.043 Uiso 1 1 calc R . . C18 C 0.6989(4) 0.3037(3) 0.7949(4) 0.0365(12) Uani 1 1 d . . . H18 H 0.6575 0.3446 0.7994 0.044 Uiso 1 1 calc R . . C19 C 0.7950(3) 0.3017(3) 0.8613(3) 0.0254(10) Uani 1 1 d . . . C20 C 0.8588(3) 0.2381(3) 0.8563(3) 0.0295(10) Uani 1 1 d . . . C21 C 0.8201(4) 0.1783(3) 0.7797(3) 0.0301(11) Uani 1 1 d . . . C22 C 0.8824(4) 0.1138(4) 0.7753(4) 0.0494(15) Uani 1 1 d . . . H22 H 0.8573 0.0744 0.7267 0.059 Uiso 1 1 calc R . . C23 C 0.9785(5) 0.1081(5) 0.8410(5) 0.067(2) Uani 1 1 d . . . H23 H 1.0179 0.0639 0.8388 0.081 Uiso 1 1 calc R . . C24 C 1.0169(5) 0.1698(5) 0.9116(5) 0.073(2) Uani 1 1 d . . . H24 H 1.0836 0.1690 0.9535 0.088 Uiso 1 1 calc R . . C25 C 0.9589(4) 0.2313(4) 0.9203(4) 0.0431(14) Uani 1 1 d . . . H25 H 0.9862 0.2696 0.9699 0.052 Uiso 1 1 calc R . . C26 C 0.8282(3) 0.3697(3) 0.9375(3) 0.0310(11) Uani 1 1 d . . . C27 C 0.3255(3) 0.1192(3) 0.6604(3) 0.0266(10) Uani 1 1 d . . . C28 C 0.2776(3) 0.1804(3) 0.6984(3) 0.0242(9) Uani 1 1 d . . . C29 C 0.3114(4) 0.1815(3) 0.7920(3) 0.0315(11) Uani 1 1 d . . . H29 H 0.3638 0.1463 0.8297 0.038 Uiso 1 1 calc R . . C30 C 0.2691(4) 0.2347(3) 0.8331(3) 0.0315(11) Uani 1 1 d . . . H30 H 0.2947 0.2353 0.8975 0.038 Uiso 1 1 calc R . . C31 C 0.1901(3) 0.2861(3) 0.7790(3) 0.0287(10) Uani 1 1 d . . . C32 C 0.1547(4) 0.3460(3) 0.8301(3) 0.0292(11) Uani 1 1 d . . . C33 C 0.1519(3) 0.2857(3) 0.6804(3) 0.0280(10) Uani 1 1 d . . . C34 C 0.0719(4) 0.3400(4) 0.6205(4) 0.0439(14) Uani 1 1 d . . . H34 H 0.0422 0.3756 0.6458 0.053 Uiso 1 1 calc R . . C35 C 0.0398(5) 0.3399(4) 0.5284(4) 0.0582(18) Uani 1 1 d . . . H35 H -0.0141 0.3737 0.4907 0.070 Uiso 1 1 calc R . . C36 C 0.0856(4) 0.2897(4) 0.4865(4) 0.0512(15) Uani 1 1 d . . . H36 H 0.0639 0.2920 0.4226 0.061 Uiso 1 1 calc R . . C37 C 0.1624(4) 0.2383(3) 0.5426(3) 0.0364(12) Uani 1 1 d . . . H37 H 0.1930 0.2054 0.5160 0.044 Uiso 1 1 calc R . . C38 C 0.1967(3) 0.2333(3) 0.6392(3) 0.0256(10) Uani 1 1 d . . . O1 O 0.5913(2) 0.1034(2) 0.5894(2) 0.0317(8) Uani 1 1 d . . . O2 O 0.7297(2) 0.1239(2) 0.5832(2) 0.0347(8) Uani 1 1 d . . . O9 O 0.4378(2) -0.0386(2) 0.5794(2) 0.0262(7) Uani 1 1 d . . . O3 O 0.4174(2) 0.1209(2) 0.6970(2) 0.0368(8) Uani 1 1 d . . . O1W O 0.8407(9) 0.2800(5) 0.5906(8) 0.078(3) Uani 0.50 1 d P . . O4 O 0.2704(3) 0.0696(2) 0.5977(2) 0.0391(9) Uani 1 1 d . . . O5 O 0.2220(2) 0.3783(2) 0.9017(2) 0.0372(8) Uani 1 1 d . . . O6 O 0.0655(3) 0.3580(3) 0.8018(3) 0.0477(10) Uani 1 1 d . . . O7 O 0.9006(3) 0.3517(2) 1.0168(3) 0.0420(9) Uani 1 1 d . . . O8 O 0.7779(3) 0.4349(2) 0.9207(2) 0.0385(9) Uani 1 1 d . . . Co1 Co 0.49339(5) 0.07830(5) 0.63431(5) 0.0299(2) Uani 1 1 d . . . Co2 Co 0.72478(5) 0.02767(4) 0.48985(5) 0.01857(18) Uani 1 1 d . . . N1 N 0.8778(3) 0.0299(3) 0.5551(3) 0.0282(9) Uani 1 1 d . . . N2 N 1.0288(3) -0.0190(3) 0.6264(3) 0.0358(10) Uani 1 1 d . . . N3 N 1.3252(4) 0.0196(3) 1.0974(3) 0.0485(12) Uani 1 1 d . . . N4 N 1.4002(3) -0.0267(3) 1.2417(3) 0.0368(10) Uani 1 1 d . . . Ca1 Ca 0.5000 0.0000 0.5000 0.0430(18) Uani 0.20 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(3) 0.032(3) 0.082(5) 0.019(3) 0.012(3) -0.006(3) C2 0.031(3) 0.077(5) 0.078(5) 0.024(4) 0.013(3) -0.015(3) C3 0.024(3) 0.036(3) 0.046(3) -0.005(2) 0.009(2) 0.001(2) C4 0.031(3) 0.072(4) 0.043(3) -0.006(3) 0.010(3) 0.019(3) C5 0.026(2) 0.046(3) 0.043(3) 0.003(3) 0.011(2) 0.011(2) C6 0.036(3) 0.053(4) 0.059(4) -0.006(3) 0.013(3) -0.003(3) C7 0.048(4) 0.058(4) 0.063(4) 0.011(3) 0.020(3) -0.008(3) C8 0.054(4) 0.056(4) 0.044(4) 0.013(3) 0.016(3) -0.010(3) C9 0.048(3) 0.054(4) 0.033(3) 0.007(3) 0.007(3) -0.007(3) C10 0.043(3) 0.049(3) 0.035(3) 0.007(3) 0.015(3) -0.003(3) C11 0.078(5) 0.081(5) 0.032(3) 0.012(3) 0.014(3) -0.028(4) C12 0.045(3) 0.053(4) 0.040(3) 0.000(3) 0.019(3) -0.007(3) C13 0.058(4) 0.053(4) 0.040(3) 0.005(3) 0.024(3) 0.013(3) C14 0.059(4) 0.070(5) 0.056(4) 0.019(3) 0.024(3) 0.026(3) C15 0.030(2) 0.024(2) 0.029(3) -0.005(2) 0.013(2) 0.003(2) C16 0.034(3) 0.027(2) 0.030(3) -0.007(2) 0.019(2) 0.001(2) C17 0.027(3) 0.041(3) 0.035(3) -0.014(2) 0.011(2) 0.004(2) C18 0.035(3) 0.038(3) 0.040(3) -0.016(2) 0.020(2) 0.006(2) C19 0.029(2) 0.024(2) 0.026(2) -0.0061(19) 0.015(2) -0.0038(19) C20 0.032(2) 0.031(3) 0.027(3) -0.005(2) 0.016(2) 0.002(2) C21 0.034(3) 0.027(3) 0.028(3) -0.006(2) 0.014(2) 0.006(2) C22 0.052(3) 0.047(3) 0.038(3) -0.018(3) 0.012(3) 0.018(3) C23 0.047(3) 0.080(5) 0.055(4) -0.019(4) 0.008(3) 0.038(3) C24 0.038(3) 0.099(6) 0.057(4) -0.032(4) 0.001(3) 0.028(4) C25 0.035(3) 0.048(3) 0.036(3) -0.015(3) 0.008(2) 0.007(2) C26 0.028(2) 0.029(3) 0.037(3) -0.014(2) 0.017(2) -0.005(2) C27 0.034(3) 0.026(2) 0.026(2) -0.003(2) 0.019(2) 0.003(2) C28 0.026(2) 0.025(2) 0.025(2) -0.0045(19) 0.0141(19) -0.0009(19) C29 0.036(3) 0.028(3) 0.029(3) -0.003(2) 0.014(2) 0.007(2) C30 0.040(3) 0.034(3) 0.021(2) -0.003(2) 0.014(2) 0.004(2) C31 0.033(2) 0.027(2) 0.032(3) -0.009(2) 0.020(2) -0.004(2) C32 0.037(3) 0.027(2) 0.032(3) -0.010(2) 0.022(2) -0.001(2) C33 0.026(2) 0.031(3) 0.029(3) -0.009(2) 0.014(2) -0.001(2) C34 0.041(3) 0.051(3) 0.036(3) -0.009(3) 0.015(3) 0.014(3) C35 0.056(4) 0.071(4) 0.035(3) -0.002(3) 0.011(3) 0.031(3) C36 0.058(4) 0.059(4) 0.033(3) -0.002(3) 0.018(3) 0.012(3) C37 0.044(3) 0.039(3) 0.028(3) -0.004(2) 0.019(2) 0.006(2) C38 0.026(2) 0.025(2) 0.028(2) -0.0079(19) 0.014(2) -0.0012(19) O1 0.0306(18) 0.0358(19) 0.0314(18) -0.0106(15) 0.0167(15) -0.0027(15) O2 0.0374(19) 0.039(2) 0.036(2) -0.0128(16) 0.0247(17) -0.0043(16) O9 0.0268(16) 0.0284(17) 0.0234(16) 0.0035(13) 0.0117(14) -0.0026(13) O3 0.0305(18) 0.048(2) 0.034(2) -0.0066(16) 0.0165(16) 0.0085(16) O1W 0.140(9) 0.019(4) 0.135(9) 0.010(5) 0.112(8) 0.005(5) O4 0.041(2) 0.039(2) 0.041(2) -0.0217(17) 0.0220(17) -0.0041(16) O5 0.0363(19) 0.039(2) 0.035(2) -0.0196(16) 0.0158(16) -0.0002(16) O6 0.033(2) 0.062(3) 0.049(2) -0.027(2) 0.0202(18) 0.0009(18) O7 0.0366(19) 0.043(2) 0.038(2) -0.0122(17) 0.0107(17) 0.0030(16) O8 0.049(2) 0.0317(19) 0.032(2) -0.0090(15) 0.0167(17) 0.0089(16) Co1 0.0307(4) 0.0321(4) 0.0294(4) -0.0009(3) 0.0163(3) 0.0003(3) Co2 0.0231(4) 0.0171(3) 0.0179(3) 0.0012(3) 0.0117(3) 0.0009(3) N1 0.027(2) 0.028(2) 0.030(2) -0.0022(17) 0.0146(17) -0.0033(17) N2 0.024(2) 0.048(3) 0.035(2) 0.002(2) 0.0132(18) 0.0058(19) N3 0.053(3) 0.056(3) 0.025(2) 0.005(2) 0.008(2) -0.001(2) N4 0.036(2) 0.043(3) 0.030(2) -0.001(2) 0.0149(19) 0.001(2) Ca1 0.046(4) 0.050(5) 0.040(4) 0.002(4) 0.026(4) 0.007(4) _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 C1 C2 1.351(9) . ? C1 N1 1.356(7) . ? C1 H1 0.9300 . ? C2 N2 1.343(8) . ? C2 H2 0.9300 . ? C3 N1 1.307(6) . ? C3 N2 1.331(6) . ? C3 H3 0.9300 . ? C4 N2 1.448(7) . ? C4 C5 1.509(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.369(8) . ? C5 C6 1.385(8) . ? C6 C7 1.367(9) . ? C6 H6 0.9300 . ? C7 C8 1.378(9) . ? C7 H7 0.9300 . ? C8 C9 1.376(8) . ? C8 H8 0.9300 . ? C9 C10 1.395(8) . ? C9 C11 1.524(9) . ? C10 H10 0.9300 . ? C11 N3 1.453(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.307(7) . ? C12 N3 1.343(8) . ? C12 H12 0.9300 . ? C13 C14 1.344(9) . ? C13 N4 1.375(7) . ? C13 H13 0.9300 . ? C14 N3 1.375(8) . ? C14 H14 0.9300 . ? C15 O2 1.242(5) . ? C15 O1 1.273(5) . ? C15 C16 1.499(6) . ? C16 C17 1.374(6) . ? C16 C21 1.433(7) . ? C17 C18 1.393(7) . ? C17 H17 0.9300 . ? C18 C19 1.365(7) . ? C18 H18 0.9300 . ? C19 C20 1.425(6) . ? C19 C26 1.526(6) . ? C20 C25 1.403(7) . ? C20 C21 1.443(6) . ? C21 C22 1.415(7) . ? C22 C23 1.364(8) . ? C22 H22 0.9300 . ? C23 C24 1.400(9) . ? C23 H23 0.9300 . ? C24 C25 1.364(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 O8 1.229(6) . ? C26 O7 1.279(6) . ? C26 Ca1 3.107(5) 2_656 ? C27 O4 1.244(6) . ? C27 O3 1.254(6) . ? C27 C28 1.503(6) . ? C28 C29 1.359(6) . ? C28 C38 1.427(6) . ? C29 C30 1.404(6) . ? C29 H29 0.9300 . ? C30 C31 1.376(7) . ? C30 H30 0.9300 . ? C31 C33 1.425(7) . ? C31 C32 1.512(6) . ? C32 O6 1.243(6) . ? C32 O5 1.246(6) . ? C33 C38 1.424(6) . ? C33 C34 1.436(7) . ? C34 C35 1.338(8) . ? C34 H34 0.9300 . ? C35 C36 1.424(8) . ? C35 H35 0.9300 . ? C36 C37 1.366(8) . ? C36 H36 0.9300 . ? C37 C38 1.405(6) . ? C37 H37 0.9300 . ? O1 Co1 1.999(3) . ? O1 Ca1 2.186(3) . ? O2 Co2 2.110(3) . ? O9 Ca1 2.026(3) . ? O9 Co1 2.033(3) . ? O9 Co2 2.221(3) 3_656 ? O3 Co1 1.993(3) . ? O4 Co2 2.105(3) 3_656 ? O5 Co2 2.037(3) 4_566 ? O7 Co1 2.080(4) 4_666 ? O7 Ca1 2.857(4) 2_656 ? O8 Co2 2.065(3) 2_656 ? Co1 N4 2.074(4) 3_757 ? Co1 O7 2.080(4) 4_565 ? Co2 O5 2.037(3) 4_665 ? Co2 O8 2.065(3) 2_646 ? Co2 N1 2.084(4) . ? Co2 O4 2.105(3) 3_656 ? Co2 O9 2.221(3) 3_656 ? N4 Co1 2.074(4) 3_757 ? Ca1 O9 2.026(3) 3_656 ? Ca1 O1 2.186(3) 3_656 ? Ca1 O7 2.857(4) 4_565 ? Ca1 O7 2.857(4) 2_646 ? 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 C2 C1 N1 108.6(5) . . ? C2 C1 H1 125.7 . . ? N1 C1 H1 125.7 . . ? N2 C2 C1 107.7(5) . . ? N2 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? N1 C3 N2 112.5(5) . . ? N1 C3 H3 123.7 . . ? N2 C3 H3 123.7 . . ? N2 C4 C5 110.6(4) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C10 C5 C6 118.7(6) . . ? C10 C5 C4 121.0(5) . . ? C6 C5 C4 120.3(5) . . ? C7 C6 C5 120.0(6) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 121.3(6) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.6(6) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.7(6) . . ? C8 C9 C11 124.0(6) . . ? C10 C9 C11 117.3(5) . . ? C5 C10 C9 121.7(5) . . ? C5 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N3 C11 C9 113.9(5) . . ? N3 C11 H11A 108.8 . . ? C9 C11 H11A 108.8 . . ? N3 C11 H11B 108.8 . . ? C9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N4 C12 N3 111.9(5) . . ? N4 C12 H12 124.0 . . ? N3 C12 H12 124.0 . . ? C14 C13 N4 108.7(5) . . ? C14 C13 H13 125.6 . . ? N4 C13 H13 125.6 . . ? C13 C14 N3 107.3(5) . . ? C13 C14 H14 126.3 . . ? N3 C14 H14 126.3 . . ? O2 C15 O1 122.6(4) . . ? O2 C15 C16 117.6(4) . . ? O1 C15 C16 119.7(4) . . ? C17 C16 C21 119.2(4) . . ? C17 C16 C15 118.8(4) . . ? C21 C16 C15 121.8(4) . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 122.1(4) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 119.5(4) . . ? C18 C19 C26 116.9(4) . . ? C20 C19 C26 123.5(4) . . ? C25 C20 C19 123.9(4) . . ? C25 C20 C21 117.2(4) . . ? C19 C20 C21 118.8(4) . . ? C22 C21 C16 121.7(4) . . ? C22 C21 C20 119.1(4) . . ? C16 C21 C20 119.2(4) . . ? C23 C22 C21 121.4(5) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 118.9(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 121.6(6) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C20 121.5(5) . . ? C24 C25 H25 119.2 . . ? C20 C25 H25 119.2 . . ? O8 C26 O7 124.6(4) . . ? O8 C26 C19 117.2(4) . . ? O7 C26 C19 117.8(4) . . ? O8 C26 Ca1 83.3(3) . 2_656 ? O7 C26 Ca1 66.8(3) . 2_656 ? C19 C26 Ca1 129.0(3) . 2_656 ? O4 C27 O3 126.0(4) . . ? O4 C27 C28 116.9(4) . . ? O3 C27 C28 117.0(4) . . ? C29 C28 C38 120.2(4) . . ? C29 C28 C27 117.7(4) . . ? C38 C28 C27 122.1(4) . . ? C28 C29 C30 121.5(4) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C31 C30 C29 120.6(4) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C33 119.4(4) . . ? C30 C31 C32 116.6(4) . . ? C33 C31 C32 123.7(4) . . ? O6 C32 O5 125.3(4) . . ? O6 C32 C31 120.7(4) . . ? O5 C32 C31 113.9(4) . . ? C38 C33 C31 119.8(4) . . ? C38 C33 C34 118.1(4) . . ? C31 C33 C34 122.1(4) . . ? C35 C34 C33 120.6(5) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 122.0(5) . . ? C34 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C37 C36 C35 118.1(5) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C36 C37 C38 122.3(5) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C37 C38 C33 118.9(4) . . ? C37 C38 C28 122.5(4) . . ? C33 C38 C28 118.5(4) . . ? C15 O1 Co1 137.7(3) . . ? C15 O1 Ca1 140.5(3) . . ? Co1 O1 Ca1 74.77(11) . . ? C15 O2 Co2 129.6(3) . . ? Ca1 O9 Co1 77.65(11) . . ? Ca1 O9 Co2 114.39(14) . 3_656 ? Co1 O9 Co2 107.29(14) . 3_656 ? C27 O3 Co1 123.7(3) . . ? C27 O4 Co2 140.8(3) . 3_656 ? C32 O5 Co2 133.0(3) . 4_566 ? C26 O7 Co1 135.2(3) . 4_666 ? C26 O7 Ca1 88.9(3) . 2_656 ? Co1 O7 Ca1 59.63(10) 4_666 2_656 ? C26 O8 Co2 129.8(3) . 2_656 ? O3 Co1 O1 147.86(15) . . ? O3 Co1 O9 107.20(14) . . ? O1 Co1 O9 104.47(13) . . ? O3 Co1 N4 91.06(16) . 3_757 ? O1 Co1 N4 92.45(16) . 3_757 ? O9 Co1 N4 93.32(15) . 3_757 ? O3 Co1 O7 88.82(15) . 4_565 ? O1 Co1 O7 82.71(14) . 4_565 ? O9 Co1 O7 95.73(14) . 4_565 ? N4 Co1 O7 170.56(16) 3_757 4_565 ? O3 Co1 Ca1 150.25(10) . . ? O1 Co1 Ca1 55.95(9) . . ? O9 Co1 Ca1 51.05(8) . . ? N4 Co1 Ca1 108.46(12) 3_757 . ? O7 Co1 Ca1 75.53(12) 4_565 . ? O5 Co2 O8 177.38(15) 4_665 2_646 ? O5 Co2 N1 89.53(15) 4_665 . ? O8 Co2 N1 92.54(15) 2_646 . ? O5 Co2 O4 92.18(16) 4_665 3_656 ? O8 Co2 O4 89.50(16) 2_646 3_656 ? N1 Co2 O4 88.06(15) . 3_656 ? O5 Co2 O2 88.62(15) 4_665 . ? O8 Co2 O2 89.83(15) 2_646 . ? N1 Co2 O2 88.34(14) . . ? O4 Co2 O2 176.31(14) 3_656 . ? O5 Co2 O9 86.67(12) 4_665 3_656 ? O8 Co2 O9 91.16(13) 2_646 3_656 ? N1 Co2 O9 174.65(14) . 3_656 ? O4 Co2 O9 95.83(13) 3_656 3_656 ? O2 Co2 O9 87.82(12) . 3_656 ? O5 Co2 Ca1 114.75(10) 4_665 . ? O8 Co2 Ca1 62.80(10) 2_646 . ? N1 Co2 Ca1 150.38(11) . . ? O4 Co2 Ca1 106.68(10) 3_656 . ? O2 Co2 Ca1 76.20(9) . . ? O9 Co2 Ca1 31.11(8) 3_656 . ? C3 N1 C1 105.3(4) . . ? C3 N1 Co2 124.4(3) . . ? C1 N1 Co2 130.3(4) . . ? C3 N2 C2 105.8(5) . . ? C3 N2 C4 126.7(5) . . ? C2 N2 C4 127.5(5) . . ? C12 N3 C14 105.9(5) . . ? C12 N3 C11 128.2(6) . . ? C14 N3 C11 125.8(6) . . ? C12 N4 C13 106.1(5) . . ? C12 N4 Co1 127.1(4) . 3_757 ? C13 N4 Co1 126.6(4) . 3_757 ? O9 Ca1 O9 180.0 . 3_656 ? O9 Ca1 O1 98.32(12) . . ? O9 Ca1 O1 81.68(12) 3_656 . ? O9 Ca1 O1 81.68(12) . 3_656 ? O9 Ca1 O1 98.32(12) 3_656 3_656 ? O1 Ca1 O1 180.00(12) . 3_656 ? O9 Ca1 Co1 51.30(9) . . ? O9 Ca1 Co1 128.70(9) 3_656 . ? O1 Ca1 Co1 49.28(8) . . ? O1 Ca1 Co1 130.72(8) 3_656 . ? O9 Ca1 Co1 128.70(9) . 3_656 ? O9 Ca1 Co1 51.30(9) 3_656 3_656 ? O1 Ca1 Co1 130.72(8) . 3_656 ? O1 Ca1 Co1 49.28(8) 3_656 3_656 ? Co1 Ca1 Co1 180.0 . 3_656 ? O9 Ca1 O7 75.19(12) . 4_565 ? O9 Ca1 O7 104.81(12) 3_656 4_565 ? O1 Ca1 O7 63.01(11) . 4_565 ? O1 Ca1 O7 116.99(11) 3_656 4_565 ? Co1 Ca1 O7 44.84(7) . 4_565 ? Co1 Ca1 O7 135.16(7) 3_656 4_565 ? O9 Ca1 O7 104.81(12) . 2_646 ? O9 Ca1 O7 75.19(12) 3_656 2_646 ? O1 Ca1 O7 116.99(11) . 2_646 ? O1 Ca1 O7 63.01(11) 3_656 2_646 ? Co1 Ca1 O7 135.16(7) . 2_646 ? Co1 Ca1 O7 44.84(7) 3_656 2_646 ? O7 Ca1 O7 180.0 4_565 2_646 ? O9 Ca1 C26 79.44(12) . 4_565 ? O9 Ca1 C26 100.56(12) 3_656 4_565 ? O1 Ca1 C26 85.38(13) . 4_565 ? O1 Ca1 C26 94.62(13) 3_656 4_565 ? Co1 Ca1 C26 66.17(10) . 4_565 ? Co1 Ca1 C26 113.83(10) 3_656 4_565 ? O7 Ca1 C26 24.32(12) 4_565 4_565 ? O7 Ca1 C26 155.68(12) 2_646 4_565 ? O9 Ca1 C26 100.56(12) . 2_646 ? O9 Ca1 C26 79.44(12) 3_656 2_646 ? O1 Ca1 C26 94.62(13) . 2_646 ? O1 Ca1 C26 85.38(13) 3_656 2_646 ? Co1 Ca1 C26 113.83(10) . 2_646 ? Co1 Ca1 C26 66.17(10) 3_656 2_646 ? O7 Ca1 C26 155.68(12) 4_565 2_646 ? O7 Ca1 C26 24.32(12) 2_646 2_646 ? C26 Ca1 C26 180.0 4_565 2_646 ? O9 Ca1 Co2 34.49(9) . 3_656 ? O9 Ca1 Co2 145.51(9) 3_656 3_656 ? O1 Ca1 Co2 113.24(8) . 3_656 ? O1 Ca1 Co2 66.76(8) 3_656 3_656 ? Co1 Ca1 Co2 65.69(2) . 3_656 ? Co1 Ca1 Co2 114.31(2) 3_656 3_656 ? O7 Ca1 Co2 61.19(7) 4_565 3_656 ? O7 Ca1 Co2 118.81(7) 2_646 3_656 ? C26 Ca1 Co2 52.92(9) 4_565 3_656 ? C26 Ca1 Co2 127.08(9) 2_646 3_656 ? O9 Ca1 Co2 145.51(9) . . ? O9 Ca1 Co2 34.49(9) 3_656 . ? O1 Ca1 Co2 66.76(8) . . ? O1 Ca1 Co2 113.24(8) 3_656 . ? Co1 Ca1 Co2 114.31(2) . . ? Co1 Ca1 Co2 65.69(2) 3_656 . ? O7 Ca1 Co2 118.81(7) 4_565 . ? O7 Ca1 Co2 61.19(7) 2_646 . ? C26 Ca1 Co2 127.08(9) 4_565 . ? C26 Ca1 Co2 52.92(9) 2_646 . ? Co2 Ca1 Co2 180.0 3_656 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 67.12 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.084 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.092