# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Raphael Raptis' _publ_contact_author_email RAPHAEL@EPSCOR.UPR.EDU _publ_section_title ; Tri-, deca- and dodecanuclear Co(III)-pyrazolate metallacycles ; loop_ _publ_author_name 'Raphael Raptis' 'Indranil Chakraborty' 'Haralampos N. Miras' # Attachment 'Co3__1_.cif' data_co3 _database_code_depnum_ccdc_archive 'CCDC 750242' #TrackingRef 'Co3__1_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H27 Co3 N23 O21 P4' _chemical_formula_weight 2235.16 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 33.330(7) _cell_length_b 16.335(3) _cell_length_c 19.603(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.20(3) _cell_angle_gamma 90.00 _cell_volume 10079(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3355 _cell_measurement_theta_min 4.524 _cell_measurement_theta_max 51.331 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4484 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.9392 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Kappa CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean 15.9832 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36062 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 26.71 _reflns_number_total 10796 _reflns_number_gt 6495 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v. 3.2' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1132P)^2^+39.8021P] 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 none _refine_ls_number_reflns 10796 _refine_ls_number_parameters 673 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1338 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2294 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.911 _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 0.54078(6) 0.5000 0.18834(10) 0.0147(5) Uani 1 2 d S . . Co2 Co 0.60683(4) 0.59487(8) 0.31173(7) 0.0172(4) Uani 1 1 d . . . P1 P 0.32046(11) 0.0000 0.98766(19) 0.0174(8) Uani 1 2 d S . . P2 P 0.23802(11) 0.0000 0.8574(2) 0.0179(8) Uani 1 2 d S . . P3 P 0.49742(11) 0.0000 1.2672(2) 0.0197(8) Uani 1 2 d S . . P4 P 0.58035(11) 0.0000 1.3952(2) 0.0228(9) Uani 1 2 d S . . O1 O 0.5851(3) 0.5000 0.2703(5) 0.017(2) Uani 1 2 d S . . O2 O 0.5967(3) 0.7117(5) -0.0040(4) 0.042(2) Uani 1 1 d . . . O3 O 0.6477(3) 0.7662(5) 0.0839(4) 0.040(2) Uani 1 1 d . . . O4 O 0.4133(2) 0.6918(5) 0.2598(4) 0.0323(19) Uani 1 1 d . . . O5 O 0.4588(2) 0.7538(6) 0.3508(4) 0.044(2) Uani 1 1 d . . . O6 O 0.7889(2) 0.5666(5) 0.3674(4) 0.036(2) Uani 1 1 d . . . O7 O 0.6112(3) 0.5663(5) 0.6106(4) 0.037(2) Uani 1 1 d . . . O8 O 0.6598(2) 0.7300(4) 0.3383(4) 0.0267(17) Uani 1 1 d . . . O9 O 0.6147(2) 0.7328(5) 0.3954(4) 0.0298(18) Uani 1 1 d . . . O10 O 0.4783(2) 0.4343(4) 0.0720(4) 0.0259(17) Uani 1 1 d . . . N1 N 0.5716(2) 0.5856(5) 0.1594(4) 0.0149(17) Uani 1 1 d . . . N2 N 0.6016(2) 0.6270(5) 0.2143(4) 0.0165(17) Uani 1 1 d . . . N3 N 0.5188(2) 0.5838(5) 0.2354(4) 0.0157(17) Uani 1 1 d . . . N4 N 0.5478(2) 0.6258(5) 0.2909(4) 0.0203(19) Uani 1 1 d . . . N5 N 0.6611(2) 0.5427(5) 0.3264(4) 0.0178(18) Uani 1 1 d . . . N6 N 0.6084(2) 0.5425(5) 0.4008(4) 0.0202(19) Uani 1 1 d . . . N7 N 0.6169(3) 0.7202(5) 0.0608(5) 0.028(2) Uani 1 1 d . . . N8 N 0.4499(3) 0.7052(6) 0.3000(5) 0.026(2) Uani 1 1 d . . . N9 N 0.7705(4) 0.5000 0.3614(7) 0.027(3) Uani 1 2 d S . . N10 N 0.6111(4) 0.5000 0.5806(7) 0.029(3) Uani 1 2 d S . . N11 N 0.6299(3) 0.6976(5) 0.3535(5) 0.024(2) Uani 1 1 d . . . N12 N 0.4937(3) 0.5000 0.1004(6) 0.017(2) Uani 1 2 d S . . N13 N 0.2821(4) 0.0000 0.9168(7) 0.052(5) Uani 1 2 d S A . N14 N 0.5342(4) 0.0000 1.3403(7) 0.037(4) Uani 1 2 d S B . C1 C 0.5727(3) 0.6143(5) 0.0966(5) 0.014(2) Uani 1 1 d . . . H1 H 0.5557 0.5973 0.0510 0.017 Uiso 1 1 calc R . . C2 C 0.6041(3) 0.6747(6) 0.1118(5) 0.017(2) Uani 1 1 d . . . C3 C 0.6212(3) 0.6798(5) 0.1856(5) 0.015(2) Uani 1 1 d . . . H3 H 0.6430 0.7147 0.2111 0.018 Uiso 1 1 calc R . . C4 C 0.4799(3) 0.6072(6) 0.2316(5) 0.017(2) Uani 1 1 d . . . H4 H 0.4547 0.5886 0.1983 0.021 Uiso 1 1 calc R . . C5 C 0.4835(3) 0.6640(6) 0.2858(5) 0.020(2) Uani 1 1 d . . . C6 C 0.5266(3) 0.6740(7) 0.3214(5) 0.023(2) Uani 1 1 d . . . H6 H 0.5387 0.7088 0.3603 0.028 Uiso 1 1 calc R . . C7 C 0.7005(3) 0.5685(6) 0.3392(5) 0.018(2) Uani 1 1 d . . . H7 H 0.7094 0.6228 0.3423 0.022 Uiso 1 1 calc R . . C8 C 0.7261(4) 0.5000 0.3471(7) 0.020(3) Uani 1 2 d S . . C9 C 0.6099(3) 0.5680(7) 0.4658(5) 0.023(2) Uani 1 1 d . . . H9 H 0.6105 0.6223 0.4805 0.028 Uiso 1 1 calc R . . C10 C 0.6106(4) 0.5000 0.5080(8) 0.023(3) Uani 1 2 d S . . C21 C 0.2279(4) 0.0957(7) 0.8004(7) 0.011(5) Uiso 0.50 1 d PGD A 1 C22 C 0.2620(3) 0.1461(8) 0.8031(7) 0.016(4) Uiso 0.50 1 d PGD A 1 C23 C 0.2552(3) 0.2179(7) 0.7629(8) 0.021(5) Uiso 0.50 1 d PGD A 1 C24 C 0.2144(4) 0.2393(6) 0.7198(7) 0.025(5) Uiso 0.50 1 d PGD A 1 C25 C 0.1803(3) 0.1889(8) 0.7171(7) 0.021(4) Uiso 0.50 1 d PGD A 1 C26 C 0.1870(3) 0.1171(7) 0.7573(7) 0.018(4) Uiso 0.50 1 d PGD A 1 C21' C 0.2369(5) 0.0845(7) 0.8038(7) 0.020(5) Uiso 0.50 1 d PGD A 2 C22' C 0.2653(4) 0.1478(8) 0.8325(6) 0.017(4) Uiso 0.50 1 d PGD A 2 C23' C 0.2641(4) 0.2184(7) 0.7923(7) 0.021(5) Uiso 0.50 1 d PGD A 2 C24' C 0.2346(4) 0.2256(7) 0.7234(7) 0.022(4) Uiso 0.50 1 d PGD A 2 C25' C 0.2062(4) 0.1623(8) 0.6947(6) 0.029(5) Uiso 0.50 1 d PGD A 2 C26' C 0.2074(4) 0.0917(7) 0.7349(7) 0.028(5) Uiso 0.50 1 d PGD A 2 C27 C 0.1939(4) 0.0000 0.8915(8) 0.018(3) Uani 1 2 d SD . 3 C28 C 0.1641(6) 0.0639(12) 0.8713(12) 0.029(5) Uani 0.50 1 d PD . 3 C29 C 0.1312(6) 0.0634(14) 0.9019(12) 0.035(6) Uani 0.50 1 d PD . 3 C30 C 0.1275(5) 0.0000 0.9471(9) 0.034(4) Uani 1 2 d SD . 3 C28' C 0.1911(6) 0.0604(13) 0.9401(11) 0.023(4) Uiso 0.50 1 d PD . 4 C29' C 0.1573(7) 0.0616(14) 0.9665(13) 0.031(5) Uiso 0.50 1 d PD . 4 C31 C 0.4941(4) 0.0899(7) 1.2220(7) 0.015(4) Uani 0.50 1 d PGD B 5 C36 C 0.5307(3) 0.1205(8) 1.2120(8) 0.020(5) Uiso 0.50 1 d PGD B 5 C35 C 0.5286(4) 0.1908(9) 1.1710(9) 0.024(6) Uiso 0.50 1 d PGD B 5 C34 C 0.4900(5) 0.2304(7) 1.1400(8) 0.028(5) Uani 0.50 1 d PGD B 5 C33 C 0.4534(4) 0.1997(7) 1.1499(7) 0.023(5) Uani 0.50 1 d PGD B 5 C32 C 0.4554(3) 0.1295(7) 1.1909(7) 0.019(4) Uani 0.50 1 d PGD B 5 C31' C 0.5014(4) 0.0836(6) 1.2027(6) 0.010(5) Uiso 0.50 1 d PGD B 6 C32' C 0.4781(4) 0.0742(6) 1.1299(6) 0.015(4) Uani 0.50 1 d PGD B 6 C33' C 0.4782(4) 0.1358(8) 1.0811(5) 0.025(5) Uani 0.50 1 d PGD B 6 C34' C 0.5015(4) 0.2069(7) 1.1050(6) 0.020(4) Uani 0.50 1 d PGD B 6 C36' C 0.5248(4) 0.2163(7) 1.1778(7) 0.021(5) Uani 0.50 1 d PGD B 6 C35' C 0.5247(4) 0.1547(8) 1.2266(5) 0.015(4) Uani 0.50 1 d PGD B 6 C49 C 0.6210(4) 0.0000 1.3536(8) 0.024(3) Uani 1 2 d S . 6 C50 C 0.6352(3) -0.0740(7) 1.3349(6) 0.028(3) Uani 1 1 d . . 6 H50 H 0.6260 -0.1234 1.3482 0.034 Uiso 1 1 calc R . 6 C51 C 0.6637(3) -0.0731(7) 1.2955(6) 0.033(3) Uani 1 1 d . . 6 H51 H 0.6732 -0.1221 1.2821 0.040 Uiso 1 1 calc R . 6 C52 C 0.6772(5) 0.0000 1.2770(9) 0.034(4) Uani 1 2 d S . 6 H52 H 0.6962 0.0000 1.2512 0.041 Uiso 1 2 calc SR . 6 O51 O 0.3261(5) 0.5000 0.8526(9) 0.078(5) Uani 1 2 d S . 6 C82 C 0.3013(4) 0.4269(8) 0.8511(9) 0.058(5) Uani 1 1 d . . 6 C80 C 0.2562(5) 0.4555(13) 0.8290(8) 0.097(9) Uani 1 1 d . . 6 C17 C 0.4433(3) 0.0313(7) 0.9324(7) 0.022(4) Uiso 0.50 1 d PGD . 7 C18 C 0.4357(3) 0.0845(7) 0.9821(7) 0.021(4) Uiso 0.50 1 d PGD . 7 C20 C 0.3987(4) 0.0773(7) 0.9995(6) 0.017(4) Uiso 0.50 1 d PGD . 7 C18' C 0.3692(3) 0.0169(7) 0.9672(6) 0.015(4) Uiso 0.50 1 d PGD . 7 C19 C 0.3768(3) -0.0364(6) 0.9175(6) 0.020(4) Uiso 0.50 1 d PGD . 7 C19' C 0.4138(4) -0.0292(7) 0.9001(7) 0.026(5) Uiso 0.50 1 d PGD . 7 C42' C 0.4216(4) 0.0905(6) 1.2524(7) 0.024(5) Uani 0.50 1 d PGD . 8 C41' C 0.3846(4) 0.1038(7) 1.2691(8) 0.027(5) Uani 0.50 1 d PGD . 8 C40' C 0.3737(4) 0.0508(9) 1.3156(8) 0.029(5) Uani 0.50 1 d PGD . 8 C39' C 0.3998(4) -0.0155(8) 1.3455(7) 0.027(7) Uani 0.50 1 d PGD . 8 C37' C 0.4367(4) -0.0287(6) 1.3288(7) 0.020(5) Uani 0.50 1 d PGD . 8 C38' C 0.4476(3) 0.0243(6) 1.2823(7) 0.011(4) Uiso 0.50 1 d PGD . 8 C43 C 0.5878(3) -0.0885(6) 1.4521(5) 0.022(2) Uani 1 1 d . B 8 C48 C 0.6281(3) -0.1096(6) 1.4992(5) 0.021(2) Uani 1 1 d . B 8 H48 H 0.6517 -0.0792 1.4993 0.025 Uiso 1 1 calc R B 8 C44 C 0.5532(4) -0.1358(8) 1.4520(6) 0.036(3) Uani 1 1 d . B 8 H44 H 0.5262 -0.1231 1.4207 0.043 Uiso 1 1 calc R B 8 C47 C 0.6328(4) -0.1747(6) 1.5451(6) 0.026(2) Uani 1 1 d . B 8 H47 H 0.6596 -0.1879 1.5766 0.031 Uiso 1 1 calc R B 8 C46 C 0.5980(4) -0.2213(7) 1.5449(6) 0.030(3) Uani 1 1 d . B 8 H46 H 0.6015 -0.2654 1.5763 0.036 Uiso 1 1 calc R B 8 C45 C 0.5587(4) -0.2020(8) 1.4985(7) 0.040(3) Uani 1 1 d . B 8 H45 H 0.5353 -0.2335 1.4981 0.048 Uiso 1 1 calc R B 8 O60 O 0.7333(9) 0.521(3) 0.5417(17) 0.174(17) Uiso 0.50 1 d PD . -1 C90 C 0.7683(8) 0.5489(14) 0.5196(14) 0.043(6) Uiso 0.50 1 d PD . . C92 C 0.7643(10) 0.6444(17) 0.5123(19) 0.073(10) Uiso 0.50 1 d PD . . C93 C 0.7346(11) 0.691(2) 0.538(2) 0.087(11) Uiso 0.50 1 d PD . . C94 C 0.726(2) 0.607(3) 0.561(4) 0.19(3) Uiso 0.50 1 d PD . . C96 C 0.5086(9) 0.5723(15) 0.4762(14) 0.133(9) Uiso 1 1 d . . . C95 C 0.4983(7) 0.5000 0.4349(11) 0.053(5) Uiso 1 2 d S . . C16 C 0.3034(4) 0.1605(8) 1.0296(5) 0.021(4) Uiso 0.50 1 d PGD . 9 C11 C 0.3206(4) 0.0840(7) 1.0531(6) 0.021(6) Uiso 0.50 1 d PGD . 9 C12 C 0.3399(4) 0.0691(6) 1.1265(7) 0.018(4) Uiso 0.50 1 d PGD . 9 C14 C 0.3418(4) 0.1307(8) 1.1763(5) 0.022(4) Uiso 0.50 1 d PGD . 9 C13 C 0.3246(5) 0.2073(6) 1.1528(6) 0.022(4) Uiso 0.50 1 d PGD . 9 C15 C 0.3053(4) 0.2222(6) 1.0795(7) 0.020(5) Uiso 0.50 1 d PGD . 9 C11' C 0.3199(6) 0.0892(11) 1.0325(13) 0.014(4) Uiso 0.50 1 d PD . 10 C16' C 0.2817(6) 0.1157(12) 1.0382(11) 0.025(5) Uiso 0.50 1 d PD . 10 C12' C 0.3571(6) 0.1358(11) 1.0599(11) 0.022(4) Uiso 0.50 1 d PD . 10 C13' C 0.3548(7) 0.2079(13) 1.0975(13) 0.036(6) Uiso 0.50 1 d PD . 10 C15' C 0.2806(7) 0.1873(13) 1.0766(12) 0.034(5) Uiso 0.50 1 d PD . 10 C14' C 0.3170(7) 0.2315(13) 1.1066(14) 0.028(5) Uiso 0.50 1 d PD . 10 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 0.0114(9) 0.0207(10) 0.0122(10) 0.000 0.0042(8) 0.000 Co2 0.0137(7) 0.0263(7) 0.0121(7) -0.0017(6) 0.0049(6) -0.0006(6) P1 0.0146(18) 0.0252(19) 0.0129(19) 0.000 0.0052(16) 0.000 P2 0.0146(18) 0.0246(19) 0.0139(19) 0.000 0.0039(16) 0.000 P3 0.0130(18) 0.031(2) 0.0144(19) 0.000 0.0041(16) 0.000 P4 0.0136(19) 0.041(2) 0.015(2) 0.000 0.0065(17) 0.000 O1 0.015(5) 0.024(5) 0.010(5) 0.000 0.001(4) 0.000 O2 0.069(6) 0.033(5) 0.016(4) 0.004(4) 0.004(4) -0.018(4) O3 0.053(5) 0.036(5) 0.023(4) 0.004(4) 0.000(4) -0.027(4) O4 0.018(4) 0.039(5) 0.039(5) -0.003(4) 0.009(4) 0.004(3) O5 0.031(5) 0.069(6) 0.033(5) -0.017(5) 0.014(4) 0.009(4) O6 0.018(4) 0.050(5) 0.037(5) -0.001(4) 0.008(4) -0.010(4) O7 0.049(5) 0.046(5) 0.016(4) -0.012(4) 0.013(4) -0.016(4) O8 0.017(4) 0.037(4) 0.027(4) -0.010(4) 0.009(3) -0.007(3) O9 0.033(4) 0.036(4) 0.027(4) -0.012(4) 0.018(4) -0.003(3) O10 0.021(4) 0.029(4) 0.024(4) -0.008(3) 0.003(3) -0.002(3) N1 0.012(4) 0.018(4) 0.013(4) -0.001(3) 0.002(4) 0.000(3) N2 0.013(4) 0.023(4) 0.011(4) -0.001(3) 0.000(4) 0.001(3) N3 0.014(4) 0.018(4) 0.015(4) -0.002(3) 0.005(4) -0.001(3) N4 0.015(4) 0.032(5) 0.013(4) -0.006(4) 0.004(4) 0.000(4) N5 0.018(4) 0.022(4) 0.017(4) -0.001(3) 0.010(4) -0.002(3) N6 0.014(4) 0.031(5) 0.017(4) -0.002(4) 0.007(4) -0.002(4) N7 0.042(6) 0.020(5) 0.021(5) 0.001(4) 0.006(5) -0.005(4) N8 0.024(5) 0.033(5) 0.023(5) 0.002(4) 0.011(5) 0.006(4) N9 0.017(7) 0.044(8) 0.022(7) 0.000 0.007(6) 0.000 N10 0.021(7) 0.053(9) 0.012(7) 0.000 0.006(6) 0.000 N11 0.019(5) 0.033(5) 0.019(5) -0.001(4) 0.006(4) 0.003(4) N12 0.014(6) 0.020(6) 0.017(6) 0.000 0.005(5) 0.000 N13 0.013(7) 0.123(15) 0.019(8) 0.000 0.003(6) 0.000 N14 0.014(7) 0.083(11) 0.014(7) 0.000 0.003(6) 0.000 C1 0.018(5) 0.011(4) 0.014(5) 0.000(4) 0.004(4) 0.003(4) C2 0.020(5) 0.013(5) 0.016(5) 0.006(4) 0.006(5) 0.003(4) C3 0.015(5) 0.013(5) 0.017(5) -0.002(4) 0.005(4) 0.004(4) C4 0.010(5) 0.023(5) 0.017(5) 0.004(4) 0.002(4) 0.000(4) C5 0.013(5) 0.028(5) 0.020(5) 0.003(5) 0.007(5) 0.003(4) C6 0.019(5) 0.034(6) 0.017(6) -0.002(5) 0.006(5) 0.003(4) C7 0.010(5) 0.029(5) 0.015(5) -0.002(4) 0.003(4) -0.004(4) C8 0.010(7) 0.036(8) 0.015(8) 0.000 0.005(6) 0.000 C9 0.014(5) 0.041(6) 0.015(5) -0.007(5) 0.005(5) -0.002(5) C10 0.013(7) 0.044(9) 0.013(8) 0.000 0.005(6) 0.000 C27 0.021(7) 0.015(7) 0.023(8) 0.000 0.013(7) 0.000 C28 0.021(11) 0.030(11) 0.030(13) -0.019(10) 0.001(11) 0.001(9) C29 0.013(11) 0.062(16) 0.030(14) -0.024(13) 0.006(11) 0.002(11) C30 0.024(9) 0.059(11) 0.019(9) 0.000 0.006(8) 0.000 C31 0.015(10) 0.023(11) 0.009(10) 0.005(8) 0.007(9) 0.004(8) C34 0.046(15) 0.009(10) 0.030(13) -0.005(9) 0.016(13) -0.004(10) C33 0.036(13) 0.015(10) 0.017(11) -0.003(8) 0.007(10) 0.000(9) C32 0.025(11) 0.019(10) 0.013(10) -0.004(8) 0.005(9) -0.002(8) C32' 0.021(10) 0.013(9) 0.014(10) -0.003(8) 0.010(9) 0.002(8) C33' 0.033(12) 0.022(11) 0.027(12) 0.000(9) 0.020(11) -0.005(9) C34' 0.020(11) 0.016(10) 0.028(12) -0.008(9) 0.012(10) -0.001(8) C36' 0.034(14) 0.014(11) 0.021(13) 0.000(10) 0.016(11) 0.003(10) C35' 0.012(9) 0.011(9) 0.019(11) -0.008(8) 0.002(9) 0.000(8) C49 0.011(7) 0.046(9) 0.014(8) 0.000 0.004(6) 0.000 C50 0.023(6) 0.040(7) 0.022(6) 0.000(5) 0.009(5) -0.001(5) C51 0.025(6) 0.043(7) 0.036(7) -0.007(6) 0.017(6) 0.003(5) C52 0.024(9) 0.050(10) 0.035(10) 0.000 0.019(8) 0.000 O51 0.089(12) 0.060(10) 0.100(13) 0.000 0.053(11) 0.000 C82 0.025(7) 0.033(7) 0.088(12) 0.035(8) -0.021(7) -0.019(5) C80 0.044(8) 0.21(3) 0.047(9) -0.033(11) 0.028(8) -0.060(11) C42' 0.025(11) 0.020(10) 0.027(12) -0.004(9) 0.009(10) -0.002(9) C41' 0.029(12) 0.025(11) 0.032(13) -0.013(10) 0.018(11) -0.007(9) C40' 0.022(12) 0.039(14) 0.028(13) -0.009(11) 0.012(11) -0.007(10) C39' 0.022(10) 0.03(2) 0.024(10) -0.003(10) 0.007(9) 0.001(10) C37' 0.013(9) 0.023(10) 0.025(11) -0.001(8) 0.006(9) -0.012(7) C43 0.017(5) 0.036(6) 0.014(5) -0.009(5) 0.007(5) -0.008(4) C48 0.022(5) 0.021(5) 0.020(5) -0.007(4) 0.008(5) -0.006(4) C44 0.020(6) 0.061(8) 0.024(6) 0.003(6) 0.004(5) -0.012(6) C47 0.033(6) 0.024(6) 0.021(6) -0.005(5) 0.009(5) -0.003(5) C46 0.047(7) 0.023(6) 0.028(6) -0.010(5) 0.025(6) -0.013(5) C45 0.032(7) 0.060(8) 0.036(7) -0.012(7) 0.022(6) -0.023(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.790(9) . ? Co1 N12 1.912(12) . ? Co1 N3 1.926(7) . ? Co1 N3 1.926(7) 6_565 ? Co1 N1 1.928(7) 6_565 ? Co1 N1 1.928(8) . ? Co2 O1 1.788(5) . ? Co2 N11 1.915(9) . ? Co2 N6 1.931(8) . ? Co2 N2 1.932(8) . ? Co2 N5 1.934(8) . ? Co2 N4 1.941(8) . ? P1 N13 1.547(14) . ? P1 C11' 1.705(19) . ? P1 C11' 1.705(19) 6 ? P1 C18' 1.819(9) 6 ? P1 C18' 1.819(8) . ? P1 C11 1.877(9) . ? P1 C11 1.877(15) 6 ? P2 N13 1.546(14) . ? P2 C21' 1.728(9) 6 ? P2 C21' 1.728(9) . ? P2 C27 1.804(13) . ? P2 C21 1.887(9) 6 ? P2 C21 1.887(9) . ? P3 N14 1.550(13) . ? P3 C31 1.700(9) 6 ? P3 C31 1.700(9) . ? P3 C38' 1.824(8) . ? P3 C38' 1.824(10) 6 ? P3 C31' 1.896(9) 6 ? P3 C31' 1.896(9) . ? P4 N14 1.559(13) . ? P4 C43 1.793(11) 6 ? P4 C43 1.793(11) . ? P4 C49 1.796(13) . ? O1 Co2 1.788(5) 6_565 ? O2 N7 1.235(11) . ? O3 N7 1.232(11) . ? O4 N8 1.235(11) . ? O5 N8 1.232(11) . ? O6 N9 1.235(9) . ? O7 N10 1.233(9) . ? O8 N11 1.248(10) . ? O9 N11 1.240(10) . ? O10 N12 1.240(9) . ? N1 C1 1.328(11) . ? N1 N2 1.381(11) . ? N2 C3 1.314(11) . ? N3 C4 1.329(11) . ? N3 N4 1.377(11) . ? N4 C6 1.323(12) . ? N5 C7 1.322(11) . ? N5 N5 1.395(16) 6_565 ? N6 C9 1.325(12) . ? N6 N6 1.387(16) 6_565 ? N7 C2 1.419(12) . ? N8 C5 1.410(12) . ? N9 O6 1.235(9) 6_565 ? N9 C8 1.412(17) . ? N10 O7 1.233(9) 6_565 ? N10 C10 1.416(17) . ? N12 O10 1.240(9) 6_565 ? C1 C2 1.398(13) . ? C1 H1 0.9300 . ? C2 C3 1.372(13) . ? C3 H3 0.9300 . ? C4 C5 1.386(13) . ? C4 H4 0.9300 . ? C5 C6 1.385(13) . ? C6 H6 0.9300 . ? C7 C8 1.385(12) . ? C7 H7 0.9300 . ? C8 C7 1.385(12) 6_565 ? C9 C10 1.381(13) . ? C9 H9 0.9300 . ? C10 C9 1.381(13) 6_565 ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C21' C22' 1.3900 . ? C21' C26' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? C27 C28 1.405(19) . ? C27 C28 1.41(2) 6 ? C28 C29 1.41(2) . ? C29 C30 1.39(2) . ? C30 C29 1.39(2) 6 ? C28' C29' 1.39(2) . ? C28' C28' 1.97(4) 6 ? C29' C29' 2.01(5) 6 ? C31 C36 1.3900 . ? C31 C32 1.3900 . ? C36 C35 1.3900 . ? C35 C34 1.3900 . ? C34 C33 1.3900 . ? C33 C32 1.3900 . ? C31' C32' 1.3900 . ? C31' C35' 1.3900 . ? C32' C33' 1.3900 . ? C33' C34' 1.3900 . ? C34' C36' 1.3900 . ? C36' C35' 1.3900 . ? C49 C50 1.391(12) 6 ? C49 C50 1.391(12) . ? C50 C51 1.407(13) . ? C50 H50 0.9300 . ? C51 C52 1.367(13) . ? C51 H51 0.9300 . ? C52 C51 1.367(13) 6 ? C52 H52 0.9300 . ? O51 C82 1.447(14) 6_565 ? O51 C82 1.447(14) . ? C82 C80 1.50(2) . ? C80 C80 1.45(4) 6_565 ? C17 C19' 0.9789 6 ? C17 C17 1.02(2) 6 ? C17 C18 1.3900 . ? C17 C19' 1.3900 . ? C18 C20 1.3900 . ? C18 C19' 1.779(11) 6 ? C20 C18' 1.3900 . ? C20 C19 1.671(9) 6 ? C20 C18' 1.824(19) 6 ? C18' C18' 0.55(2) 6 ? C18' C19 1.130(6) 6 ? C18' C19 1.3900 . ? C18' C20 1.824(18) 6 ? C19 C18' 1.130(6) 6 ? C19 C19 1.19(2) 6 ? C19 C19' 1.3900 . ? C19 C20 1.671(9) 6 ? C19 C19' 1.751(14) 6 ? C19' C19' 0.95(2) 6 ? C19' C17 0.979(7) 6 ? C19' C19 1.751(13) 6 ? C19' C18 1.779(11) 6 ? C42' C41' 1.3900 . ? C42' C38' 1.3900 . ? C42' C37' 1.738(12) 6 ? C41' C40' 1.3900 . ? C41' C39' 2.021(19) 6 ? C40' C39' 1.046(15) 6 ? C40' C39' 1.3900 . ? C40' C40' 1.66(3) 6 ? C39' C39' 0.51(3) 6 ? C39' C40' 1.046(16) 6 ? C39' C37' 1.3900 . ? C39' C37' 1.551(10) 6 ? C39' C41' 2.021(16) 6 ? C37' C37' 0.94(2) 6 ? C37' C38' 1.0899(15) 6 ? C37' C38' 1.3900 . ? C37' C39' 1.551(12) 6 ? C37' C42' 1.738(17) 6 ? C38' C38' 0.79(2) 6 ? C38' C37' 1.0899(14) 6 ? C43 C44 1.389(14) . ? C43 C48 1.398(14) . ? C48 C47 1.368(14) . ? C48 H48 0.9300 . ? C44 C45 1.388(17) . ? C44 H44 0.9300 . ? C47 C46 1.385(14) . ? C47 H47 0.9300 . ? C46 C45 1.364(17) . ? C46 H46 0.9300 . ? C45 H45 0.9300 . ? O60 C90 1.45(3) . ? O60 C94 1.49(3) . ? O60 C90 1.78(4) 6_565 ? C90 C92 1.57(3) . ? C90 C90 1.60(5) 6_565 ? C90 O60 1.78(4) 6_565 ? C92 C93 1.47(3) . ? C92 C94 1.94(7) . ? C93 C94 1.52(3) . ? C96 C96 1.25(4) 2_656 ? C96 C95 1.41(3) . ? C95 C96 1.41(3) 6_565 ? C16 C11 1.3900 . ? C16 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C14 1.3900 . ? C14 C13 1.3900 . ? C13 C15 1.3900 . ? C11' C16' 1.38(2) . ? C11' C12' 1.40(2) . ? C16' C15' 1.40(2) . ? C12' C13' 1.41(2) . ? C13' C14' 1.38(2) . ? C15' C14' 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N12 179.6(4) . . ? O1 Co1 N3 84.4(3) . . ? N12 Co1 N3 95.9(3) . . ? O1 Co1 N3 84.4(3) . 6_565 ? N12 Co1 N3 95.9(3) . 6_565 ? N3 Co1 N3 90.7(4) . 6_565 ? O1 Co1 N1 84.4(3) . 6_565 ? N12 Co1 N1 95.4(3) . 6_565 ? N3 Co1 N1 168.7(4) . 6_565 ? N3 Co1 N1 87.1(3) 6_565 6_565 ? O1 Co1 N1 84.4(3) . . ? N12 Co1 N1 95.4(3) . . ? N3 Co1 N1 87.1(3) . . ? N3 Co1 N1 168.7(4) 6_565 . ? N1 Co1 N1 93.0(4) 6_565 . ? O1 Co2 N11 178.4(4) . . ? O1 Co2 N6 85.0(4) . . ? N11 Co2 N6 96.6(4) . . ? O1 Co2 N2 84.0(4) . . ? N11 Co2 N2 94.4(3) . . ? N6 Co2 N2 169.0(3) . . ? O1 Co2 N5 84.6(3) . . ? N11 Co2 N5 95.6(3) . . ? N6 Co2 N5 85.7(3) . . ? N2 Co2 N5 92.4(3) . . ? O1 Co2 N4 84.2(4) . . ? N11 Co2 N4 95.7(3) . . ? N6 Co2 N4 91.6(3) . . ? N2 Co2 N4 88.1(3) . . ? N5 Co2 N4 168.6(3) . . ? N13 P1 C11' 108.5(7) . . ? N13 P1 C11' 108.5(7) . 6 ? C11' P1 C11' 117.4(16) . 6 ? N13 P1 C18' 109.6(6) . 6 ? C11' P1 C18' 113.9(7) . 6 ? C11' P1 C18' 98.4(7) 6 6 ? N13 P1 C18' 109.6(6) . . ? C11' P1 C18' 98.4(7) . . ? C11' P1 C18' 113.9(7) 6 . ? C18' P1 C18' 17.4(7) 6 . ? N13 P1 C11 115.4(5) . . ? C11' P1 C11 11.8(9) . . ? C11' P1 C11 105.7(9) 6 . ? C18' P1 C11 117.4(6) 6 . ? C18' P1 C11 103.8(6) . . ? N13 P1 C11 115.4(10) . 6 ? C11' P1 C11 105.7(11) . 6 ? C11' P1 C11 11.8(11) 6 6 ? C18' P1 C11 103.8(10) 6 6 ? C18' P1 C11 117.4(11) . 6 ? C11 P1 C11 93.9(12) . 6 ? N13 P2 C21' 106.5(5) . 6 ? N13 P2 C21' 106.5(5) . . ? C21' P2 C21' 106.0(10) 6 . ? N13 P2 C27 114.2(7) . . ? C21' P2 C27 111.6(6) 6 . ? C21' P2 C27 111.6(6) . . ? N13 P2 C21 112.8(5) . 6 ? C21' P2 C21 9.5(7) 6 6 ? C21' P2 C21 109.7(5) . 6 ? C27 P2 C21 102.2(5) . 6 ? N13 P2 C21 112.8(5) . . ? C21' P2 C21 109.7(5) 6 . ? C21' P2 C21 9.5(7) . . ? C27 P2 C21 102.2(5) . . ? C21 P2 C21 111.9(8) 6 . ? N14 P3 C31 112.2(5) . 6 ? N14 P3 C31 112.2(5) . . ? C31 P3 C31 119.4(10) 6 . ? N14 P3 C38' 109.7(6) . . ? C31 P3 C38' 111.4(6) 6 . ? C31 P3 C38' 89.4(6) . . ? N14 P3 C38' 109.7(6) . 6 ? C31 P3 C38' 89.4(6) 6 6 ? C31 P3 C38' 111.4(6) . 6 ? C38' P3 C38' 25.1(7) . 6 ? N14 P3 C31' 114.1(5) . 6 ? C31 P3 C31' 15.5(5) 6 6 ? C31 P3 C31' 106.3(7) . 6 ? C38' P3 C31' 122.1(6) . 6 ? C38' P3 C31' 102.6(6) 6 6 ? N14 P3 C31' 114.1(5) . . ? C31 P3 C31' 106.3(7) 6 . ? C31 P3 C31' 15.5(5) . . ? C38' P3 C31' 102.6(5) . . ? C38' P3 C31' 122.1(6) 6 . ? C31' P3 C31' 92.2(8) 6 . ? N14 P4 C43 109.5(4) . 6 ? N14 P4 C43 109.5(4) . . ? C43 P4 C43 107.5(6) 6 . ? N14 P4 C49 113.9(7) . . ? C43 P4 C49 108.1(4) 6 . ? C43 P4 C49 108.1(4) . . ? Co2 O1 Co2 120.1(5) . 6_565 ? Co2 O1 Co1 119.9(3) . . ? Co2 O1 Co1 119.9(3) 6_565 . ? C1 N1 N2 108.5(7) . . ? C1 N1 Co1 135.1(7) . . ? N2 N1 Co1 116.4(6) . . ? C3 N2 N1 108.7(8) . . ? C3 N2 Co2 134.9(7) . . ? N1 N2 Co2 116.4(6) . . ? C4 N3 N4 108.6(7) . . ? C4 N3 Co1 134.0(7) . . ? N4 N3 Co1 117.0(6) . . ? C6 N4 N3 108.3(8) . . ? C6 N4 Co2 135.6(7) . . ? N3 N4 Co2 115.8(6) . . ? C7 N5 N5 108.6(6) . 6_565 ? C7 N5 Co2 135.2(7) . . ? N5 N5 Co2 116.1(2) 6_565 . ? C9 N6 N6 108.3(6) . 6_565 ? C9 N6 Co2 135.3(8) . . ? N6 N6 Co2 116.3(2) 6_565 . ? O3 N7 O2 123.7(9) . . ? O3 N7 C2 117.8(9) . . ? O2 N7 C2 118.5(9) . . ? O5 N8 O4 123.6(8) . . ? O5 N8 C5 118.2(9) . . ? O4 N8 C5 118.2(9) . . ? O6 N9 O6 123.4(12) . 6_565 ? O6 N9 C8 118.3(6) . . ? O6 N9 C8 118.3(6) 6_565 . ? O7 N10 O7 122.9(12) . 6_565 ? O7 N10 C10 118.5(6) . . ? O7 N10 C10 118.5(6) 6_565 . ? O9 N11 O8 119.7(9) . . ? O9 N11 Co2 119.6(7) . . ? O8 N11 Co2 120.7(6) . . ? O10 N12 O10 119.9(12) 6_565 . ? O10 N12 Co1 120.0(6) 6_565 . ? O10 N12 Co1 120.0(6) . . ? P2 N13 P1 167.4(9) . . ? P3 N14 P4 159.9(9) . . ? N1 C1 C2 107.3(8) . . ? N1 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? C3 C2 C1 106.8(8) . . ? C3 C2 N7 126.5(9) . . ? C1 C2 N7 126.6(9) . . ? N2 C3 C2 108.7(8) . . ? N2 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? N3 C4 C5 108.2(8) . . ? N3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? C6 C5 C4 106.2(8) . . ? C6 C5 N8 127.1(10) . . ? C4 C5 N8 126.6(9) . . ? N4 C6 C5 108.7(9) . . ? N4 C6 H6 125.6 . . ? C5 C6 H6 125.6 . . ? N5 C7 C8 107.4(9) . . ? N5 C7 H7 126.3 . . ? C8 C7 H7 126.3 . . ? C7 C8 C7 107.9(11) . 6_565 ? C7 C8 N9 126.1(6) . . ? C7 C8 N9 126.1(6) 6_565 . ? N6 C9 C10 108.1(10) . . ? N6 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? C9 C10 C9 107.1(12) 6_565 . ? C9 C10 N10 126.4(6) 6_565 . ? C9 C10 N10 126.4(6) . . ? C22 C21 C26 120.0 . . ? C22 C21 P2 118.9(7) . . ? C26 C21 P2 121.1(7) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C22' C21' C26' 120.0 . . ? C22' C21' P2 118.2(8) . . ? C26' C21' P2 121.7(8) . . ? C23' C22' C21' 120.0 . . ? C22' C23' C24' 120.0 . . ? C23' C24' C25' 120.0 . . ? C26' C25' C24' 120.0 . . ? C25' C26' C21' 120.0 . . ? C28 C27 C28 96.0(19) . 6 ? C28 C27 P2 118.8(10) . . ? C28 C27 P2 118.8(10) 6 . ? C27 C28 C29 116.8(19) . . ? C30 C29 C28 121.2(19) . . ? C29 C30 C29 95.9(19) 6 . ? C29' C28' C28' 90.8(13) . 6 ? C28' C29' C29' 89.2(13) . 6 ? C36 C31 C32 120.0 . . ? C36 C31 P3 118.3(8) . . ? C32 C31 P3 121.5(8) . . ? C31 C36 C35 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C34 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C32 C31 120.0 . . ? C32' C31' C35' 120.0 . . ? C32' C31' P3 117.9(7) . . ? C35' C31' P3 122.0(7) . . ? C31' C32' C33' 120.0 . . ? C32' C33' C34' 120.0 . . ? C36' C34' C33' 120.0 . . ? C34' C36' C35' 120.0 . . ? C36' C35' C31' 120.0 . . ? C50 C49 C50 120.7(12) 6 . ? C50 C49 P4 119.5(6) 6 . ? C50 C49 P4 119.5(6) . . ? C49 C50 C51 119.1(10) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C52 C51 C50 119.7(11) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C51 121.8(13) 6 . ? C51 C52 H52 119.1 6 . ? C51 C52 H52 119.1 . . ? C82 O51 C82 111.2(15) 6_565 . ? O51 C82 C80 105.1(12) . . ? C80 C80 C82 108.2(9) 6_565 . ? C19' C17 C17 88.0(13) 6 6 ? C19' C17 C18 95.8(8) 6 . ? C17 C17 C18 128.7(4) 6 . ? C19' C17 C19' 43.3(13) 6 . ? C17 C17 C19' 44.7(4) 6 . ? C18 C17 C19' 120.0 . . ? C20 C18 C17 120.0 . . ? C20 C18 C19' 92.60(9) . 6 ? C17 C18 C19' 33.2(3) . 6 ? C18 C20 C18' 120.0 . . ? C18 C20 C19 86.56(8) . 6 ? C18' C20 C19 42.1(5) . 6 ? C18 C20 C18' 114.0(2) . 6 ? C18' C20 C18' 12.3(4) . 6 ? C19 C20 C18' 46.6(5) 6 6 ? C18' C18' C19 106.4(10) 6 6 ? C18' C18' C20 135.3 6 . ? C19 C18' C20 82.4(7) 6 . ? C18' C18' C19 51.3 6 . ? C19 C18' C19 55.1(10) 6 . ? C20 C18' C19 120.0 . . ? C18' C18' P1 81.3(7) 6 . ? C19 C18' P1 134.6(8) 6 . ? C20 C18' P1 123.8(6) . . ? C19 C18' P1 116.2(6) . . ? C18' C18' C20 32.4(4) 6 6 ? C19 C18' C20 106.8(8) 6 6 ? C20 C18' C20 102.8(4) . 6 ? C19 C18' C20 60.92(17) . 6 ? P1 C18' C20 102.3(9) . 6 ? C18' C19 C19 73.6(11) 6 6 ? C18' C19 C19' 131.0(4) 6 . ? C19 C19 C19' 85.2 6 . ? C18' C19 C18' 22.4(11) 6 . ? C19 C19 C18' 51.3 6 . ? C19' C19 C18' 120.0 . . ? C18' C19 C20 55.5(5) 6 6 ? C19 C19 C20 113.6(7) 6 6 ? C19' C19 C20 97.3 . 6 ? C18' C19 C20 72.5(6) . 6 ? C18' C19 C19' 111.6(10) 6 6 ? C19 C19 C19' 52.3(6) 6 6 ? C19' C19 C19' 32.9(6) . 6 ? C18' C19 C19' 93.2(5) . 6 ? C20 C19 C19' 108.6(4) 6 6 ? C19' C19' C17 92.0(14) 6 6 ? C19' C19' C19 94.8 6 . ? C17 C19' C19 128.4(5) 6 . ? C19' C19' C17 44.7 6 . ? C17 C19' C17 47.3(14) 6 . ? C19 C19' C17 120.0 . . ? C19' C19' C19 52.3(6) 6 6 ? C17 C19' C19 121.1(9) 6 6 ? C19 C19' C19 42.6(6) . 6 ? C17 C19' C19 85.1(5) . 6 ? C19' C19' C18 120.5(6) 6 6 ? C17 C19' C18 51.0(10) 6 6 ? C19 C19' C18 82.5 . 6 ? C17 C19' C18 86.0(5) . 6 ? C19 C19' C18 103.9(4) 6 6 ? C41' C42' C38' 120.0 . . ? C41' C42' C37' 85.18(15) . 6 ? C38' C42' C37' 38.8(4) . 6 ? C42' C41' C40' 120.0 . . ? C42' C41' C39' 92.23(14) . 6 ? C40' C41' C39' 28.8 . 6 ? C39' C40' C39' 17.7(12) 6 . ? C39' C40' C41' 111.3(7) 6 . ? C39' C40' C41' 120.0 . . ? C39' C40' C40' 56.5(12) 6 6 ? C39' C40' C40' 38.9 . 6 ? C41' C40' C40' 128.5 . 6 ? C39' C39' C40' 123.5(13) 6 6 ? C39' C39' C40' 38.9 6 . ? C40' C39' C40' 84.6(13) 6 . ? C39' C39' C37' 99.0 6 . ? C40' C39' C37' 114.7(7) 6 . ? C40' C39' C37' 120.0 . . ? C39' C39' C37' 62.3(7) 6 6 ? C40' C39' C37' 135.1(2) 6 6 ? C40' C39' C37' 88.7(6) . 6 ? C37' C39' C37' 36.7(7) . 6 ? C39' C39' C41' 135.6(5) 6 6 ? C40' C39' C41' 39.9(7) 6 6 ? C40' C39' C41' 105.9(4) . 6 ? C37' C39' C41' 74.8 . 6 ? C37' C39' C41' 101.4(5) 6 6 ? C37' C37' C38' 86.2(11) 6 6 ? C37' C37' C39' 81.0 6 . ? C38' C37' C39' 138.7(4) 6 . ? C37' C37' C38' 51.5 6 . ? C38' C37' C38' 34.7(11) 6 . ? C39' C37' C38' 120.0 . . ? C37' C37' C39' 62.3(9) 6 6 ? C38' C37' C39' 130.6(9) 6 6 ? C39' C37' C39' 18.8(9) . 6 ? C38' C37' C39' 104.2(7) . 6 ? C37' C37' C42' 125.5(9) 6 6 ? C38' C37' C42' 53.1(6) 6 6 ? C39' C37' C42' 105.4(7) . 6 ? C38' C37' C42' 82.0(9) . 6 ? C39' C37' C42' 115.3(7) 6 6 ? C38' C38' C37' 93.8(11) 6 6 ? C38' C38' C37' 51.5 6 . ? C37' C38' C37' 42.4(11) 6 . ? C38' C38' C42' 141.1 6 . ? C37' C38' C42' 88.1(9) 6 . ? C37' C38' C42' 120.0 . . ? C38' C38' P3 77.4(6) 6 . ? C37' C38' P3 136.2(8) 6 . ? C37' C38' P3 114.8(6) . . ? C42' C38' P3 125.2(6) . . ? C44 C43 C48 118.7(10) . . ? C44 C43 P4 120.2(9) . . ? C48 C43 P4 121.1(7) . . ? C47 C48 C43 120.2(9) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C45 C44 C43 120.2(11) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C48 C47 C46 120.7(11) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C45 C46 C47 119.7(11) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C46 C45 C44 120.5(10) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C90 O60 C94 90(4) . . ? C90 O60 C90 58(2) . 6_565 ? C94 O60 C90 147(4) . 6_565 ? O60 C90 C92 107(3) . . ? O60 C90 C90 72(2) . 6_565 ? C92 C90 C90 174.1(17) . 6_565 ? O60 C90 O60 21(3) . 6_565 ? C92 C90 O60 128(2) . 6_565 ? C90 C90 O60 50.2(13) 6_565 6_565 ? C93 C92 C90 122(3) . . ? C93 C92 C94 50.6(19) . . ? C90 C92 C94 72(2) . . ? C92 C93 C94 81(3) . . ? O60 C94 C93 135(5) . . ? O60 C94 C92 88(4) . . ? C93 C94 C92 48(2) . . ? C96 C96 C95 110.1(19) 2_656 . ? C96 C95 C96 114(3) . 6_565 ? C11 C16 C15 120.0 . . ? C16 C11 C12 120.0 . . ? C16 C11 P1 121.6(7) . . ? C12 C11 P1 118.4(7) . . ? C14 C12 C11 120.0 . . ? C13 C14 C12 120.0 . . ? C14 C13 C15 120.0 . . ? C13 C15 C16 120.0 . . ? C16' C11' C12' 121.4(17) . . ? C16' C11' P1 118.4(14) . . ? C12' C11' P1 120.2(14) . . ? C11' C16' C15' 119.6(19) . . ? C11' C12' C13' 117.5(17) . . ? C14' C13' C12' 121(2) . . ? C14' C15' C16' 120(2) . . ? C15' C14' C13' 121(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.805 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.128 # Attachment 'Co10.cif' data_co10 _database_code_depnum_ccdc_archive 'CCDC 750243' #TrackingRef 'Co10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H172 Co10 N53 O32' _chemical_formula_weight 3362.33 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.606(5) _cell_length_b 29.622(6) _cell_length_c 34.452(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.59(3) _cell_angle_gamma 90.00 _cell_volume 22698(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 3.2434 _cell_measurement_theta_max 23.7040 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6964 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7883 _exptl_absorpt_correction_T_max 0.8911 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The low completeness of the data set reulted due to poor diffraction of the crystal. Several crystallisation effort didn't afforded any better crystals. Theta max for this data set has been truncated at 23.76 as higher angle data resulted in even lower completeness. ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Kappa CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean 15.9832 _diffrn_reflns_number 31197 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.2396 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 23.76 _reflns_number_total 14584 _reflns_number_gt 5626 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The thermal ellipsoids of C-atoms on the TBA counter ions are fixed but the coordinates are refined. Some large and some small thermal ellipsoids resulted in the disordered counter ions,which in some cases could not be modeled properly.This in turn also resulted in relatively high R value. After refinement as above,the raw data file was modified by the program SQUEEZE to eliminate unaccounted electron density attributed to interstitial solvent molecules that were not located in the difference map. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.056 0.500 0.000 890 351 ' ' 2 -0.009 0.000 0.500 890 345 ' ' _platon_squeeze_details ; ; _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^)+(0.1942P)^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 14584 _refine_ls_number_parameters 836 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.1683 _refine_ls_R_factor_gt 0.1085 _refine_ls_wR_factor_ref 0.3174 _refine_ls_wR_factor_gt 0.2932 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.847 _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 0.90280(8) 0.13060(5) 0.03846(5) 0.0427(5) Uani 1 1 d . . . Co2 Co 0.87754(8) 0.16414(5) 0.11682(5) 0.0435(5) Uani 1 1 d . . . Co3 Co 0.80821(8) 0.23092(5) 0.15383(5) 0.0446(5) Uani 1 1 d . . . Co5 Co 0.63075(8) 0.35965(5) 0.05611(5) 0.0473(5) Uani 1 1 d . . . Co4 Co 0.71274(8) 0.30682(5) 0.13162(5) 0.0472(5) Uani 1 1 d . . . N1 N 0.9548(5) 0.1360(3) 0.1257(3) 0.047(3) Uani 1 1 d . . . N4 N 0.8474(5) 0.0965(3) 0.0557(3) 0.055(3) Uani 1 1 d . . . O4 O 0.8045(4) 0.1940(2) 0.1077(2) 0.047(2) Uani 1 1 d . . . H3 H 0.7710 0.1912 0.0840 0.057 Uiso 1 1 calc R . . C16 C 0.9668(6) 0.2378(4) 0.1378(4) 0.042(3) Uani 1 1 d . . . H8 H 0.9954 0.2254 0.1279 0.051 Uiso 1 1 calc R . . O10 O 0.6663(4) 0.3045(2) 0.0760(2) 0.052(2) Uani 1 1 d . . . H5 H 0.6615 0.2786 0.0600 0.062 Uiso 1 1 calc R . . O1 O 0.8827(3) 0.1814(2) 0.0651(2) 0.047(2) Uani 1 1 d . . . H2 H 0.8764 0.2105 0.0543 0.057 Uiso 1 1 calc R . . N8 N 0.8846(5) 0.2487(3) 0.1558(3) 0.055(3) Uani 1 1 d . . . C14 C 0.9185(6) 0.2870(4) 0.1644(3) 0.039(3) Uani 1 1 d . . . H6 H 0.9088 0.3132 0.1757 0.047 Uiso 1 1 calc R . . O6 O 1.0563(5) 0.3044(4) 0.1453(3) 0.086(3) Uani 1 1 d . . . N14 N 0.7277(5) 0.2137(4) 0.1469(3) 0.050(3) Uani 1 1 d . . . N19 N 0.7420(5) 0.3642(3) 0.1215(3) 0.041(3) Uani 1 1 d . . . N13 N 0.6856(5) 0.2467(3) 0.1381(3) 0.042(3) Uani 1 1 d . . . N12 N 0.8105(5) 0.2740(3) 0.1963(3) 0.048(3) Uani 1 1 d . . . C10 C 0.8475(6) 0.1111(4) 0.2200(4) 0.049(4) Uani 1 1 d . . . H1 H 0.8453 0.0898 0.2392 0.059 Uiso 1 1 calc R . . N10 N 1.0129(6) 0.3152(4) 0.1571(3) 0.061(3) Uani 1 1 d . . . N16 N 0.6038(5) 0.3576(4) 0.1048(3) 0.058(3) Uani 1 1 d . . . N3 N 0.8320(5) 0.1119(3) 0.0890(3) 0.057(3) Uani 1 1 d . . . N17 N 0.6430(5) 0.3337(4) 0.1386(3) 0.057(3) Uani 1 1 d . . . N11 N 0.7696(5) 0.3069(4) 0.1880(3) 0.052(3) Uani 1 1 d . . . C1 C 1.0064(6) 0.1340(4) 0.1580(4) 0.044(3) Uani 1 1 d . . . C6 C 0.7860(6) 0.0887(4) 0.0927(4) 0.056(4) Uani 1 1 d . . . H9A H 0.7676 0.0925 0.1125 0.067 Uiso 1 1 calc R . . N2 N 0.9664(5) 0.1221(3) 0.0914(3) 0.046(3) Uani 1 1 d . . . N9 N 0.9175(5) 0.2184(3) 0.1395(3) 0.047(3) Uani 1 1 d . . . C32 C 0.7947(7) 0.3869(4) 0.1365(4) 0.062(4) Uani 1 1 d . . . H36 H 0.8280 0.3783 0.1588 0.074 Uiso 1 1 calc R . . O5 O 1.0109(6) 0.3508(3) 0.1743(4) 0.108(4) Uani 1 1 d . . . C11 C 0.8725(6) 0.1069(4) 0.1902(4) 0.054(4) Uani 1 1 d . . . C8 C 0.8095(6) 0.0646(4) 0.0390(4) 0.054(4) Uani 1 1 d . . . H11 H 0.8085 0.0489 0.0154 0.065 Uiso 1 1 calc R . . C23 C 0.6399(9) 0.1831(5) 0.1322(5) 0.077(5) Uani 1 1 d . . . N18 N 0.7037(5) 0.3865(3) 0.0880(3) 0.045(3) Uani 1 1 d . . . C18 C 0.8363(7) 0.3224(5) 0.2486(4) 0.065(4) Uani 1 1 d . . . H27 H 0.8569 0.3367 0.2734 0.078 Uiso 1 1 calc R . . N7 N 0.8680(5) 0.1456(3) 0.1673(3) 0.054(3) Uani 1 1 d . . . C2 C 1.0491(6) 0.1181(4) 0.1438(4) 0.053(4) Uani 1 1 d . . . H13 H 1.0888 0.1120 0.1596 0.064 Uiso 1 1 calc R . . C9 C 0.8253(6) 0.1559(5) 0.2149(4) 0.051(4) Uani 1 1 d . . . C4 C 1.0106(6) 0.1452(4) 0.2006(4) 0.062(4) Uani 1 1 d . . . H15A H 0.9736 0.1587 0.2005 0.093 Uiso 1 1 calc R . . H15B H 1.0431 0.1660 0.2121 0.093 Uiso 1 1 calc R . . H15C H 1.0178 0.1181 0.2169 0.093 Uiso 1 1 calc R . . C17 C 0.7839(7) 0.3372(5) 0.2199(4) 0.068(4) Uani 1 1 d . . . C3 C 1.0237(7) 0.1124(4) 0.1022(4) 0.055(4) Uani 1 1 d . . . C30 C 0.7328(6) 0.4228(4) 0.0824(4) 0.055(4) Uani 1 1 d . . . H34 H 0.7177 0.4439 0.0615 0.066 Uiso 1 1 calc R . . C25 C 0.5534(7) 0.3667(5) 0.1104(5) 0.073(5) Uani 1 1 d . . . C26 C 0.5535(6) 0.3478(5) 0.1494(4) 0.067(4) Uani 1 1 d . . . H32 H 0.5231 0.3493 0.1609 0.080 Uiso 1 1 calc R . . N6 N 0.8370(5) 0.1762(3) 0.1851(3) 0.049(3) Uani 1 1 d . . . C20 C 0.7437(8) 0.3782(5) 0.2208(4) 0.109(7) Uani 1 1 d . . . H25A H 0.7685 0.4044 0.2302 0.163 Uiso 1 1 calc R . . H25B H 0.7218 0.3720 0.2392 0.163 Uiso 1 1 calc R . . H25C H 0.7160 0.3836 0.1936 0.163 Uiso 1 1 calc R . . C19 C 0.8535(6) 0.2825(4) 0.2345(4) 0.056(4) Uani 1 1 d . . . C13 C 0.9014(6) 0.0649(4) 0.1740(5) 0.083(5) Uani 1 1 d . . . H5A H 0.8979 0.0698 0.1458 0.124 Uiso 1 1 calc R . . H5B H 0.8805 0.0377 0.1762 0.124 Uiso 1 1 calc R . . H5C H 0.9431 0.0621 0.1904 0.124 Uiso 1 1 calc R . . C15 C 0.9669(7) 0.2814(4) 0.1543(3) 0.049(4) Uani 1 1 d . . . C12 C 0.7949(7) 0.1779(5) 0.2422(4) 0.079(5) Uani 1 1 d . . . H4A H 0.8248 0.1889 0.2668 0.118 Uiso 1 1 calc R . . H4B H 0.7698 0.1562 0.2493 0.118 Uiso 1 1 calc R . . H4C H 0.7707 0.2027 0.2277 0.118 Uiso 1 1 calc R . . O8 O 0.5379(6) 0.1654(5) 0.1128(7) 0.190(9) Uani 1 1 d . . . C27 C 0.6096(8) 0.3271(5) 0.1659(5) 0.069(4) Uani 1 1 d . . . C7 C 0.7710(9) 0.0572(4) 0.0606(5) 0.078(5) Uani 1 1 d . . . O9 O 0.6064(6) 0.1112(4) 0.1265(6) 0.165(7) Uani 1 1 d U . . C22 C 0.6305(7) 0.2292(5) 0.1278(4) 0.063(4) Uani 1 1 d . . . H22 H 0.5940 0.2445 0.1194 0.075 Uiso 1 1 calc R . . C31 C 0.7900(7) 0.4247(5) 0.1129(5) 0.073(5) Uani 1 1 d . . . C24 C 0.6975(6) 0.1734(4) 0.1446(4) 0.066(5) Uani 1 1 d . . . H24 H 0.7147 0.1449 0.1507 0.079 Uiso 1 1 calc R . . C21 C 0.9079(7) 0.2557(5) 0.2549(4) 0.071(4) Uani 1 1 d . . . H29A H 0.8980 0.2311 0.2697 0.107 Uiso 1 1 calc R . . H29B H 0.9377 0.2745 0.2739 0.107 Uiso 1 1 calc R . . H29C H 0.9236 0.2440 0.2346 0.107 Uiso 1 1 calc R . . C28 C 0.4985(6) 0.3908(5) 0.0794(4) 0.068(4) Uani 1 1 d . . . H30A H 0.5036 0.3923 0.0529 0.102 Uiso 1 1 calc R . . H30B H 0.4953 0.4208 0.0890 0.102 Uiso 1 1 calc R . . H30C H 0.4625 0.3742 0.0770 0.102 Uiso 1 1 calc R . . C29 C 0.6342(8) 0.3004(6) 0.2032(4) 0.101(7) Uani 1 1 d . . . H77A H 0.6422 0.2703 0.1960 0.152 Uiso 1 1 calc R . . H77B H 0.6058 0.2993 0.2176 0.152 Uiso 1 1 calc R . . H77C H 0.6709 0.3139 0.2205 0.152 Uiso 1 1 calc R . . N15 N 0.5888(9) 0.1514(6) 0.1223(6) 0.128(6) Uani 1 1 d U . . C5 C 1.0556(6) 0.0944(5) 0.0727(4) 0.076(5) Uani 1 1 d . . . H16A H 1.0720 0.0650 0.0817 0.113 Uiso 1 1 calc R . . H16B H 1.0875 0.1146 0.0729 0.113 Uiso 1 1 calc R . . H16C H 1.0272 0.0923 0.0453 0.113 Uiso 1 1 calc R . . O15 O 0.8428(4) 0.1442(2) -0.0109(3) 0.054(2) Uani 1 1 d . . . H1A H 0.8037 0.1520 -0.0128 0.081 Uiso 1 1 calc R . . N23 N 0.9164(4) 0.0781(3) 0.0085(3) 0.048(3) Uani 1 1 d . . . N25 N 0.9528(5) 0.1673(3) 0.0193(3) 0.056(3) Uani 1 1 d . . . N21 N 0.5600(5) 0.3306(4) 0.0225(4) 0.057(3) Uani 1 1 d . . . C33 C 0.5242(8) 0.3012(6) 0.0295(4) 0.074(5) Uani 1 1 d . . . H37 H 0.5272 0.2919 0.0559 0.089 Uiso 1 1 calc R . . N24 N 0.9031(5) 0.0815(4) -0.0327(3) 0.060(3) Uani 1 1 d . . . C35 C 0.9276(6) 0.0345(4) 0.0192(4) 0.057(4) Uani 1 1 d . . . C38 C 0.9432(7) 0.0169(4) 0.0612(4) 0.077(5) Uani 1 1 d . . . H18A H 0.9823 0.0276 0.0775 0.116 Uiso 1 1 calc R . . H18B H 0.9434 -0.0155 0.0605 0.116 Uiso 1 1 calc R . . H18C H 0.9141 0.0271 0.0732 0.116 Uiso 1 1 calc R . . C40 C 1.0002(7) 0.1950(5) 0.0365(4) 0.073(5) Uani 1 1 d . . . H100 H 1.0182 0.2001 0.0646 0.088 Uiso 1 1 calc R . . C34 C 0.4815(8) 0.2850(6) -0.0053(5) 0.082(5) Uani 1 1 d . . . C36 C 0.9211(6) 0.0109(5) -0.0160(4) 0.060(4) Uani 1 1 d . . . H19 H 0.9272 -0.0200 -0.0176 0.072 Uiso 1 1 calc R . . O11 O 0.8269(6) 0.4886(4) 0.0931(5) 0.146(6) Uani 1 1 d U . . O12 O 0.8830(6) 0.4553(5) 0.1493(5) 0.174(8) Uani 1 1 d U . . C37 C 0.9039(6) 0.0401(4) -0.0485(4) 0.063(4) Uani 1 1 d . . . O14 O 0.4036(8) 0.2457(7) -0.0471(5) 0.212(10) Uani 1 1 d U . . N20 N 0.8392(8) 0.4567(5) 0.1206(6) 0.128(6) Uani 1 1 d U . . N22 N 0.4319(9) 0.2566(7) -0.0142(6) 0.150(8) Uani 1 1 d U . . C39 C 0.8853(7) 0.0330(5) -0.0958(4) 0.077(5) Uani 1 1 d . . . H21A H 0.8653 0.0595 -0.1098 0.116 Uiso 1 1 calc R . . H21B H 0.8585 0.0076 -0.1037 0.116 Uiso 1 1 calc R . . H21C H 0.9205 0.0273 -0.1031 0.116 Uiso 1 1 calc R . . O7 O 0.7777(3) 0.2796(2) 0.1196(2) 0.040(2) Uani 1 1 d . . . H4 H 0.7922 0.2895 0.0991 0.048 Uiso 1 1 calc R . . N5 N 0.7212(8) 0.0281(6) 0.0532(6) 0.114(6) Uani 1 1 d U . . O13 O 0.4287(10) 0.2354(7) 0.0157(5) 0.221(10) Uani 1 1 d U . . O3 O 0.7126(7) 0.0021(5) 0.0216(5) 0.166(7) Uani 1 1 d U . . O2 O 0.6891(7) 0.0286(5) 0.0740(6) 0.155(7) Uani 1 1 d U . . N27 N 0.0227(16) 0.4144(12) 0.2533(12) 0.132(13) Uiso 0.50 1 d PD A -1 O16 O 0.0739(18) 0.4269(19) 0.2532(16) 0.27(2) Uiso 0.50 1 d PD A -1 O17 O 0.017(4) 0.4564(14) 0.245(2) 0.31(3) Uiso 0.50 1 d PD A -1 N26 N 0.4717(9) 0.0315(7) 0.9015(6) 0.153 Uiso 1 1 d D . . C49 C 0.4573(11) 0.0384(7) 0.9389(7) 0.178 Uiso 1 1 d D . . H49A H 0.4386 0.0107 0.9437 0.214 Uiso 1 1 calc R . . H49B H 0.4953 0.0411 0.9613 0.214 Uiso 1 1 calc R . . C52 C 0.3704(18) 0.1236(10) 0.9863(12) 0.326 Uiso 1 1 d D . . H52A H 0.3995 0.1458 1.0006 0.489 Uiso 1 1 calc R . . H52B H 0.3492 0.1131 1.0040 0.489 Uiso 1 1 calc R . . H52C H 0.3424 0.1369 0.9620 0.489 Uiso 1 1 calc R . . C55 C 0.3163(9) 0.0114(7) 0.8178(6) 0.138 Uiso 1 1 d D . . H55A H 0.3312 0.0138 0.7948 0.166 Uiso 1 1 calc R . . H55B H 0.2917 0.0376 0.8179 0.166 Uiso 1 1 calc R . . C56 C 0.2833(9) -0.0290(7) 0.8154(6) 0.152 Uiso 1 1 d D . . H56A H 0.2478 -0.0283 0.7913 0.228 Uiso 1 1 calc R . . H56B H 0.2718 -0.0319 0.8395 0.228 Uiso 1 1 calc R . . H56C H 0.3077 -0.0543 0.8137 0.228 Uiso 1 1 calc R . . C54 C 0.3638(9) 0.0074(7) 0.8553(6) 0.134 Uiso 1 1 d D . . H54A H 0.3790 -0.0232 0.8564 0.160 Uiso 1 1 calc R . . H54B H 0.3463 0.0098 0.8769 0.160 Uiso 1 1 calc R . . C53 C 0.4159(9) 0.0371(8) 0.8667(6) 0.143 Uiso 1 1 d D . . H53A H 0.4008 0.0668 0.8702 0.172 Uiso 1 1 calc R . . H53B H 0.4280 0.0391 0.8425 0.172 Uiso 1 1 calc R . . C41 C 0.5116(9) 0.0690(7) 0.9011(6) 0.137 Uiso 1 1 d D . . H41A H 0.5208 0.0672 0.8757 0.165 Uiso 1 1 calc R . . H41B H 0.4896 0.0968 0.9001 0.165 Uiso 1 1 calc R . . C42 C 0.5675(9) 0.0724(8) 0.9346(6) 0.142 Uiso 1 1 d D . . H42A H 0.5587 0.0713 0.9601 0.171 Uiso 1 1 calc R . . H42B H 0.5913 0.0460 0.9339 0.171 Uiso 1 1 calc R . . C44 C 0.6690(11) 0.1198(9) 0.9560(8) 0.188 Uiso 1 1 d D . . H44A H 0.6790 0.1493 0.9486 0.283 Uiso 1 1 calc R . . H44B H 0.6914 0.0974 0.9471 0.283 Uiso 1 1 calc R . . H44C H 0.6789 0.1180 0.9853 0.283 Uiso 1 1 calc R . . C43 C 0.6037(11) 0.1116(8) 0.9358(8) 0.181 Uiso 1 1 d D . . H43A H 0.5845 0.1353 0.9463 0.217 Uiso 1 1 calc R . . H43B H 0.5961 0.1189 0.9070 0.217 Uiso 1 1 calc R . . C45 C 0.5052(12) -0.0093(8) 0.9127(8) 0.177 Uiso 1 1 d D . . H45A H 0.4826 -0.0298 0.9240 0.213 Uiso 1 1 calc R . . H45B H 0.5424 -0.0024 0.9347 0.213 Uiso 1 1 calc R . . C46 C 0.5209(12) -0.0340(9) 0.8798(8) 0.188 Uiso 1 1 d D . . H46A H 0.5389 -0.0112 0.8674 0.226 Uiso 1 1 calc R . . H46B H 0.4824 -0.0411 0.8592 0.226 Uiso 1 1 calc R . . C47 C 0.5584(12) -0.0753(9) 0.8819(8) 0.183 Uiso 1 1 d D . . H47A H 0.5954 -0.0726 0.9051 0.220 Uiso 1 1 calc R . . H47B H 0.5368 -0.1015 0.8866 0.220 Uiso 1 1 calc R . . C48 C 0.5725(12) -0.0823(9) 0.8457(8) 0.192 Uiso 1 1 d D . . H48A H 0.5983 -0.1081 0.8492 0.287 Uiso 1 1 calc R . . H48B H 0.5926 -0.0561 0.8403 0.287 Uiso 1 1 calc R . . H48C H 0.5361 -0.0873 0.8229 0.287 Uiso 1 1 calc R . . C50 C 0.4208 0.0741 0.9432 0.658 Uiso 1 1 d D . . H50A H 0.3845 0.0711 0.9194 0.789 Uiso 1 1 calc R . . H50B H 0.4408 0.1009 0.9379 0.789 Uiso 1 1 calc R . . C51 C 0.3995(6) 0.0875(4) 0.9753(3) 0.050 Uiso 1 1 d D . . H51A H 0.3740 0.0623 0.9766 0.060 Uiso 1 1 calc R . . H51B H 0.4351 0.0842 0.9994 0.060 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 0.0432(12) 0.0278(9) 0.0480(10) -0.0050(8) 0.0033(8) 0.0064(8) Co2 0.0475(12) 0.0268(9) 0.0505(10) -0.0019(8) 0.0088(9) 0.0043(8) Co3 0.0471(12) 0.0345(10) 0.0522(11) 0.0007(8) 0.0163(9) 0.0081(9) Co5 0.0510(13) 0.0370(10) 0.0455(10) -0.0053(8) 0.0049(9) 0.0083(9) Co4 0.0549(13) 0.0386(10) 0.0439(10) -0.0042(8) 0.0112(9) 0.0118(9) N1 0.065(8) 0.026(5) 0.045(6) 0.005(5) 0.012(6) 0.011(5) N4 0.060(8) 0.019(5) 0.046(7) -0.010(5) -0.036(6) 0.015(5) O4 0.052(6) 0.043(5) 0.041(5) -0.007(4) 0.008(4) -0.002(4) C16 0.019(8) 0.048(8) 0.051(8) -0.011(6) 0.000(6) 0.003(6) O10 0.061(6) 0.034(5) 0.047(5) -0.010(4) 0.001(4) 0.006(4) O1 0.051(6) 0.018(4) 0.069(6) -0.004(4) 0.015(5) -0.001(4) N8 0.091(10) 0.028(6) 0.035(6) 0.004(5) 0.008(6) 0.025(6) C14 0.038(9) 0.035(8) 0.043(7) -0.005(6) 0.009(7) -0.010(7) O6 0.080(8) 0.081(8) 0.111(9) -0.007(7) 0.051(7) -0.032(7) N14 0.067(8) 0.049(7) 0.035(6) 0.008(5) 0.016(5) 0.049(7) N19 0.042(7) 0.048(6) 0.029(5) 0.007(5) 0.007(5) 0.019(6) N13 0.038(7) 0.058(7) 0.037(6) 0.001(5) 0.023(5) 0.006(6) N12 0.054(8) 0.058(7) 0.025(6) 0.013(5) 0.005(5) 0.022(6) C10 0.060(10) 0.059(10) 0.033(7) 0.003(6) 0.021(7) 0.006(7) N10 0.066(10) 0.059(9) 0.059(8) -0.007(6) 0.022(7) -0.019(8) N16 0.059(9) 0.065(8) 0.049(7) 0.000(6) 0.018(6) 0.007(7) N3 0.064(9) 0.024(6) 0.065(8) -0.004(6) -0.002(6) 0.005(6) N17 0.054(8) 0.064(7) 0.040(6) -0.002(6) -0.001(6) 0.020(6) N11 0.046(7) 0.049(7) 0.055(7) 0.008(6) 0.010(6) 0.024(6) C1 0.021(8) 0.049(8) 0.040(8) -0.010(6) -0.016(7) -0.012(6) C6 0.048(10) 0.050(9) 0.073(10) -0.011(7) 0.027(8) -0.018(8) N2 0.032(7) 0.036(6) 0.054(7) 0.000(5) -0.006(6) 0.015(5) N9 0.044(8) 0.048(7) 0.039(6) -0.002(5) -0.001(5) 0.008(6) C32 0.058(11) 0.041(9) 0.069(9) -0.002(7) -0.002(8) 0.001(8) O5 0.161(12) 0.042(6) 0.128(10) -0.027(7) 0.057(9) -0.042(7) C11 0.044(9) 0.019(7) 0.081(10) 0.006(7) -0.002(8) -0.007(6) C8 0.063(11) 0.049(9) 0.045(8) -0.008(7) 0.011(8) 0.011(8) C23 0.084(14) 0.051(10) 0.102(12) 0.004(9) 0.040(11) 0.005(10) N18 0.054(8) 0.031(6) 0.045(6) -0.002(5) 0.010(6) 0.002(6) C18 0.070(11) 0.062(10) 0.045(8) -0.017(7) -0.005(8) -0.005(8) N7 0.054(8) 0.035(6) 0.066(7) -0.010(6) 0.009(6) 0.005(6) C2 0.021(8) 0.069(10) 0.064(10) -0.007(7) 0.007(7) 0.017(7) C9 0.049(9) 0.059(10) 0.049(8) 0.000(7) 0.024(7) 0.013(7) C4 0.042(9) 0.052(8) 0.061(9) -0.009(7) -0.022(7) 0.001(7) C17 0.090(13) 0.052(9) 0.043(8) -0.006(7) -0.002(8) 0.030(9) C3 0.072(12) 0.040(8) 0.048(9) -0.012(6) 0.014(9) 0.010(8) C30 0.054(10) 0.036(8) 0.050(8) 0.002(6) -0.015(7) -0.008(7) C25 0.060(12) 0.067(10) 0.113(14) -0.006(9) 0.054(11) 0.026(9) C26 0.048(10) 0.096(12) 0.069(10) -0.003(9) 0.036(8) 0.035(9) N6 0.057(8) 0.048(7) 0.045(6) -0.003(5) 0.022(6) 0.000(6) C20 0.122(16) 0.099(13) 0.057(9) -0.038(9) -0.034(9) 0.061(11) C19 0.064(11) 0.045(9) 0.060(9) 0.017(7) 0.024(9) 0.025(7) C13 0.063(11) 0.028(8) 0.125(13) 0.026(8) -0.009(10) 0.005(7) C15 0.076(12) 0.037(8) 0.028(7) 0.007(6) 0.012(7) -0.007(8) C12 0.087(13) 0.084(11) 0.062(10) 0.017(8) 0.020(9) -0.003(9) O8 0.024(8) 0.122(12) 0.40(3) 0.043(14) 0.042(12) -0.002(8) C27 0.085(13) 0.067(10) 0.067(10) -0.016(8) 0.043(10) 0.004(9) C7 0.131(16) 0.032(8) 0.073(11) -0.033(8) 0.036(11) -0.032(10) O9 0.098(11) 0.060(9) 0.36(2) 0.024(11) 0.101(13) -0.008(8) C22 0.045(11) 0.069(11) 0.089(11) 0.029(8) 0.042(9) 0.029(8) C31 0.058(11) 0.039(9) 0.112(13) 0.012(9) 0.017(10) 0.014(8) C24 0.026(9) 0.031(8) 0.116(12) 0.018(8) -0.009(9) 0.004(7) C21 0.077(12) 0.079(11) 0.055(9) -0.009(8) 0.019(8) 0.013(9) C28 0.052(10) 0.071(10) 0.081(10) 0.011(8) 0.022(8) 0.020(8) C29 0.119(15) 0.140(16) 0.065(10) 0.054(11) 0.058(10) 0.085(13) N15 0.091(15) 0.062(11) 0.24(2) -0.004(12) 0.073(14) 0.001(11) C5 0.068(11) 0.070(10) 0.071(10) -0.024(8) -0.001(8) 0.020(8) O15 0.036(5) 0.034(5) 0.084(6) 0.001(4) 0.009(5) -0.001(4) N23 0.036(7) 0.054(7) 0.042(7) -0.002(5) -0.002(5) 0.011(5) N25 0.050(8) 0.046(6) 0.046(7) -0.001(5) -0.017(6) -0.002(6) N21 0.036(7) 0.052(7) 0.074(9) 0.007(6) 0.005(6) -0.020(6) C33 0.097(14) 0.094(12) 0.026(8) 0.002(8) 0.015(9) 0.004(11) N24 0.048(8) 0.081(9) 0.041(7) 0.012(6) 0.002(6) 0.030(6) C35 0.074(11) 0.044(8) 0.030(8) -0.001(7) -0.015(7) 0.022(7) C38 0.111(14) 0.029(8) 0.080(11) 0.000(7) 0.018(10) 0.028(8) C40 0.066(11) 0.088(11) 0.042(9) -0.036(9) -0.012(8) 0.000(9) C34 0.104(15) 0.082(12) 0.063(11) 0.006(9) 0.033(11) -0.027(11) C36 0.076(11) 0.052(8) 0.029(7) 0.016(7) -0.011(7) 0.019(8) O11 0.095(10) 0.081(9) 0.217(15) 0.039(10) -0.006(10) -0.046(8) O12 0.093(11) 0.131(12) 0.186(14) 0.034(10) -0.099(10) -0.065(9) C37 0.043(9) 0.042(8) 0.087(11) -0.041(8) 0.000(8) 0.018(7) O14 0.180(17) 0.28(2) 0.108(11) -0.026(13) -0.045(11) -0.172(15) N20 0.098(14) 0.054(9) 0.180(17) 0.028(10) -0.022(12) -0.041(9) N22 0.161(18) 0.184(18) 0.112(15) -0.012(13) 0.057(14) -0.139(15) C39 0.117(14) 0.055(9) 0.073(10) -0.015(8) 0.048(10) 0.023(9) O7 0.047(5) 0.032(4) 0.045(5) 0.003(4) 0.022(4) 0.011(4) N5 0.115(15) 0.087(11) 0.139(15) -0.037(11) 0.040(11) -0.068(11) O13 0.30(2) 0.24(2) 0.142(14) -0.040(13) 0.095(15) -0.205(18) O3 0.202(16) 0.113(11) 0.192(15) -0.082(11) 0.079(12) -0.108(11) O2 0.151(14) 0.124(12) 0.244(18) -0.067(12) 0.138(14) -0.078(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O15 1.856(8) . ? Co1 N25 1.879(11) . ? Co1 N4 1.900(12) . ? Co1 O1 1.905(7) . ? Co1 N23 1.950(10) . ? Co1 N2 1.950(10) . ? Co2 O4 1.868(8) . ? Co2 N9 1.895(10) . ? Co2 O1 1.897(8) . ? Co2 N7 1.908(11) . ? Co2 N1 1.935(10) . ? Co2 N3 1.943(11) . ? Co3 O7 1.851(7) . ? Co3 N8 1.858(12) . ? Co3 N14 1.905(12) . ? Co3 O4 1.907(7) . ? Co3 N12 1.927(10) . ? Co3 N6 1.939(10) . ? Co5 O10 1.860(7) . ? Co5 O15 1.868(9) 7_655 ? Co5 N18 1.881(10) . ? Co5 N21 1.892(10) . ? Co5 N24 1.972(11) 7_655 ? Co5 N16 1.984(11) . ? Co4 O10 1.862(7) . ? Co4 O7 1.896(7) . ? Co4 N19 1.910(10) . ? Co4 N17 1.916(11) . ? Co4 N13 1.932(10) . ? Co4 N11 1.957(10) . ? N1 C1 1.348(14) . ? N1 N2 1.365(12) . ? N4 C8 1.295(15) . ? N4 N3 1.392(14) . ? C16 N9 1.317(14) . ? C16 C15 1.410(16) . ? N8 C14 1.362(14) . ? N8 N9 1.419(13) . ? C14 C15 1.311(16) . ? O6 N10 1.262(13) . ? N14 N13 1.353(12) . ? N14 C24 1.379(15) . ? N19 C32 1.355(15) . ? N19 N18 1.373(12) . ? N13 C22 1.333(15) . ? N12 N11 1.335(12) . ? N12 C19 1.390(16) . ? C10 C11 1.351(16) . ? C10 C9 1.415(17) . ? N10 O5 1.220(13) . ? N10 C15 1.456(17) . ? N16 C25 1.296(15) . ? N16 N17 1.411(13) . ? N3 C6 1.327(15) . ? N17 C27 1.429(16) . ? N11 C17 1.371(15) . ? C1 C2 1.344(16) . ? C1 C4 1.475(16) . ? C6 C7 1.399(17) . ? N2 C3 1.310(15) . ? C32 C31 1.367(18) . ? C11 N7 1.375(15) . ? C11 C13 1.605(19) . ? C8 C7 1.372(18) . ? C23 C24 1.315(19) . ? C23 C22 1.382(18) . ? C23 N15 1.48(2) . ? N18 C30 1.324(14) . ? C18 C17 1.372(17) . ? C18 C19 1.389(17) . ? N7 N6 1.426(13) . ? C2 C3 1.368(16) . ? C9 N6 1.296(14) . ? C9 C12 1.509(17) . ? C17 C20 1.547(18) . ? C3 C5 1.547(17) . ? C30 C31 1.407(18) . ? C25 C26 1.455(19) . ? C25 C28 1.550(19) . ? C26 C27 1.395(18) . ? C19 C21 1.473(17) . ? O8 N15 1.207(17) . ? C27 C29 1.454(19) . ? C7 N5 1.41(2) . ? O9 N15 1.255(17) . ? C31 N20 1.453(19) . ? O15 Co5 1.868(9) 7_655 ? N23 C35 1.346(14) . ? N23 N24 1.352(13) . ? N25 C40 1.354(16) . ? N25 N21 1.369(13) 7_655 ? N21 C33 1.290(17) . ? N21 N25 1.369(13) 7_655 ? C33 C34 1.37(2) . ? N24 C37 1.344(15) . ? N24 Co5 1.972(11) 7_655 ? C35 C36 1.363(16) . ? C35 C38 1.463(17) . ? C40 C34 1.412(19) 7_655 ? C34 N22 1.39(2) . ? C34 C40 1.412(19) 7_655 ? C36 C37 1.365(17) . ? O11 N20 1.301(18) . ? O12 N20 1.168(17) . ? C37 C39 1.554(18) . ? O14 N22 1.152(18) . ? N22 O13 1.232(19) . ? N5 O2 1.206(17) . ? N5 O3 1.291(19) . ? N27 O16 1.267(19) . ? N27 O17 1.27(2) . ? N26 C45 1.427(16) . ? N26 C49 1.451(16) . ? N26 C41 1.459(16) . ? N26 C53 1.462(16) . ? C49 C50 1.404(13) . ? C52 C51 1.390(13) . ? C55 C54 1.404(16) . ? C55 C56 1.417(16) . ? C54 C53 1.455(16) . ? C41 C42 1.434(16) . ? C42 C43 1.433(17) . ? C44 C43 1.484(17) . ? C45 C46 1.496(17) . ? C46 C47 1.499(17) . ? C47 C48 1.410(16) . ? C50 C51 1.417(10) . ? 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 O15 Co1 N25 86.0(4) . . ? O15 Co1 N4 90.4(4) . . ? N25 Co1 N4 175.6(4) . . ? O15 Co1 O1 91.9(3) . . ? N25 Co1 O1 89.9(4) . . ? N4 Co1 O1 87.8(4) . . ? O15 Co1 N23 84.2(4) . . ? N25 Co1 N23 92.4(5) . . ? N4 Co1 N23 89.7(4) . . ? O1 Co1 N23 175.3(4) . . ? O15 Co1 N2 174.9(4) . . ? N25 Co1 N2 91.5(5) . . ? N4 Co1 N2 91.9(4) . . ? O1 Co1 N2 83.7(4) . . ? N23 Co1 N2 100.3(4) . . ? O4 Co2 N9 88.4(4) . . ? O4 Co2 O1 93.5(3) . . ? N9 Co2 O1 88.7(4) . . ? O4 Co2 N7 84.6(4) . . ? N9 Co2 N7 93.6(4) . . ? O1 Co2 N7 176.9(4) . . ? O4 Co2 N1 177.2(4) . . ? N9 Co2 N1 89.3(4) . . ? O1 Co2 N1 84.9(4) . . ? N7 Co2 N1 97.2(4) . . ? O4 Co2 N3 88.1(4) . . ? N9 Co2 N3 174.5(4) . . ? O1 Co2 N3 87.2(4) . . ? N7 Co2 N3 90.3(5) . . ? N1 Co2 N3 94.1(5) . . ? O7 Co3 N8 88.2(4) . . ? O7 Co3 N14 88.2(4) . . ? N8 Co3 N14 175.1(4) . . ? O7 Co3 O4 91.0(3) . . ? N8 Co3 O4 88.1(4) . . ? N14 Co3 O4 88.7(4) . . ? O7 Co3 N12 82.7(3) . . ? N8 Co3 N12 90.2(4) . . ? N14 Co3 N12 92.6(4) . . ? O4 Co3 N12 173.5(4) . . ? O7 Co3 N6 174.5(4) . . ? N8 Co3 N6 93.6(4) . . ? N14 Co3 N6 89.7(4) . . ? O4 Co3 N6 83.8(4) . . ? N12 Co3 N6 102.5(4) . . ? O10 Co5 O15 91.0(3) . 7_655 ? O10 Co5 N18 86.8(4) . . ? O15 Co5 N18 90.9(4) 7_655 . ? O10 Co5 N21 91.4(4) . . ? O15 Co5 N21 86.3(5) 7_655 . ? N18 Co5 N21 176.6(5) . . ? O10 Co5 N24 175.9(4) . 7_655 ? O15 Co5 N24 85.2(4) 7_655 7_655 ? N18 Co5 N24 91.8(4) . 7_655 ? N21 Co5 N24 89.8(5) . 7_655 ? O10 Co5 N16 84.0(4) . . ? O15 Co5 N16 174.7(4) 7_655 . ? N18 Co5 N16 90.6(5) . . ? N21 Co5 N16 92.1(5) . . ? N24 Co5 N16 99.9(5) 7_655 . ? O10 Co4 O7 89.9(3) . . ? O10 Co4 N19 88.2(4) . . ? O7 Co4 N19 88.2(4) . . ? O10 Co4 N17 84.9(4) . . ? O7 Co4 N17 174.8(4) . . ? N19 Co4 N17 91.8(4) . . ? O10 Co4 N13 89.0(4) . . ? O7 Co4 N13 87.6(4) . . ? N19 Co4 N13 174.9(4) . . ? N17 Co4 N13 92.1(5) . . ? O10 Co4 N11 173.1(4) . . ? O7 Co4 N11 83.3(4) . . ? N19 Co4 N11 90.7(4) . . ? N17 Co4 N11 101.9(4) . . ? N13 Co4 N11 91.7(4) . . ? C1 N1 N2 108.3(10) . . ? C1 N1 Co2 133.9(9) . . ? N2 N1 Co2 116.4(8) . . ? C8 N4 N3 105.9(12) . . ? C8 N4 Co1 133.9(11) . . ? N3 N4 Co1 118.7(8) . . ? Co2 O4 Co3 110.4(4) . . ? N9 C16 C15 105.2(11) . . ? Co5 O10 Co4 112.6(4) . . ? Co2 O1 Co1 110.1(4) . . ? C14 N8 N9 104.7(11) . . ? C14 N8 Co3 137.4(9) . . ? N9 N8 Co3 117.3(8) . . ? C15 C14 N8 109.7(12) . . ? N13 N14 C24 106.6(11) . . ? N13 N14 Co3 117.6(9) . . ? C24 N14 Co3 135.4(9) . . ? C32 N19 N18 110.1(10) . . ? C32 N19 Co4 135.6(8) . . ? N18 N19 Co4 113.9(8) . . ? C22 N13 N14 110.9(11) . . ? C22 N13 Co4 131.3(9) . . ? N14 N13 Co4 116.3(9) . . ? N11 N12 C19 108.4(10) . . ? N11 N12 Co3 119.2(7) . . ? C19 N12 Co3 131.7(8) . . ? C11 C10 C9 103.4(11) . . ? O5 N10 O6 122.9(13) . . ? O5 N10 C15 118.6(13) . . ? O6 N10 C15 118.2(12) . . ? C25 N16 N17 111.2(11) . . ? C25 N16 Co5 133.6(11) . . ? N17 N16 Co5 113.9(9) . . ? C6 N3 N4 110.9(10) . . ? C6 N3 Co2 134.5(10) . . ? N4 N3 Co2 114.4(9) . . ? N16 N17 C27 105.0(11) . . ? N16 N17 Co4 117.3(8) . . ? C27 N17 Co4 135.4(9) . . ? N12 N11 C17 110.0(10) . . ? N12 N11 Co4 114.6(8) . . ? C17 N11 Co4 134.4(9) . . ? C2 C1 N1 107.2(11) . . ? C2 C1 C4 129.2(12) . . ? N1 C1 C4 123.5(12) . . ? N3 C6 C7 105.6(13) . . ? C3 N2 N1 107.9(10) . . ? C3 N2 Co1 133.8(10) . . ? N1 N2 Co1 117.2(8) . . ? C16 N9 N8 110.6(10) . . ? C16 N9 Co2 132.5(9) . . ? N8 N9 Co2 115.9(9) . . ? N19 C32 C31 107.4(12) . . ? C10 C11 N7 112.8(12) . . ? C10 C11 C13 132.9(12) . . ? N7 C11 C13 114.0(12) . . ? N4 C8 C7 111.1(13) . . ? C24 C23 C22 111.3(15) . . ? C24 C23 N15 127.8(15) . . ? C22 C23 N15 120.9(16) . . ? C30 N18 N19 106.6(10) . . ? C30 N18 Co5 132.6(8) . . ? N19 N18 Co5 120.2(8) . . ? C17 C18 C19 108.6(12) . . ? C11 N7 N6 103.7(10) . . ? C11 N7 Co2 138.8(9) . . ? N6 N7 Co2 116.3(7) . . ? C1 C2 C3 107.9(12) . . ? N6 C9 C10 111.4(11) . . ? N6 C9 C12 124.4(12) . . ? C10 C9 C12 124.2(13) . . ? N11 C17 C18 106.8(11) . . ? N11 C17 C20 122.9(12) . . ? C18 C17 C20 130.3(12) . . ? N2 C3 C2 108.6(12) . . ? N2 C3 C5 125.0(12) . . ? C2 C3 C5 126.3(14) . . ? N18 C30 C31 109.8(12) . . ? N16 C25 C26 109.9(13) . . ? N16 C25 C28 126.2(14) . . ? C26 C25 C28 123.8(13) . . ? C27 C26 C25 104.7(12) . . ? C9 N6 N7 108.7(10) . . ? C9 N6 Co3 134.4(9) . . ? N7 N6 Co3 115.3(7) . . ? C18 C19 N12 106.3(11) . . ? C18 C19 C21 127.0(13) . . ? N12 C19 C21 126.6(12) . . ? C14 C15 C16 109.8(13) . . ? C14 C15 N10 126.3(13) . . ? C16 C15 N10 123.8(14) . . ? C26 C27 N17 109.2(13) . . ? C26 C27 C29 130.0(14) . . ? N17 C27 C29 120.7(14) . . ? C8 C7 C6 106.5(13) . . ? C8 C7 N5 131.6(15) . . ? C6 C7 N5 121.7(16) . . ? N13 C22 C23 104.4(13) . . ? C32 C31 C30 106.1(13) . . ? C32 C31 N20 121.7(15) . . ? C30 C31 N20 132.1(14) . . ? C23 C24 N14 106.6(12) . . ? O8 N15 O9 128.1(18) . . ? O8 N15 C23 120.4(16) . . ? O9 N15 C23 111.4(16) . . ? Co1 O15 Co5 112.6(4) . 7_655 ? C35 N23 N24 108.3(10) . . ? C35 N23 Co1 132.2(9) . . ? N24 N23 Co1 118.4(8) . . ? C40 N25 N21 106.8(11) . 7_655 ? C40 N25 Co1 136.3(10) . . ? N21 N25 Co1 116.9(8) 7_655 . ? C33 N21 N25 107.5(11) . 7_655 ? C33 N21 Co5 133.7(11) . . ? N25 N21 Co5 117.5(9) 7_655 . ? N21 C33 C34 114.1(13) . . ? C37 N24 N23 109.1(11) . . ? C37 N24 Co5 134.4(9) . 7_655 ? N23 N24 Co5 114.5(8) . 7_655 ? N23 C35 C36 107.2(11) . . ? N23 C35 C38 125.0(11) . . ? C36 C35 C38 127.8(12) . . ? N25 C40 C34 110.0(12) . 7_655 ? C33 C34 N22 136.4(17) . . ? C33 C34 C40 101.3(14) . 7_655 ? N22 C34 C40 122.3(16) . 7_655 ? C35 C36 C37 108.5(12) . . ? N24 C37 C36 106.8(12) . . ? N24 C37 C39 120.7(12) . . ? C36 C37 C39 132.5(11) . . ? O12 N20 O11 124.1(15) . . ? O12 N20 C31 123.9(16) . . ? O11 N20 C31 111.9(15) . . ? O14 N22 O13 120.2(18) . . ? O14 N22 C34 123.8(18) . . ? O13 N22 C34 114.0(19) . . ? Co3 O7 Co4 111.2(4) . . ? O2 N5 O3 123.8(16) . . ? O2 N5 C7 122.4(17) . . ? O3 N5 C7 113.8(17) . . ? O16 N27 O17 75(4) . . ? C45 N26 C49 98.7(16) . . ? C45 N26 C41 110(2) . . ? C49 N26 C41 104(2) . . ? C45 N26 C53 126(2) . . ? C49 N26 C53 107.3(19) . . ? C41 N26 C53 108.3(17) . . ? C50 C49 N26 122.2(18) . . ? C54 C55 C56 103.7(17) . . ? C55 C54 C53 122.8(19) . . ? C54 C53 N26 126.9(19) . . ? C42 C41 N26 118.0(19) . . ? C43 C42 C41 117(2) . . ? C42 C43 C44 131(2) . . ? N26 C45 C46 118(2) . . ? C45 C46 C47 131(2) . . ? C48 C47 C46 113(2) . . ? C49 C50 C51 133.2(11) . . ? C52 C51 C50 140.0(19) . . ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 23.76 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 1.449 _refine_diff_density_min -2.062 _refine_diff_density_rms 0.146 # Attachment 'Co12.cif' data_co12 _database_code_depnum_ccdc_archive 'CCDC 750244' #TrackingRef 'Co12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C176 H198 Co12 N64 O43 P4' _chemical_formula_weight 4729.02 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' 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' P P 0.1023 0.0942 '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' H H 0.0000 0.0000 '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 18.694(4) _cell_length_b 19.172(4) _cell_length_c 35.964(7) _cell_angle_alpha 83.77(3) _cell_angle_beta 86.82(3) _cell_angle_gamma 70.93(3) _cell_volume 12108(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20927 _cell_measurement_theta_min 3.1858 _cell_measurement_theta_max 28.5976 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4082 _exptl_crystal_size_mid 0.3092 _exptl_crystal_size_min 0.1448 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4860 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7081 _exptl_absorpt_correction_T_max 0.8838 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The low completeness of the data set reulted due to poor diffraction of the crystal. Several crystallisation effort didn't afforded any better crystals. Theta max used for this data set was 28.66. Lowering the theta max value did not improve the completeness. ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Kappa CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean 15.9832 _diffrn_reflns_number 105317 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.1711 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 28.66 _reflns_number_total 52366 _reflns_number_gt 22613 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The ADPs of the atoms namely, O11, O12, O19, N20 are restrained using SIMU. The large ADP ratio of N21 and N23 atoms could not be restrained applying any thermal restrains. Some thermal ellipsoids resulted in the disordered counter ions,which in some cases could not be modeled properly. This in turn also resulted in relatively high R value. After refinement as above, the raw data file was modified by the program SQUEEZE to eliminate unaccounted electron density attributed to interstitial solvent molecules that were not located in the difference map. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.498 1.000 0.000 1432 207 ' ' 2 0.037 0.500 0.500 1112 144 ' ' 3 0.042 0.906 0.411 6 1 ' ' 4 0.056 0.512 0.261 7 1 ' ' 5 0.071 0.971 0.443 13 2 ' ' 6 0.167 0.833 0.694 7 0 ' ' 7 0.269 0.573 0.825 87 15 ' ' 8 0.731 0.427 0.175 87 14 ' ' 9 0.833 0.167 0.306 7 0 ' ' 10 0.930 0.032 0.558 13 2 ' ' 11 0.943 0.488 0.739 8 2 ' ' 12 0.961 0.099 0.590 7 1 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1812P)^2^+0.0200P] 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 52366 _refine_ls_number_parameters 2418 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.3168 _refine_ls_wR_factor_gt 0.2934 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 2.122 _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 O41 O 0.2591(14) 0.8016(12) 0.7559(6) 0.110 Uiso 1 1 d D A 1 Co1 Co 0.18090(12) 1.09978(11) 0.81564(6) 0.024 Uani 1 1 d . B 1 Co2 Co 0.35236(12) 1.02084(12) 0.83109(6) 0.025 Uani 1 1 d . B 1 Co3 Co 0.49419(13) 0.87914(12) 0.82704(6) 0.026 Uani 1 1 d . B 1 Co4 Co 0.57341(13) 0.71510(12) 0.80887(7) 0.028 Uani 1 1 d . B 1 Co5 Co 0.57365(14) 0.57250(12) 0.77471(9) 0.041 Uani 1 1 d . B 1 Co6 Co 0.49104(15) 0.49403(12) 0.72915(10) 0.049 Uani 1 1 d . B 1 Co7 Co 0.34195(14) 0.49684(12) 0.69363(9) 0.044 Uani 1 1 d . B 1 Co8 Co 0.17220(14) 0.58029(12) 0.67549(8) 0.035 Uani 1 1 d . B 1 Co9 Co 0.03052(13) 0.72272(11) 0.67784(7) 0.027 Uani 1 1 d . B 1 Co10 Co -0.05321(12) 0.88205(11) 0.70094(6) 0.024 Uani 1 1 d . B 1 Co11 Co -0.05656(12) 1.02073(11) 0.74015(6) 0.025 Uani 1 1 d . B 1 Co12 Co 0.02919(12) 1.09792(11) 0.78480(6) 0.025 Uani 1 1 d . B 1 O1 O 0.2554(6) 1.0070(6) 0.8301(3) 0.028 Uani 1 1 d . B 1 H51B H 0.2463 0.9621 0.8357 0.034 Uiso 1 1 calc R B 1 O2 O 0.4026(7) 1.1316(7) 0.6803(3) 0.039 Uani 1 1 d . B 1 O3 O 0.2820(8) 1.1843(7) 0.6681(3) 0.042 Uani 1 1 d . B 1 O4 O 0.4038(6) 0.9389(5) 0.8031(3) 0.020 Uani 1 1 d . B 1 H50A H 0.3869 0.9297 0.7809 0.023 Uiso 1 1 calc R B 1 O5 O 0.4029(14) 0.7940(12) 0.9769(5) 0.115 Uani 1 1 d . C 1 O6 O 0.3128(12) 0.8952(11) 0.9809(5) 0.090 Uani 1 1 d . C 1 O7 O 0.4800(6) 0.7854(6) 0.8253(3) 0.028 Uani 1 1 d . B 1 H50B H 0.4352 0.7751 0.8314 0.034 Uiso 1 1 calc R B 1 O8 O 0.5801(10) 0.8276(7) 0.6588(4) 0.057 Uani 1 1 d . B 1 O9 O 0.5227(8) 0.9431(7) 0.6679(4) 0.047 Uani 1 1 d . B 1 O10 O 0.5325(6) 0.6779(5) 0.7702(3) 0.031 Uani 1 1 d . B 1 H50C H 0.4983 0.7066 0.7524 0.037 Uiso 1 1 calc R B 1 O11 O 0.4503(16) 0.5002(15) 0.9185(7) 0.141 Uani 1 1 d U B 1 O12 O 0.4655(16) 0.5899(15) 0.9456(8) 0.141 Uani 1 1 d U B 1 O13 O 0.4797(7) 0.5599(6) 0.7669(4) 0.043 Uani 1 1 d . B 1 H50D H 0.4346 0.5824 0.7795 0.052 Uiso 1 1 calc R B 1 O14 O 0.6167(12) 0.6262(11) 0.5980(6) 0.093 Uani 1 1 d . B 1 O15 O 0.6927(12) 0.6614(11) 0.6314(6) 0.091 Uani 1 1 d . B 1 O16 O 0.3993(8) 0.5552(6) 0.7069(4) 0.046 Uani 1 1 d . B 1 H50E H 0.3846 0.6066 0.7031 0.055 Uiso 1 1 calc R B 1 O17 O 0.2928(16) 0.3399(14) 0.8357(7) 0.141 Uani 1 1 d . B 1 O18 O 0.3961(13) 0.3418(11) 0.8606(6) 0.100 Uani 1 1 d . B 1 O19 O 0.2499(16) 0.5652(14) 0.7105(8) 0.141 Uani 1 1 d . B 1 H50F H 0.2438 0.5879 0.7326 0.169 Uiso 1 1 calc R B 1 O20 O 0.2888(11) 0.6787(9) 0.5340(5) 0.078 Uani 1 1 d . B 1 O21 O 0.4055(10) 0.6241(9) 0.5467(6) 0.077 Uani 1 1 d . B 1 O22 O 0.1391(6) 0.6859(6) 0.6753(3) 0.031 Uani 1 1 d . B 1 H50G H 0.1707 0.7148 0.6741 0.037 Uiso 1 1 calc R B 1 O23 O -0.0446(11) 0.5796(9) 0.8177(5) 0.072 Uani 1 1 d . B 1 O24 O 0.0508(12) 0.4789(9) 0.8146(5) 0.088 Uani 1 1 d . B 1 O25 O 0.0198(6) 0.7873(6) 0.7161(3) 0.028 Uani 1 1 d . B 1 H50H H 0.0457 0.7750 0.7385 0.034 Uiso 1 1 calc R B 1 O26 O 0.0901(11) 0.9806(9) 0.5695(5) 0.077 Uani 1 1 d . B 1 O27 O 0.1563(11) 0.8712(11) 0.5570(5) 0.082 Uani 1 1 d . B 1 O28 O 0.0037(6) 0.9427(5) 0.7122(3) 0.021 Uani 1 1 d . B 1 H50I H 0.0540 0.9353 0.7051 0.026 Uiso 1 1 calc R B 1 O29 O -0.1639(13) 0.8821(11) 0.8717(5) 0.091 Uani 1 1 d . B 1 O30 O -0.1506(12) 0.7791(11) 0.8479(4) 0.084 Uani 1 1 d . B 1 O31 O 0.0188(6) 1.0060(5) 0.7763(3) 0.025 Uani 1 1 d . B 1 H50J H 0.0464 0.9603 0.7882 0.030 Uiso 1 1 calc R B 1 O32 O 0.0831(10) 1.2426(9) 0.6422(5) 0.067 Uani 1 1 d . B 1 O33 O 0.0366(11) 1.1811(10) 0.6097(5) 0.074 Uani 1 1 d . B 1 O34 O 0.1366(6) 1.0656(5) 0.7782(3) 0.025 Uani 1 1 d . B 1 H51A H 0.1632 1.0373 0.7594 0.030 Uiso 1 1 calc R B 1 O35 O 0.0941(13) 0.9615(13) 0.9533(5) 0.097 Uani 1 1 d . B 1 O36 O -0.0014(11) 0.9444(11) 0.9293(5) 0.085 Uani 1 1 d . B 1 O37 O 0.3927(10) 0.6877(8) 0.6648(6) 0.076 Uani 1 1 d . D 1 O38 O 0.5643(18) 0.1489(13) 0.7127(8) 0.140 Uani 1 1 d . E 1 N1 N 0.2999(8) 1.1011(8) 0.8607(4) 0.030 Uani 1 1 d . B 1 N2 N 0.2232(8) 1.1331(8) 0.8551(4) 0.034 Uani 1 1 d . B 1 N3 N 0.3266(8) 1.0839(7) 0.7851(4) 0.025 Uani 1 1 d . B 1 N4 N 0.2520(8) 1.1169(7) 0.7782(4) 0.030 Uani 1 1 d . B 1 N5 N 0.3339(9) 1.1503(7) 0.6897(4) 0.034 Uani 1 1 d . B 1 N6 N 0.5122(8) 0.9725(8) 0.8258(4) 0.029 Uani 1 1 d . B 1 N7 N 0.4503(8) 1.0353(8) 0.8287(4) 0.030 Uani 1 1 d . B 1 N8 N 0.4392(8) 0.8924(8) 0.8726(4) 0.029 Uani 1 1 d . B 1 N9 N 0.3764(9) 0.9539(8) 0.8750(4) 0.035 Uani 1 1 d . B 1 N11 N 0.6143(8) 0.7492(7) 0.8485(4) 0.033 Uani 1 1 d . B 1 N12 N 0.5842(8) 0.8219(8) 0.8537(4) 0.035 Uani 1 1 d . B 1 N13 N 0.5799(8) 0.7928(7) 0.7720(4) 0.030 Uani 1 1 d . B 1 N14 N 0.5408(8) 0.8630(7) 0.7786(4) 0.032 Uani 1 1 d . B 1 N15 N 0.5541(9) 0.8772(8) 0.6792(4) 0.036 Uani 1 1 d . B 1 N16 N 0.6710(9) 0.5842(8) 0.7793(5) 0.046 Uani 1 1 d . B 1 N17 N 0.6699(8) 0.6508(7) 0.7914(4) 0.035 Uani 1 1 d . B 1 N18 N 0.5483(10) 0.5785(9) 0.8276(5) 0.046 Uani 1 1 d . B 1 N19 N 0.5524(9) 0.6389(8) 0.8423(5) 0.041 Uani 1 1 d . B 1 N20 N 0.4698(14) 0.5550(13) 0.9180(7) 0.091 Uani 1 1 d U B 1 N21 N 0.5786(10) 0.4311(7) 0.7587(6) 0.061 Uani 1 1 d U B 1 N22 N 0.6085(9) 0.4664(8) 0.7819(6) 0.055 Uani 1 1 d U B 1 N23 N 0.5515(8) 0.5459(7) 0.7006(6) 0.046 Uani 1 1 d U B 1 N24 N 0.5925(9) 0.5759(7) 0.7216(5) 0.044 Uani 1 1 d U B 1 N25 N 0.6437(15) 0.6294(11) 0.6292(7) 0.084 Uani 1 1 d . B 1 N26 N 0.4347(10) 0.4327(8) 0.6730(6) 0.056 Uani 1 1 d . B 1 N27 N 0.5020(10) 0.4331(9) 0.6879(6) 0.062 Uani 1 1 d . B 1 N28 N 0.3630(9) 0.4475(8) 0.7430(5) 0.049 Uani 1 1 d . B 1 N29 N 0.4304(9) 0.4459(8) 0.7578(6) 0.052 Uani 1 1 d . B 1 N30 N 0.3514(14) 0.3566(12) 0.8340(7) 0.079 Uani 1 1 d . B 1 N31 N 0.2048(9) 0.4740(8) 0.6783(5) 0.041 Uani 1 1 d . B 1 N32 N 0.2795(9) 0.4379(8) 0.6859(6) 0.054 Uani 1 1 d . B 1 N33 N 0.2466(8) 0.5849(8) 0.6369(5) 0.041 Uani 1 1 d . B 1 N34 N 0.3228(10) 0.5508(8) 0.6446(5) 0.049 Uani 1 1 d . B 1 N35 N 0.3370(12) 0.6387(10) 0.5546(6) 0.063 Uani 1 1 d . B 1 N36 N 0.0393(8) 0.6623(7) 0.6368(4) 0.032 Uani 1 1 d . B 1 N37 N 0.1001(9) 0.5974(7) 0.6369(4) 0.037 Uani 1 1 d . B 1 N38 N 0.0381(8) 0.6422(7) 0.7156(4) 0.031 Uani 1 1 d . B 1 N39 N 0.1001(9) 0.5804(8) 0.7152(4) 0.037 Uani 1 1 d . B 1 N40 N 0.0128(12) 0.5421(10) 0.8020(6) 0.062 Uani 1 1 d . B 1 N41 N -0.1148(8) 0.8227(7) 0.6916(4) 0.028 Uani 1 1 d . B 1 N42 N -0.0785(8) 0.7524(7) 0.6814(4) 0.026 Uani 1 1 d . B 1 N43 N -0.0046(8) 0.8742(7) 0.6533(4) 0.029 Uani 1 1 d . B 1 N44 N 0.0356(9) 0.8030(8) 0.6431(4) 0.036 Uani 1 1 d . B 1 N45 N 0.1087(10) 0.9139(10) 0.5754(5) 0.047 Uani 1 1 d . B 1 N46 N -0.1294(8) 1.0371(7) 0.7017(4) 0.028 Uani 1 1 d . B 1 N47 N -0.1236(8) 0.9752(7) 0.6829(4) 0.028 Uani 1 1 d . B 1 N48 N -0.0937(8) 0.9493(8) 0.7682(4) 0.034 Uani 1 1 d . B 1 N49 N -0.0912(7) 0.8885(7) 0.7514(4) 0.025 Uani 1 1 d . B 1 N50 N -0.1481(11) 0.8403(11) 0.8461(5) 0.059 Uani 1 1 d . B 1 N51 N -0.0789(7) 1.1252(7) 0.7939(4) 0.029 Uani 1 1 d . B 1 N52 N -0.1169(8) 1.0946(7) 0.7722(4) 0.032 Uani 1 1 d . B 1 N53 N 0.0199(8) 1.1260(7) 0.7320(4) 0.027 Uani 1 1 d . B 1 N54 N -0.0139(7) 1.0888(7) 0.7122(4) 0.024 Uani 1 1 d . B 1 N55 N 0.0495(10) 1.1977(9) 0.6392(5) 0.049 Uani 1 1 d . B 1 N56 N 0.1072(8) 1.1937(7) 0.8004(4) 0.031 Uani 1 1 d . B 1 N57 N 0.0382(7) 1.1945(7) 0.7901(4) 0.030 Uani 1 1 d . B 1 N58 N 0.1123(8) 1.0704(7) 0.8503(4) 0.029 Uani 1 1 d . B 1 N59 N 0.0490(8) 1.0643(7) 0.8361(4) 0.030 Uani 1 1 d . B 1 N60 N 0.0511(12) 0.9681(11) 0.9279(5) 0.063 Uani 1 1 d . B 1 N62 N 0.2385(6) 0.8433(6) 0.4513(3) 0.011 Uiso 1 1 d D F 1 N63 N 0.2635(9) 0.0475(8) 0.5420(4) 0.038 Uani 1 1 d . . . N64 N 0.1183(19) 0.6647(14) 0.9646(8) 0.119 Uani 1 1 d . . . C1 C 0.3177(13) 1.1241(12) 0.8920(6) 0.053 Uani 1 1 d . . . C2 C 0.2515(12) 1.1729(11) 0.9067(6) 0.049 Uani 1 1 d . B . H2A H 0.2467 1.1976 0.9280 0.059 Uiso 1 1 calc R . . C3 C 0.1951(12) 1.1765(11) 0.8826(6) 0.045 Uani 1 1 d . . . C4 C 0.3959(14) 1.1001(13) 0.9073(7) 0.063 Uani 1 1 d . B . H4A H 0.4276 1.0584 0.8950 0.095 Uiso 1 1 calc R . . H4B H 0.3939 1.0862 0.9337 0.095 Uiso 1 1 calc R . . H4C H 0.4163 1.1402 0.9029 0.095 Uiso 1 1 calc R . . C5 C 0.1111(15) 1.2213(14) 0.8877(7) 0.069 Uani 1 1 d . B . H5A H 0.0815 1.1883 0.8900 0.104 Uiso 1 1 calc R . . H5B H 0.0948 1.2569 0.8665 0.104 Uiso 1 1 calc R . . H5C H 0.1043 1.2465 0.9099 0.104 Uiso 1 1 calc R . . C6 C 0.3673(9) 1.0925(8) 0.7546(4) 0.024 Uani 1 1 d . . . H6A H 0.4197 1.0751 0.7520 0.028 Uiso 1 1 calc R B 1 C7 C 0.3163(10) 1.1325(9) 0.7276(5) 0.028 Uani 1 1 d . B . C8 C 0.2433(9) 1.1458(8) 0.7437(4) 0.023 Uani 1 1 d . . . H8 H 0.1976 1.1705 0.7319 0.028 Uiso 1 1 calc R B 1 C9 C 0.5729(10) 0.9939(10) 0.8172(5) 0.037 Uani 1 1 d . . . C10 C 0.5500(11) 1.0711(10) 0.8138(6) 0.043 Uani 1 1 d . B . H10 H 0.5804 1.1007 0.8078 0.052 Uiso 1 1 calc R . . C11 C 0.4732(11) 1.0946(10) 0.8212(6) 0.040 Uani 1 1 d . . . C12 C 0.6507(12) 0.9427(12) 0.8099(7) 0.052 Uani 1 1 d . B . H12A H 0.6873 0.9605 0.8199 0.078 Uiso 1 1 calc R . . H12B H 0.6593 0.9406 0.7834 0.078 Uiso 1 1 calc R . . H12C H 0.6555 0.8940 0.8216 0.078 Uiso 1 1 calc R . . C13 C 0.4220(13) 1.1732(11) 0.8196(7) 0.056 Uani 1 1 d . B . H13A H 0.3718 1.1754 0.8137 0.083 Uiso 1 1 calc R . . H13B H 0.4404 1.2027 0.8006 0.083 Uiso 1 1 calc R . . H13C H 0.4211 1.1919 0.8434 0.083 Uiso 1 1 calc R . . C14 C 0.4405(12) 0.8490(11) 0.9048(6) 0.047 Uani 1 1 d . . . H14A H 0.4762 0.8027 0.9105 0.057 Uiso 1 1 calc R B 1 C15 C 0.3819(11) 0.8830(10) 0.9275(5) 0.041 Uani 1 1 d . C . C16 C 0.3430(12) 0.9475(11) 0.9085(6) 0.046 Uani 1 1 d . . . H16 H 0.2996 0.9822 0.9172 0.055 Uiso 1 1 calc R B 1 C17 C 0.6638(12) 0.7151(11) 0.8756(6) 0.047 Uani 1 1 d . . . C18 C 0.6638(14) 0.7669(13) 0.8988(7) 0.064 Uani 1 1 d . B . H18A H 0.6918 0.7585 0.9204 0.077 Uiso 1 1 calc R . . C19 C 0.6145(12) 0.8343(11) 0.8844(6) 0.047 Uani 1 1 d . . . C20 C 0.5944(15) 0.9058(13) 0.9016(7) 0.066 Uani 1 1 d . B . H20A H 0.6394 0.9185 0.9041 0.098 Uiso 1 1 calc R . . H20B H 0.5713 0.9009 0.9258 0.098 Uiso 1 1 calc R . . H20C H 0.5596 0.9442 0.8859 0.098 Uiso 1 1 calc R . . C21 C 0.7108(15) 0.6333(13) 0.8779(7) 0.070 Uani 1 1 d . B . H21A H 0.6845 0.6065 0.8661 0.105 Uiso 1 1 calc R . . H21B H 0.7187 0.6141 0.9037 0.105 Uiso 1 1 calc R . . H21C H 0.7589 0.6276 0.8655 0.105 Uiso 1 1 calc R . . C22 C 0.5915(10) 0.7874(9) 0.7359(5) 0.031 Uani 1 1 d . . . H22 H 0.6163 0.7446 0.7244 0.038 Uiso 1 1 calc R B 1 C23 C 0.5586(10) 0.8598(9) 0.7180(5) 0.033 Uani 1 1 d . B . C24 C 0.5285(9) 0.9040(9) 0.7462(5) 0.029 Uani 1 1 d . . . H24A H 0.5033 0.9548 0.7431 0.035 Uiso 1 1 calc R B 1 C25 C 0.7423(13) 0.5509(11) 0.7670(7) 0.052 Uani 1 1 d . . . C26 C 0.7835(12) 0.5966(11) 0.7696(6) 0.049 Uani 1 1 d . B . H26 H 0.8341 0.5872 0.7625 0.059 Uiso 1 1 calc R . . C27 C 0.7374(11) 0.6588(11) 0.7843(6) 0.044 Uani 1 1 d . . . C28 C 0.7684(16) 0.4791(14) 0.7495(8) 0.077 Uani 1 1 d . B . H28A H 0.7875 0.4388 0.7684 0.115 Uiso 1 1 calc R . . H28B H 0.8079 0.4797 0.7313 0.115 Uiso 1 1 calc R . . H28C H 0.7267 0.4727 0.7374 0.115 Uiso 1 1 calc R . . C29 C 0.7573(12) 0.7242(11) 0.7932(7) 0.050 Uani 1 1 d . B . H29A H 0.7124 0.7666 0.7933 0.075 Uiso 1 1 calc R . . H29B H 0.7927 0.7340 0.7747 0.075 Uiso 1 1 calc R . . H29C H 0.7797 0.7141 0.8174 0.075 Uiso 1 1 calc R . . C30 C 0.5180(12) 0.5399(12) 0.8528(7) 0.055 Uani 1 1 d . . . H30 H 0.5086 0.4963 0.8495 0.065 Uiso 1 1 calc R B 1 C31 C 0.5032(14) 0.5762(13) 0.8847(7) 0.063 Uani 1 1 d U B . C32 C 0.5261(13) 0.6375(12) 0.8772(6) 0.056 Uani 1 1 d . . . H32 H 0.5236 0.6722 0.8939 0.067 Uiso 1 1 calc R B 1 C33 C 0.6045(16) 0.3591(13) 0.7697(8) 0.073 Uani 1 1 d . . . C34 C 0.6535(18) 0.3475(15) 0.7977(9) 0.086 Uani 1 1 d . B . H34 H 0.6806 0.3019 0.8098 0.103 Uiso 1 1 calc R . . C35 C 0.6557(15) 0.4152(13) 0.8049(8) 0.067 Uani 1 1 d . . . C36 C 0.5820(18) 0.3002(14) 0.7528(10) 0.089 Uani 1 1 d . B . H36A H 0.5299 0.3060 0.7590 0.134 Uiso 1 1 calc R . . H36B H 0.6132 0.2519 0.7627 0.134 Uiso 1 1 calc R . . H36C H 0.5887 0.3054 0.7262 0.134 Uiso 1 1 calc R . . C37 C 0.6973(17) 0.4303(14) 0.8351(8) 0.082 Uani 1 1 d . B . H37A H 0.7198 0.4673 0.8258 0.123 Uiso 1 1 calc R . . H37B H 0.7362 0.3855 0.8438 0.123 Uiso 1 1 calc R . . H37C H 0.6629 0.4479 0.8554 0.123 Uiso 1 1 calc R . . C38 C 0.5654(13) 0.5620(12) 0.6632(6) 0.053 Uani 1 1 d . . . H38 H 0.5452 0.5488 0.6430 0.064 Uiso 1 1 calc R B 1 C39 C 0.6156(12) 0.6018(11) 0.6618(7) 0.049 Uani 1 1 d . B . C40 C 0.6325(12) 0.6064(10) 0.6986(6) 0.044 Uani 1 1 d . . . H40 H 0.6670 0.6279 0.7056 0.053 Uiso 1 1 calc R B 1 C41 C 0.4524(14) 0.3969(12) 0.6436(7) 0.060 Uani 1 1 d . . . C42 C 0.5309(14) 0.3735(12) 0.6370(8) 0.068 Uani 1 1 d . B . H42 H 0.5578 0.3471 0.6177 0.081 Uiso 1 1 calc R . . C43 C 0.5603(13) 0.3993(11) 0.6666(7) 0.054 Uani 1 1 d . . . C44 C 0.3984(16) 0.3857(14) 0.6164(8) 0.078 Uani 1 1 d . B . H44A H 0.3590 0.3715 0.6302 0.116 Uiso 1 1 calc R . . H44B H 0.4257 0.3474 0.6009 0.116 Uiso 1 1 calc R . . H44C H 0.3764 0.4311 0.6010 0.116 Uiso 1 1 calc R . . C45 C 0.6421(17) 0.3856(15) 0.6749(10) 0.089 Uani 1 1 d . B . H45A H 0.6451 0.4161 0.6938 0.133 Uiso 1 1 calc R . . H45B H 0.6680 0.3975 0.6526 0.133 Uiso 1 1 calc R . . H45C H 0.6654 0.3343 0.6836 0.133 Uiso 1 1 calc R . . C46 C 0.3264(12) 0.4162(11) 0.7681(6) 0.050 Uani 1 1 d . . . H46 H 0.2798 0.4100 0.7652 0.061 Uiso 1 1 calc R B 1 C47 C 0.3703(13) 0.3943(11) 0.7997(7) 0.057 Uani 1 1 d . B . C48 C 0.4352(13) 0.4127(12) 0.7919(7) 0.057 Uani 1 1 d . . . H48 H 0.4753 0.4032 0.8080 0.069 Uiso 1 1 calc R B 1 C49 C 0.1680(11) 0.4234(10) 0.6815(6) 0.047 Uani 1 1 d . . . C50 C 0.2209(13) 0.3531(11) 0.6899(7) 0.055 Uani 1 1 d . B . H50 H 0.2116 0.3081 0.6928 0.066 Uiso 1 1 calc R . . C51 C 0.2897(12) 0.3641(10) 0.6929(7) 0.052 Uani 1 1 d . . . C52 C 0.0848(13) 0.4401(12) 0.6775(7) 0.059 Uani 1 1 d . B . H52A H 0.0591 0.4571 0.7003 0.088 Uiso 1 1 calc R . . H52B H 0.0748 0.3961 0.6724 0.088 Uiso 1 1 calc R . . H52C H 0.0671 0.4780 0.6573 0.088 Uiso 1 1 calc R . . C53 C 0.3635(13) 0.3068(11) 0.7007(8) 0.061 Uani 1 1 d . B . H53A H 0.4029 0.3291 0.6974 0.092 Uiso 1 1 calc R . . H53B H 0.3724 0.2694 0.6837 0.092 Uiso 1 1 calc R . . H53C H 0.3633 0.2847 0.7259 0.092 Uiso 1 1 calc R . . C54 C 0.2444(12) 0.6220(10) 0.6027(6) 0.041 Uani 1 1 d . . . H54 H 0.2007 0.6512 0.5904 0.049 Uiso 1 1 calc R B 1 C55 C 0.3160(12) 0.6099(11) 0.5892(6) 0.046 Uani 1 1 d . B . C56 C 0.3643(13) 0.5678(11) 0.6161(7) 0.050 Uani 1 1 d . . . H56 H 0.4168 0.5534 0.6147 0.060 Uiso 1 1 calc R B 1 C57 C 0.0048(12) 0.6761(10) 0.6046(6) 0.043 Uani 1 1 d . . . C58 C 0.0409(13) 0.6170(11) 0.5840(6) 0.051 Uani 1 1 d . B . H58 H 0.0283 0.6111 0.5602 0.061 Uiso 1 1 calc R . . C59 C 0.0978(11) 0.5697(10) 0.6047(6) 0.041 Uani 1 1 d . . . C60 C -0.0655(12) 0.7426(11) 0.5937(6) 0.047 Uani 1 1 d . B . H60A H -0.1066 0.7419 0.6108 0.070 Uiso 1 1 calc R . . H60B H -0.0796 0.7398 0.5687 0.070 Uiso 1 1 calc R . . H60C H -0.0543 0.7878 0.5946 0.070 Uiso 1 1 calc R . . C61 C 0.1571(14) 0.5008(12) 0.5925(7) 0.061 Uani 1 1 d . B . H61A H 0.1967 0.5143 0.5786 0.092 Uiso 1 1 calc R . . H61B H 0.1344 0.4764 0.5770 0.092 Uiso 1 1 calc R . . H61C H 0.1779 0.4679 0.6142 0.092 Uiso 1 1 calc R . . C62 C -0.0020(10) 0.6356(9) 0.7468(5) 0.031 Uani 1 1 d . . . H62 H -0.0475 0.6695 0.7540 0.037 Uiso 1 1 calc R B 1 C63 C 0.0363(11) 0.5700(10) 0.7660(5) 0.040 Uani 1 1 d . B . C64 C 0.0988(12) 0.5366(10) 0.7460(6) 0.043 Uani 1 1 d . . . H64 H 0.1347 0.4909 0.7526 0.052 Uiso 1 1 calc R B 1 C65 C -0.1888(9) 0.8302(9) 0.6975(5) 0.029 Uani 1 1 d . . . C66 C -0.1978(9) 0.7641(8) 0.6903(4) 0.025 Uani 1 1 d . B . H66 H -0.2432 0.7538 0.6918 0.031 Uiso 1 1 calc R . . C67 C -0.1297(10) 0.7170(9) 0.6806(5) 0.034 Uani 1 1 d . . . C68 C -0.2470(11) 0.9003(10) 0.7088(6) 0.041 Uani 1 1 d . B . H68A H -0.2227 0.9278 0.7213 0.061 Uiso 1 1 calc R . . H68B H -0.2841 0.8879 0.7253 0.061 Uiso 1 1 calc R . . H68C H -0.2714 0.9298 0.6869 0.061 Uiso 1 1 calc R . . C69 C -0.1117(11) 0.6375(10) 0.6720(6) 0.041 Uani 1 1 d . B . H69A H -0.0855 0.6310 0.6482 0.062 Uiso 1 1 calc R . . H69B H -0.1578 0.6261 0.6711 0.062 Uiso 1 1 calc R . . H69C H -0.0802 0.6049 0.6911 0.062 Uiso 1 1 calc R . . C70 C 0.0183(10) 0.9217(9) 0.6295(5) 0.032 Uani 1 1 d . . . H70 H 0.0009 0.9730 0.6297 0.039 Uiso 1 1 calc R B 1 C71 C 0.0706(11) 0.8837(10) 0.6049(5) 0.041 Uani 1 1 d . B . C72 C 0.0798(11) 0.8089(10) 0.6136(5) 0.036 Uani 1 1 d . . . H72 H 0.1113 0.7700 0.6010 0.044 Uiso 1 1 calc R B 1 C73 C -0.1744(11) 1.0967(10) 0.6819(6) 0.038 Uani 1 1 d . . . C74 C -0.1989(11) 1.0773(10) 0.6510(6) 0.043 Uani 1 1 d . B . H74 H -0.2307 1.1085 0.6328 0.051 Uiso 1 1 calc R . . C75 C -0.1656(11) 0.9994(10) 0.6525(6) 0.039 Uani 1 1 d . . . C76 C -0.1932(12) 1.1751(11) 0.6921(6) 0.050 Uani 1 1 d . B . H76A H -0.1710 1.1746 0.7157 0.075 Uiso 1 1 calc R . . H76B H -0.2471 1.1973 0.6942 0.075 Uiso 1 1 calc R . . H76C H -0.1734 1.2034 0.6731 0.075 Uiso 1 1 calc R . . C77 C -0.1720(12) 0.9505(11) 0.6237(6) 0.048 Uani 1 1 d . B . H77A H -0.1276 0.9394 0.6078 0.071 Uiso 1 1 calc R . . H77B H -0.2159 0.9755 0.6089 0.071 Uiso 1 1 calc R . . H77C H -0.1767 0.9052 0.6361 0.071 Uiso 1 1 calc R . . C78 C -0.1151(10) 0.9397(10) 0.8047(5) 0.034 Uani 1 1 d . . . H78 H -0.1211 0.9731 0.8225 0.040 Uiso 1 1 calc R B 1 C79 C -0.1262(11) 0.8738(10) 0.8106(5) 0.037 Uani 1 1 d . B . C80 C -0.1123(10) 0.8437(9) 0.7773(5) 0.029 Uani 1 1 d . . . H80 H -0.1170 0.7983 0.7732 0.035 Uiso 1 1 calc R B 1 C81 C -0.1276(12) 1.1615(11) 0.8197(6) 0.045 Uani 1 1 d . . . C82 C -0.1959(13) 1.1535(11) 0.8152(6) 0.052 Uani 1 1 d . B . H82 H -0.2395 1.1718 0.8297 0.062 Uiso 1 1 calc R . . C83 C -0.1882(11) 1.1119(11) 0.7841(6) 0.044 Uani 1 1 d . . . C84 C -0.1042(14) 1.2014(12) 0.8492(6) 0.057 Uani 1 1 d . B . H84A H -0.0962 1.1708 0.8725 0.086 Uiso 1 1 calc R . . H84B H -0.1434 1.2475 0.8524 0.086 Uiso 1 1 calc R . . H84C H -0.0582 1.2110 0.8411 0.086 Uiso 1 1 calc R . . C85 C -0.2503(13) 1.0895(12) 0.7690(7) 0.055 Uani 1 1 d . B . H85A H -0.2385 1.0790 0.7434 0.082 Uiso 1 1 calc R . . H85B H -0.2974 1.1293 0.7702 0.082 Uiso 1 1 calc R . . H85C H -0.2546 1.0461 0.7837 0.082 Uiso 1 1 calc R . . C86 C 0.0452(9) 1.1697(8) 0.7087(5) 0.025 Uani 1 1 d . . . H86 H 0.0703 1.2012 0.7151 0.030 Uiso 1 1 calc R B 1 C87 C 0.0287(10) 1.1617(9) 0.6732(5) 0.032 Uani 1 1 d . B . C88 C -0.0099(10) 1.1112(9) 0.6763(5) 0.032 Uani 1 1 d . . . H88 H -0.0295 1.0956 0.6567 0.039 Uiso 1 1 calc R B 1 C89 C 0.1104(10) 1.2633(9) 0.7943(5) 0.032 Uani 1 1 d . . . C90 C 0.0417(11) 1.3066(10) 0.7790(5) 0.037 Uani 1 1 d . B . H90 H 0.0283 1.3567 0.7708 0.044 Uiso 1 1 calc R . . C91 C -0.0026(11) 1.2632(10) 0.7782(5) 0.038 Uani 1 1 d . . . C92 C 0.1769(12) 1.2853(10) 0.8010(6) 0.044 Uani 1 1 d . B . H92A H 0.2109 1.2474 0.8172 0.067 Uiso 1 1 calc R . . H92B H 0.1608 1.3310 0.8124 0.067 Uiso 1 1 calc R . . H92C H 0.2024 1.2918 0.7776 0.067 Uiso 1 1 calc R . . C93 C -0.0809(14) 1.2860(13) 0.7629(7) 0.062 Uani 1 1 d . B . H93A H -0.0867 1.2461 0.7507 0.093 Uiso 1 1 calc R . . H93B H -0.0885 1.3289 0.7452 0.093 Uiso 1 1 calc R . . H93C H -0.1175 1.2975 0.7830 0.093 Uiso 1 1 calc R . . C94 C 0.1203(12) 1.0386(10) 0.8851(6) 0.046 Uani 1 1 d . . . H94 H 0.1585 1.0362 0.9012 0.055 Uiso 1 1 calc R B 1 C95 C 0.0617(12) 1.0096(11) 0.8934(5) 0.043 Uani 1 1 d . B . C96 C 0.0158(12) 1.0281(10) 0.8624(5) 0.040 Uani 1 1 d . . . H96 H -0.0289 1.0177 0.8602 0.048 Uiso 1 1 calc R B 1 C97 C 0.27390(17) 0.11123(14) 0.47021(6) 0.035 Uani 1 1 d G . . C98 C 0.25595(19) 0.16961(14) 0.44213(6) 0.048 Uani 1 1 d G . . H98 H 0.2226 0.2157 0.4472 0.057 Uiso 1 1 calc R . . C99 C 0.2878(2) 0.15911(15) 0.40648(6) 0.056 Uani 1 1 d G . . H99 H 0.2758 0.1982 0.3877 0.067 Uiso 1 1 calc R . . C100 C 0.3377(2) 0.09023(16) 0.39891(6) 0.055 Uani 1 1 d G . . H100 H 0.3590 0.0832 0.3751 0.066 Uiso 1 1 calc R . . C101 C 0.35562(18) 0.03185(15) 0.42699(6) 0.057 Uani 1 1 d G . . H101 H 0.3890 -0.0142 0.4219 0.069 Uiso 1 1 calc R . . C102 C 0.32374(17) 0.04235(14) 0.46264(6) 0.045 Uani 1 1 d G . . H102 H 0.3358 0.0033 0.4814 0.055 Uiso 1 1 calc R . . C103 C 0.13063(15) 0.14042(15) 0.50883(7) 0.048 Uani 1 1 d G . . C104 C 0.10847(15) 0.08373(17) 0.49740(8) 0.076 Uani 1 1 d G . . H104 H 0.1441 0.0374 0.4949 0.091 Uiso 1 1 calc R . . C105 C 0.03302(16) 0.0963(2) 0.48965(9) 0.094 Uani 1 1 d G . . H105 H 0.0182 0.0583 0.4820 0.113 Uiso 1 1 calc R . . C106 C -0.02027(15) 0.1655(2) 0.49332(10) 0.082 Uani 1 1 d G . . H106 H -0.0707 0.1739 0.4881 0.098 Uiso 1 1 calc R . . C107 C 0.00189(15) 0.22223(19) 0.50475(9) 0.093 Uani 1 1 d G . . H107 H -0.0338 0.2686 0.5072 0.111 Uiso 1 1 calc R . . C108 C 0.07734(15) 0.20968(16) 0.51250(8) 0.064 Uani 1 1 d G . . H108 H 0.0922 0.2476 0.5201 0.077 Uiso 1 1 calc R . . C109 C 0.24310(14) 0.20113(12) 0.53379(6) 0.034 Uani 1 1 d G . . C110 C 0.28981(16) 0.23888(12) 0.51641(5) 0.049 Uani 1 1 d G . . H110 H 0.3141 0.2252 0.4938 0.058 Uiso 1 1 calc R . . C111 C 0.30027(17) 0.29710(12) 0.53285(6) 0.062 Uani 1 1 d G . . H111 H 0.3315 0.3224 0.5212 0.074 Uiso 1 1 calc R . . C112 C 0.26400(15) 0.31757(11) 0.56668(5) 0.062 Uani 1 1 d G . . H112 H 0.2710 0.3565 0.5777 0.074 Uiso 1 1 calc R . . C113 C 0.21729(13) 0.27981(11) 0.58407(6) 0.068 Uani 1 1 d G . . H113 H 0.1930 0.2935 0.6067 0.081 Uiso 1 1 calc R . . C114 C 0.20684(13) 0.22159(12) 0.56763(6) 0.055 Uani 1 1 d G . . H114 H 0.1756 0.1963 0.5793 0.066 Uiso 1 1 calc R . . C115 C 0.38553(17) -0.07598(12) 0.56409(7) 0.032 Uani 1 1 d G . . C116 C 0.35147(18) -0.11863(12) 0.54723(7) 0.036 Uani 1 1 d G . . H116 H 0.3020 -0.0978 0.5390 0.043 Uiso 1 1 calc R . . C117 C 0.3913(2) -0.19245(12) 0.54270(8) 0.047 Uani 1 1 d G . . H117 H 0.3685 -0.2210 0.5314 0.057 Uiso 1 1 calc R . . C118 C 0.4652(2) -0.22363(12) 0.55503(8) 0.057 Uani 1 1 d G . . H118 H 0.4918 -0.2730 0.5520 0.068 Uiso 1 1 calc R . . C119 C 0.49922(19) -0.18099(13) 0.57189(8) 0.048 Uani 1 1 d G . . H119 H 0.5486 -0.2018 0.5801 0.058 Uiso 1 1 calc R . . C120 C 0.45940(17) -0.10716(12) 0.57642(7) 0.045 Uani 1 1 d G . . H120 H 0.4822 -0.0786 0.5877 0.054 Uiso 1 1 calc R . . C121 C 0.29290(16) 0.01548(11) 0.61786(6) 0.027 Uani 1 1 d G . . C122 C 0.21696(17) 0.02136(13) 0.62284(7) 0.042 Uani 1 1 d G . . H122 H 0.1857 0.0328 0.6023 0.050 Uiso 1 1 calc R . . C123 C 0.18774(19) 0.01012(14) 0.65854(7) 0.053 Uani 1 1 d G . . H123 H 0.1369 0.0140 0.6619 0.064 Uiso 1 1 calc R . . C124 C 0.2345(2) -0.00699(13) 0.68925(7) 0.063 Uani 1 1 d G . . H124 H 0.2149 -0.0145 0.7131 0.075 Uiso 1 1 calc R . . C125 C 0.3104(2) -0.01287(11) 0.68427(6) 0.043 Uani 1 1 d G . . H125 H 0.3417 -0.0243 0.7048 0.052 Uiso 1 1 calc R . . C126 C 0.33963(17) -0.00164(11) 0.64857(6) 0.039 Uani 1 1 d G . . H126 H 0.3904 -0.0056 0.6452 0.046 Uiso 1 1 calc R . . C127 C 0.39531(13) 0.07078(12) 0.56667(6) 0.030 Uani 1 1 d G . . C128 C 0.44239(14) 0.06525(14) 0.53506(7) 0.031 Uani 1 1 d G . . H128 H 0.4430 0.0319 0.5180 0.037 Uiso 1 1 calc R . . C129 C 0.48856(14) 0.10954(16) 0.52895(7) 0.041 Uani 1 1 d G . . H129 H 0.5200 0.1058 0.5078 0.050 Uiso 1 1 calc R . . C130 C 0.48768(14) 0.15936(16) 0.55446(7) 0.049 Uani 1 1 d G . . H130 H 0.5186 0.1890 0.5504 0.059 Uiso 1 1 calc R . . C131 C 0.44060(13) 0.16489(14) 0.58606(7) 0.042 Uani 1 1 d G . . H131 H 0.4400 0.1982 0.6031 0.050 Uiso 1 1 calc R . . C132 C 0.39442(12) 0.12060(12) 0.59217(6) 0.035 Uani 1 1 d G . . H132 H 0.3629 0.1243 0.6133 0.042 Uiso 1 1 calc R . . C133 C 0.1254(2) 0.55101(17) 0.92539(7) 0.085 Uani 1 1 d G . . C134 C 0.2005(2) 0.51666(17) 0.93525(7) 0.085 Uani 1 1 d G . . H134 H 0.2251 0.5413 0.9482 0.102 Uiso 1 1 calc R . . C135 C 0.2390(2) 0.44541(16) 0.92574(6) 0.085 Uani 1 1 d G . . H135 H 0.2893 0.4224 0.9323 0.102 Uiso 1 1 calc R . . C136 C 0.2023(2) 0.40851(16) 0.90638(6) 0.085 Uani 1 1 d G . . H136 H 0.2280 0.3608 0.9000 0.102 Uiso 1 1 calc R . . C137 C 0.1272(2) 0.44286(16) 0.89653(6) 0.085 Uani 1 1 d G . . H137 H 0.1026 0.4182 0.8836 0.102 Uiso 1 1 calc R . . C138 C 0.0887(2) 0.51412(17) 0.90603(7) 0.085 Uani 1 1 d G . . H138 H 0.0385 0.5371 0.8994 0.102 Uiso 1 1 calc R . . C139 C -0.0133(2) 0.6368(2) 0.94648(9) 0.121 Uani 1 1 d G . . C140 C -0.0308(2) 0.6100(2) 0.98211(9) 0.121 Uani 1 1 d G . . H140 H 0.0067 0.5917 0.9999 0.145 Uiso 1 1 calc R . . C141 C -0.1042(3) 0.6107(2) 0.99112(10) 0.121 Uani 1 1 d G . . H141 H -0.1159 0.5928 1.0150 0.145 Uiso 1 1 calc R . . C142 C -0.1603(2) 0.6381(3) 0.96451(11) 0.121 Uani 1 1 d G . . H142 H -0.2094 0.6385 0.9705 0.145 Uiso 1 1 calc R . . C143 C -0.1428(2) 0.6648(2) 0.92887(11) 0.121 Uani 1 1 d G . . H143 H -0.1803 0.6832 0.9111 0.145 Uiso 1 1 calc R . . C144 C -0.0694(2) 0.6642(2) 0.91986(9) 0.121 Uani 1 1 d G . . H144 H -0.0577 0.6821 0.8960 0.145 Uiso 1 1 calc R . . C145 C 0.0703(2) 0.69913(16) 0.89086(8) 0.076 Uani 1 1 d G . . C146 C 0.08382(19) 0.67176(15) 0.85600(8) 0.135 Uani 1 1 d G . . H146 H 0.0955 0.6212 0.8542 0.162 Uiso 1 1 calc R . . C147 C 0.07981(19) 0.71995(14) 0.82380(8) 0.128 Uani 1 1 d G . . H147 H 0.0888 0.7016 0.8005 0.153 Uiso 1 1 calc R . . C148 C 0.0623(2) 0.79551(14) 0.82648(9) 0.082 Uani 1 1 d G . . H148 H 0.0596 0.8278 0.8049 0.099 Uiso 1 1 calc R . . C149 C 0.0488(2) 0.82289(15) 0.86133(9) 0.105 Uani 1 1 d G . . H149 H 0.0371 0.8734 0.8631 0.126 Uiso 1 1 calc R . . C150 C 0.0529(2) 0.77470(16) 0.89352(9) 0.094 Uani 1 1 d G . . H150 H 0.0438 0.7930 0.9168 0.113 Uiso 1 1 calc R . . C151 C 0.2587(2) 0.6232(2) 0.99799(8) 0.119 Uani 1 1 d G . . C152 C 0.2317(3) 0.5807(2) 1.02545(7) 0.119 Uani 1 1 d G . . H152 H 0.1818 0.5812 1.0250 0.142 Uiso 1 1 calc R . . C153 C 0.2791(3) 0.5376(2) 1.05357(7) 0.119 Uani 1 1 d G . . H153 H 0.2611 0.5092 1.0719 0.142 Uiso 1 1 calc R . . C154 C 0.3536(3) 0.5370(2) 1.05421(8) 0.119 Uani 1 1 d G . . H154 H 0.3854 0.5081 1.0730 0.142 Uiso 1 1 calc R . . C155 C 0.3807(3) 0.5794(2) 1.02676(9) 0.145 Uani 1 1 d G . . H155 H 0.4305 0.5790 1.0272 0.174 Uiso 1 1 calc R . . C156 C 0.3332(2) 0.6225(2) 0.99863(9) 0.165 Uani 1 1 d G . . H156 H 0.3513 0.6509 0.9802 0.198 Uiso 1 1 calc R . . C157 C 0.1538(3) 0.7673(2) 1.00140(9) 0.082 Uani 1 1 d G . . C158 C 0.2034(3) 0.8004(2) 1.01322(9) 0.114 Uani 1 1 d G . . H158 H 0.2545 0.7829 1.0066 0.137 Uiso 1 1 calc R . . C159 C 0.1766(3) 0.8597(2) 1.03496(10) 0.124 Uani 1 1 d G . . H159 H 0.2098 0.8819 1.0429 0.149 Uiso 1 1 calc R . . C160 C 0.1003(3) 0.8859(2) 1.04489(10) 0.113 Uani 1 1 d G . . H160 H 0.0824 0.9255 1.0594 0.136 Uiso 1 1 calc R . . C161 C 0.0507(3) 0.8527(2) 1.03307(9) 0.129 Uani 1 1 d G . . H161 H -0.0004 0.8702 1.0397 0.155 Uiso 1 1 calc R . . C162 C 0.0774(3) 0.7934(2) 1.01133(9) 0.151 Uani 1 1 d G . . H162 H 0.0442 0.7712 1.0034 0.182 Uiso 1 1 calc R . . C163 C 0.2308(2) 0.73068(18) 0.93295(8) 0.079 Uani 1 1 d G . . C164 C 0.2857(2) 0.68088(18) 0.91253(8) 0.164 Uani 1 1 d G . . H164 H 0.3009 0.6305 0.9204 0.197 Uiso 1 1 calc R . . C165 C 0.3178(2) 0.70644(18) 0.88035(9) 0.132 Uani 1 1 d G . . H165 H 0.3545 0.6731 0.8667 0.159 Uiso 1 1 calc R . . C166 C 0.2950(2) 0.78178(18) 0.86859(9) 0.114 Uani 1 1 d G . . H166 H 0.3165 0.7989 0.8471 0.137 Uiso 1 1 calc R . . C167 C 0.2401(2) 0.83156(17) 0.88901(9) 0.093 Uani 1 1 d G . . H167 H 0.2249 0.8820 0.8811 0.112 Uiso 1 1 calc R . . C168 C 0.2080(2) 0.80601(18) 0.92121(9) 0.111 Uani 1 1 d G . . H168 H 0.1713 0.8393 0.9349 0.133 Uiso 1 1 calc R . . C169 C 0.3257(3) 0.73497(16) 0.64823(9) 0.087 Uani 1 1 d G . . H16A H 0.2824 0.7235 0.6600 0.104 Uiso 1 1 calc R D 1 H16B H 0.3266 0.7285 0.6218 0.104 Uiso 1 1 calc R D 1 C170 C 0.3197(3) 0.81413(17) 0.65331(9) 0.069 Uani 1 1 d G D . H17A H 0.2753 0.8369 0.6685 0.083 Uiso 1 1 calc R . . H17B H 0.3160 0.8433 0.6293 0.083 Uiso 1 1 calc R . . C171 C 0.3929(3) 0.8090(2) 0.67313(10) 0.063 Uani 1 1 d G . . H17C H 0.4175 0.8422 0.6600 0.075 Uiso 1 1 calc R D . H17D H 0.3820 0.8212 0.6988 0.075 Uiso 1 1 calc R . . C172 C 0.4408(3) 0.7304(2) 0.67184(10) 0.072 Uani 1 1 d G D . H17E H 0.4791 0.7264 0.6521 0.086 Uiso 1 1 calc R G 1 H17F H 0.4661 0.7116 0.6955 0.086 Uiso 1 1 calc R G 1 C173 C 0.59182(14) 0.07080(18) 0.70252(9) 0.069 Uani 1 1 d G . . H700 H 0.5567 0.0444 0.7110 0.083 Uiso 1 1 calc R E 1 H701 H 0.6415 0.0437 0.7125 0.083 Uiso 1 1 calc R E 1 C174 C 0.59466(12) 0.08460(18) 0.65878(9) 0.085 Uani 1 1 d G E . H707 H 0.6421 0.0541 0.6484 0.102 Uiso 1 1 calc R . . H706 H 0.5529 0.0755 0.6476 0.102 Uiso 1 1 calc R . . C175 C 0.58767(12) 0.16627(19) 0.65365(9) 0.091 Uani 1 1 d G . . H704 H 0.6248 0.1742 0.6352 0.110 Uiso 1 1 calc R E . H705 H 0.5377 0.1954 0.6447 0.110 Uiso 1 1 calc R . . C176 C 0.59990(12) 0.1897(2) 0.68901(10) 0.077 Uani 1 1 d G E . H702 H 0.6533 0.1762 0.6942 0.092 Uiso 1 1 calc R H 1 H703 H 0.5760 0.2426 0.6901 0.092 Uiso 1 1 calc R H 1 P1 P 0.23111(14) 0.12219(13) 0.51589(6) 0.034 Uani 1 1 d G . . P2 P 0.33035(14) 0.01878(11) 0.57104(6) 0.029 Uani 1 1 d G . . P3 P 0.0803(2) 0.63807(18) 0.93337(8) 0.078 Uani 1 1 d G . . P4 P 0.1881(2) 0.69344(19) 0.97209(8) 0.086 Uani 1 1 d G . . O40 O 0.1818(5) 0.83311(15) 0.43891(8) 0.692 Uiso 1 1 d GD . . O39 O 0.2945(4) 0.78991(18) 0.44401(8) 0.440 Uiso 1 1 d GD . . O42 O 0.2358(3) 0.91472(16) 0.77915(10) 0.216 Uiso 1 1 d GD A . N65 N 0.2802(3) 0.85044(16) 0.77337(10) 0.332 Uiso 1 1 d G . . N61 N 0.3643(3) 0.8550(2) 0.96450(11) 0.054 Uani 1 1 d GD . . O44 O 0.1410(3) 0.88240(13) 0.74850(9) 0.050 Uiso 1 1 d G . . H10A H 0.1595 0.8716 0.7254 0.060 Uiso 1 1 d R . . H10B H 0.1166 0.9297 0.7529 0.060 Uiso 1 1 d 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 0.021 0.026 0.028 -0.009 0.002 -0.009 Co2 0.022 0.027 0.026 -0.008 -0.003 -0.007 Co3 0.025 0.027 0.026 -0.004 -0.006 -0.005 Co4 0.024 0.024 0.036 0.003 -0.010 -0.008 Co5 0.028 0.019 0.078 -0.001 -0.021 -0.007 Co6 0.032 0.018 0.097 -0.006 -0.029 -0.004 Co7 0.031 0.017 0.085 -0.007 -0.024 -0.004 Co8 0.029 0.021 0.055 -0.006 -0.016 -0.004 Co9 0.023 0.022 0.036 -0.004 -0.009 -0.006 Co10 0.020 0.019 0.031 -0.001 -0.006 -0.005 Co11 0.017 0.020 0.037 -0.005 -0.001 -0.005 Co12 0.018 0.022 0.034 -0.007 0.001 -0.006 O1 0.033 0.026 0.031 -0.004 0.000 -0.017 O2 0.038 0.051 0.034 -0.013 0.009 -0.020 O3 0.046 0.035 0.033 0.000 -0.011 0.003 O4 0.024 0.020 0.010 0.003 -0.011 -0.001 O5 0.145 0.108 0.040 0.034 0.009 0.013 O6 0.088 0.116 0.050 -0.009 0.008 -0.011 O7 0.026 0.024 0.033 0.008 -0.012 -0.007 O8 0.091 0.043 0.038 -0.010 0.011 -0.021 O9 0.042 0.054 0.040 -0.001 0.003 -0.012 O10 0.031 0.015 0.045 0.001 -0.020 -0.003 O11 0.136 0.157 0.134 0.090 -0.027 -0.082 O12 0.136 0.157 0.134 0.090 -0.027 -0.082 O13 0.034 0.024 0.078 -0.004 -0.017 -0.014 O14 0.092 0.109 0.084 -0.030 -0.003 -0.034 O15 0.087 0.088 0.108 -0.023 0.016 -0.043 O16 0.045 0.019 0.076 0.002 -0.016 -0.014 O17 0.136 0.157 0.134 0.090 -0.027 -0.082 O18 0.109 0.097 0.117 0.036 -0.061 -0.069 O19 0.136 0.157 0.134 0.090 -0.027 -0.082 O20 0.070 0.060 0.092 -0.006 0.005 -0.007 O21 0.060 0.069 0.108 -0.027 0.016 -0.024 O22 0.023 0.018 0.049 0.002 -0.010 -0.003 O23 0.075 0.073 0.063 0.018 0.002 -0.024 O24 0.100 0.050 0.087 0.033 -0.005 0.001 O25 0.036 0.027 0.022 0.008 -0.016 -0.013 O26 0.098 0.074 0.069 0.023 -0.005 -0.049 O27 0.058 0.100 0.086 -0.019 0.016 -0.024 O28 0.014 0.022 0.027 0.003 0.001 -0.005 O29 0.137 0.116 0.049 -0.017 0.027 -0.081 O30 0.134 0.114 0.046 0.016 -0.023 -0.102 O31 0.025 0.018 0.031 0.006 -0.005 -0.006 O32 0.072 0.064 0.069 0.020 -0.005 -0.035 O33 0.094 0.088 0.049 0.002 -0.002 -0.043 O34 0.015 0.025 0.035 -0.012 0.005 -0.006 O35 0.103 0.164 0.039 0.014 -0.005 -0.069 O36 0.088 0.124 0.063 0.006 0.017 -0.067 O37 0.067 0.051 0.112 0.007 -0.037 -0.020 O38 0.184 0.100 0.155 -0.018 -0.009 -0.068 N1 0.031 0.034 0.023 -0.013 -0.007 -0.002 N2 0.026 0.037 0.038 -0.026 0.006 -0.005 N3 0.028 0.020 0.030 -0.010 -0.007 -0.008 N4 0.021 0.031 0.040 -0.007 0.000 -0.011 N5 0.048 0.030 0.031 -0.012 0.009 -0.022 N6 0.020 0.043 0.028 -0.015 0.005 -0.016 N7 0.030 0.038 0.027 -0.013 -0.004 -0.013 N8 0.023 0.041 0.018 0.005 -0.001 -0.005 N9 0.044 0.038 0.026 -0.008 -0.001 -0.014 N11 0.022 0.020 0.050 0.010 -0.013 0.000 N12 0.030 0.042 0.032 -0.003 -0.012 -0.006 N13 0.035 0.013 0.044 -0.003 -0.011 -0.008 N14 0.028 0.027 0.038 -0.003 -0.012 -0.003 N15 0.046 0.035 0.030 -0.003 0.001 -0.019 N16 0.025 0.027 0.081 -0.012 -0.025 0.005 N17 0.030 0.026 0.048 -0.004 -0.012 -0.008 N18 0.046 0.048 0.050 0.017 -0.021 -0.028 N19 0.036 0.034 0.053 0.009 -0.010 -0.013 N20 0.078 0.093 0.092 0.074 -0.003 -0.040 N21 0.049 0.004 0.126 0.005 -0.050 -0.001 N22 0.039 0.017 0.104 0.007 -0.050 -0.001 N23 0.020 0.008 0.109 -0.020 -0.026 0.006 N24 0.027 0.020 0.080 -0.022 -0.014 0.007 N25 0.100 0.044 0.100 -0.024 0.021 -0.011 N26 0.043 0.022 0.095 -0.014 -0.026 0.006 N27 0.038 0.045 0.105 -0.016 -0.025 -0.009 N28 0.043 0.022 0.087 0.006 -0.028 -0.017 N29 0.040 0.025 0.095 0.000 -0.035 -0.011 N30 0.087 0.069 0.099 0.003 -0.030 -0.050 N31 0.037 0.029 0.062 -0.013 -0.013 -0.012 N32 0.036 0.019 0.114 -0.002 -0.038 -0.014 N33 0.027 0.031 0.068 -0.027 -0.017 -0.003 N34 0.046 0.018 0.079 -0.014 -0.022 0.000 N35 0.061 0.043 0.088 -0.022 0.010 -0.016 N36 0.030 0.028 0.036 -0.013 -0.008 -0.003 N37 0.038 0.022 0.047 -0.011 -0.008 0.000 N38 0.032 0.013 0.042 -0.002 -0.017 0.001 N39 0.034 0.027 0.048 0.000 -0.010 -0.007 N40 0.058 0.056 0.070 0.014 0.000 -0.024 N41 0.024 0.027 0.036 -0.006 -0.007 -0.012 N42 0.024 0.021 0.033 -0.004 -0.009 -0.003 N43 0.030 0.021 0.034 0.002 -0.005 -0.007 N44 0.036 0.031 0.036 -0.009 -0.006 -0.003 N45 0.048 0.055 0.052 0.001 -0.002 -0.035 N46 0.025 0.017 0.043 -0.003 -0.007 -0.006 N47 0.022 0.036 0.026 0.001 -0.006 -0.010 N48 0.032 0.030 0.043 -0.007 0.000 -0.012 N49 0.022 0.017 0.040 0.002 -0.008 -0.009 N50 0.063 0.083 0.053 -0.003 -0.001 -0.055 N51 0.013 0.028 0.046 -0.018 0.000 -0.002 N52 0.015 0.028 0.052 -0.004 -0.003 -0.003 N53 0.025 0.023 0.031 0.000 -0.012 -0.006 N54 0.008 0.020 0.042 -0.012 0.000 0.000 N55 0.047 0.053 0.050 0.002 -0.002 -0.023 N56 0.030 0.021 0.041 -0.011 0.007 -0.007 N57 0.014 0.032 0.042 -0.007 -0.004 -0.003 N58 0.028 0.027 0.031 -0.010 0.005 -0.008 N59 0.031 0.032 0.027 -0.002 0.005 -0.012 N60 0.071 0.081 0.042 0.015 0.002 -0.041 N63 0.046 0.049 0.031 -0.002 -0.008 -0.030 N64 0.165 0.101 0.115 0.041 -0.086 -0.077 C1 0.052 0.052 0.055 -0.016 -0.005 -0.012 C2 0.050 0.053 0.049 -0.025 -0.007 -0.015 C3 0.038 0.047 0.050 -0.018 -0.002 -0.009 C4 0.068 0.066 0.060 -0.020 -0.010 -0.021 C5 0.067 0.070 0.075 -0.033 -0.006 -0.019 C6 0.021 0.022 0.025 -0.002 0.001 -0.004 C7 0.027 0.025 0.035 -0.002 -0.002 -0.012 C8 0.022 0.025 0.028 -0.006 -0.007 -0.012 C9 0.031 0.043 0.038 -0.007 -0.006 -0.012 C10 0.035 0.043 0.061 -0.014 -0.008 -0.021 C11 0.038 0.036 0.049 -0.009 -0.004 -0.016 C12 0.044 0.054 0.065 -0.015 0.003 -0.024 C13 0.047 0.047 0.077 -0.008 -0.009 -0.020 C14 0.047 0.046 0.042 -0.002 0.002 -0.006 C15 0.042 0.043 0.034 0.003 0.004 -0.010 C16 0.043 0.047 0.042 -0.008 -0.004 -0.007 C17 0.045 0.049 0.044 -0.011 -0.006 -0.006 C18 0.066 0.063 0.057 -0.006 -0.018 -0.009 C19 0.047 0.049 0.043 -0.010 -0.017 -0.010 C20 0.076 0.070 0.054 -0.024 -0.019 -0.019 C21 0.066 0.066 0.066 -0.003 -0.022 -0.003 C22 0.033 0.033 0.032 -0.011 0.000 -0.014 C23 0.032 0.032 0.033 -0.004 0.001 -0.010 C24 0.025 0.029 0.030 0.001 0.003 -0.008 C25 0.045 0.043 0.069 -0.010 -0.010 -0.011 C26 0.042 0.048 0.061 -0.009 -0.011 -0.015 C27 0.036 0.044 0.055 0.000 -0.005 -0.017 C28 0.065 0.067 0.099 -0.032 -0.007 -0.016 C29 0.047 0.046 0.069 -0.019 -0.004 -0.024 C30 0.048 0.046 0.075 0.013 -0.016 -0.025 C31 0.052 0.062 0.073 0.016 -0.003 -0.022 C32 0.053 0.051 0.051 0.008 0.001 -0.006 C33 0.075 0.050 0.099 -0.010 -0.018 -0.024 C34 0.089 0.064 0.102 -0.015 -0.020 -0.018 C35 0.068 0.048 0.087 -0.001 -0.020 -0.019 C36 0.083 0.063 0.127 -0.016 -0.014 -0.027 C37 0.075 0.070 0.098 0.015 -0.027 -0.025 C38 0.049 0.052 0.052 -0.009 -0.008 -0.007 C39 0.045 0.042 0.066 -0.015 0.004 -0.018 C40 0.044 0.031 0.062 -0.008 -0.002 -0.017 C41 0.055 0.051 0.081 -0.019 -0.017 -0.020 C42 0.057 0.053 0.095 -0.025 -0.013 -0.012 C43 0.045 0.044 0.076 -0.018 -0.006 -0.014 C44 0.068 0.065 0.101 -0.018 -0.012 -0.019 C45 0.072 0.075 0.113 -0.012 -0.007 -0.013 C46 0.042 0.044 0.075 -0.001 -0.015 -0.027 C47 0.050 0.045 0.080 0.010 -0.012 -0.024 C48 0.049 0.053 0.072 0.003 -0.015 -0.021 C49 0.038 0.039 0.070 -0.007 -0.020 -0.017 C50 0.056 0.037 0.077 -0.013 -0.005 -0.020 C51 0.048 0.034 0.078 -0.010 -0.018 -0.016 C52 0.047 0.051 0.085 -0.007 -0.012 -0.023 C53 0.052 0.041 0.102 -0.015 -0.017 -0.024 C54 0.044 0.034 0.046 -0.009 -0.003 -0.012 C55 0.051 0.041 0.057 -0.018 -0.008 -0.023 C56 0.043 0.041 0.071 -0.013 0.007 -0.019 C57 0.043 0.042 0.046 -0.009 -0.008 -0.013 C58 0.054 0.053 0.046 -0.013 -0.013 -0.012 C59 0.041 0.038 0.046 -0.012 -0.016 -0.010 C60 0.046 0.047 0.041 -0.005 -0.016 -0.005 C61 0.066 0.054 0.066 -0.024 -0.019 -0.012 C62 0.028 0.029 0.032 0.002 -0.007 -0.007 C63 0.045 0.032 0.042 0.006 -0.001 -0.015 C64 0.043 0.035 0.055 0.000 -0.008 -0.018 C65 0.023 0.036 0.028 -0.001 -0.005 -0.008 C66 0.023 0.031 0.030 -0.002 -0.007 -0.018 C67 0.032 0.028 0.043 -0.004 -0.001 -0.011 C68 0.032 0.045 0.050 -0.007 -0.004 -0.019 C69 0.038 0.038 0.053 -0.007 -0.002 -0.019 C70 0.033 0.029 0.039 -0.005 -0.003 -0.016 C71 0.040 0.045 0.037 -0.004 -0.006 -0.013 C72 0.037 0.038 0.032 -0.009 0.004 -0.008 C73 0.033 0.033 0.052 -0.004 -0.002 -0.014 C74 0.038 0.042 0.049 0.004 -0.006 -0.016 C75 0.036 0.039 0.047 -0.008 -0.010 -0.014 C76 0.044 0.049 0.059 -0.001 -0.008 -0.019 C77 0.045 0.051 0.051 -0.011 -0.013 -0.016 C78 0.031 0.036 0.033 -0.003 0.000 -0.009 C79 0.034 0.039 0.039 0.001 -0.003 -0.015 C80 0.033 0.026 0.032 -0.006 -0.005 -0.014 C81 0.044 0.042 0.049 -0.009 0.003 -0.012 C82 0.044 0.049 0.058 -0.004 0.008 -0.012 C83 0.037 0.043 0.050 -0.002 -0.006 -0.011 C84 0.060 0.053 0.053 -0.004 0.008 -0.012 C85 0.046 0.052 0.063 -0.002 -0.002 -0.013 C86 0.022 0.021 0.032 0.003 0.001 -0.009 C87 0.030 0.027 0.038 0.000 0.000 -0.011 C88 0.033 0.029 0.034 -0.002 -0.002 -0.009 C89 0.032 0.027 0.040 -0.008 -0.002 -0.014 C90 0.039 0.031 0.044 -0.005 0.001 -0.016 C91 0.036 0.035 0.045 -0.003 -0.002 -0.014 C92 0.045 0.039 0.053 -0.007 -0.002 -0.017 C93 0.054 0.059 0.070 -0.006 -0.004 -0.013 C94 0.047 0.044 0.043 -0.007 0.000 -0.010 C95 0.047 0.044 0.037 -0.006 0.001 -0.012 C96 0.041 0.042 0.036 -0.005 0.001 -0.012 C97 0.035 0.044 0.036 0.000 -0.011 -0.026 C98 0.038 0.062 0.044 0.000 -0.011 -0.018 C99 0.067 0.057 0.044 0.003 0.005 -0.024 C100 0.053 0.081 0.036 -0.003 0.009 -0.031 C101 0.054 0.066 0.056 -0.016 -0.011 -0.020 C102 0.041 0.062 0.041 -0.019 -0.001 -0.023 C103 0.039 0.057 0.045 0.003 -0.006 -0.014 C104 0.059 0.076 0.090 0.015 -0.012 -0.024 C105 0.076 0.111 0.091 0.026 -0.006 -0.035 C106 0.057 0.109 0.082 -0.001 -0.001 -0.033 C107 0.064 0.117 0.077 -0.009 0.010 -0.005 C108 0.049 0.076 0.059 0.000 -0.011 -0.007 C109 0.033 0.033 0.030 0.006 -0.012 -0.005 C110 0.043 0.035 0.067 -0.002 -0.001 -0.011 C111 0.053 0.042 0.091 -0.008 -0.006 -0.016 C112 0.063 0.058 0.066 -0.018 -0.017 -0.016 C113 0.057 0.058 0.074 -0.011 -0.016 0.003 C114 0.053 0.055 0.052 -0.009 -0.015 -0.007 C115 0.044 0.026 0.030 -0.002 0.001 -0.015 C116 0.047 0.031 0.032 0.002 0.005 -0.016 C117 0.057 0.045 0.039 -0.001 0.010 -0.017 C118 0.072 0.038 0.053 -0.010 0.003 -0.007 C119 0.049 0.037 0.050 -0.005 -0.005 -0.001 C120 0.052 0.034 0.041 0.000 0.007 -0.006 C121 0.033 0.016 0.026 -0.004 0.003 0.001 C122 0.039 0.031 0.044 -0.004 0.003 0.004 C123 0.045 0.032 0.069 -0.003 0.021 0.002 C124 0.074 0.041 0.067 -0.009 0.034 -0.014 C125 0.064 0.028 0.033 0.003 0.004 -0.011 C126 0.054 0.029 0.032 -0.008 0.007 -0.012 C127 0.023 0.028 0.038 0.001 -0.008 -0.006 C128 0.030 0.028 0.036 -0.007 -0.003 -0.009 C129 0.031 0.050 0.037 0.001 0.003 -0.008 C130 0.047 0.042 0.058 0.000 -0.006 -0.015 C131 0.042 0.037 0.045 -0.008 -0.009 -0.009 C132 0.037 0.031 0.041 -0.002 -0.007 -0.017 C133 0.057 0.098 0.078 0.033 0.001 -0.011 C134 0.057 0.098 0.078 0.033 0.001 -0.011 C135 0.057 0.098 0.078 0.033 0.001 -0.011 C136 0.057 0.098 0.078 0.033 0.001 -0.011 C137 0.057 0.098 0.078 0.033 0.001 -0.011 C138 0.057 0.098 0.078 0.033 0.001 -0.011 C139 0.099 0.137 0.098 0.024 0.012 -0.014 C140 0.099 0.137 0.098 0.024 0.012 -0.014 C141 0.099 0.137 0.098 0.024 0.012 -0.014 C142 0.099 0.137 0.098 0.024 0.012 -0.014 C143 0.099 0.137 0.098 0.024 0.012 -0.014 C144 0.099 0.137 0.098 0.024 0.012 -0.014 C145 0.072 0.072 0.080 -0.009 -0.022 -0.013 C146 0.203 0.103 0.091 0.014 -0.051 -0.038 C147 0.189 0.095 0.092 0.007 -0.040 -0.036 C148 0.057 0.085 0.099 0.017 0.001 -0.024 C149 0.111 0.095 0.105 -0.002 0.008 -0.033 C150 0.085 0.086 0.103 0.008 -0.012 -0.021 C151 0.091 0.126 0.120 0.021 -0.001 -0.020 C152 0.091 0.126 0.120 0.021 -0.001 -0.020 C153 0.091 0.126 0.120 0.021 -0.001 -0.020 C154 0.091 0.126 0.120 0.021 -0.001 -0.020 C155 0.103 0.192 0.107 0.039 -0.045 -0.014 C156 0.112 0.202 0.146 0.030 -0.066 -0.010 C157 0.108 0.078 0.060 -0.005 -0.019 -0.028 C158 0.121 0.125 0.094 -0.009 -0.036 -0.032 C159 0.141 0.115 0.102 -0.014 -0.014 -0.017 C160 0.123 0.107 0.109 -0.007 -0.008 -0.037 C161 0.148 0.123 0.130 -0.024 0.018 -0.061 C162 0.135 0.184 0.110 -0.002 0.032 -0.027 C163 0.073 0.078 0.082 -0.010 -0.003 -0.018 C164 0.104 0.171 0.155 0.050 0.003 0.020 C165 0.097 0.157 0.094 0.008 0.017 0.015 C166 0.083 0.147 0.124 -0.011 -0.005 -0.054 C167 0.091 0.102 0.089 -0.002 -0.014 -0.034 C168 0.137 0.094 0.089 0.011 -0.010 -0.027 C169 0.087 0.080 0.090 -0.012 -0.015 -0.021 C170 0.069 0.061 0.073 -0.007 -0.008 -0.015 C171 0.058 0.057 0.082 -0.013 -0.014 -0.027 C172 0.072 0.059 0.090 -0.001 -0.006 -0.030 C173 0.074 0.064 0.078 -0.019 -0.009 -0.027 C174 0.088 0.076 0.087 -0.007 0.003 -0.020 C175 0.091 0.084 0.106 0.013 -0.003 -0.045 C176 0.085 0.062 0.095 -0.010 0.012 -0.041 P1 0.034 0.043 0.029 0.004 -0.006 -0.018 P2 0.036 0.029 0.026 -0.002 -0.003 -0.015 P3 0.068 0.093 0.073 0.011 -0.026 -0.028 P4 0.073 0.109 0.076 0.027 -0.013 -0.038 N61 0.050 0.050 0.050 0.000 0.000 0.000 _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 O41 N65 1.35(2) . ? Co1 O34 1.898(11) . ? Co1 O1 1.907(11) . ? Co1 N58 1.913(14) . ? Co1 N4 1.917(14) . ? Co1 N56 1.921(14) . ? Co1 N2 1.924(14) . ? Co2 N9 1.898(15) . ? Co2 O4 1.911(10) . ? Co2 O1 1.918(11) . ? Co2 N3 1.926(14) . ? Co2 N1 1.927(13) . ? Co2 N7 1.936(14) . ? Co3 N8 1.882(14) . ? Co3 O4 1.894(10) . ? Co3 O7 1.909(11) . ? Co3 N14 1.914(15) . ? Co3 N6 1.922(14) . ? Co3 N12 1.924(14) . ? Co4 N13 1.913(14) . ? Co4 N19 1.917(15) . ? Co4 N11 1.921(15) . ? Co4 O10 1.927(11) . ? Co4 O7 1.933(12) . ? Co4 N17 1.939(15) . ? Co5 O13 1.890(12) . ? Co5 O10 1.904(10) . ? Co5 N22 1.916(14) . ? Co5 N24 1.920(19) . ? Co5 N16 1.923(16) . ? Co5 N18 1.939(18) . ? Co6 N29 1.883(19) . ? Co6 O16 1.894(13) . ? Co6 O13 1.909(13) . ? Co6 N23 1.926(18) . ? Co6 N27 1.95(2) . ? Co6 N21 1.972(15) . ? Co7 O16 1.894(12) . ? Co7 O19 1.91(3) . ? Co7 N28 1.917(18) . ? Co7 N32 1.920(14) . ? Co7 N26 1.931(18) . ? Co7 N34 1.935(19) . ? Co8 O19 1.90(3) . ? Co8 N39 1.908(16) . ? Co8 O22 1.913(10) . ? Co8 N37 1.916(15) . ? Co8 N31 1.919(14) . ? Co8 N33 1.925(18) . ? Co9 N44 1.898(15) . ? Co9 O25 1.909(11) . ? Co9 N38 1.916(14) . ? Co9 O22 1.919(11) . ? Co9 N42 1.930(14) . ? Co9 N36 1.942(13) . ? Co10 N43 1.891(14) . ? Co10 O28 1.900(10) . ? Co10 N47 1.910(13) . ? Co10 N49 1.912(14) . ? Co10 O25 1.925(11) . ? Co10 N41 1.927(13) . ? Co11 O28 1.900(10) . ? Co11 O31 1.902(11) . ? Co11 N48 1.903(15) . ? Co11 N54 1.911(13) . ? Co11 N46 1.924(14) . ? Co11 N52 1.941(14) . ? Co12 O31 1.892(10) . ? Co12 N59 1.901(14) . ? Co12 O34 1.907(10) . ? Co12 N53 1.917(14) . ? Co12 N51 1.932(13) . ? Co12 N57 1.943(14) . ? O2 N5 1.252(19) . ? O3 N5 1.237(19) . ? O5 N61 1.207(19) . ? O6 N61 1.192(19) . ? O8 N15 1.218(18) . ? O9 N15 1.240(18) . ? O11 N20 1.22(3) . ? O12 N20 1.24(4) . ? O14 N25 1.27(3) . ? O15 N25 1.27(3) . ? O17 N30 1.24(3) . ? O18 N30 1.25(3) . ? O20 N35 1.20(3) . ? O21 N35 1.24(2) . ? O23 N40 1.23(2) . ? O24 N40 1.24(2) . ? O26 N45 1.21(2) . ? O27 N45 1.21(2) . ? O29 N50 1.25(2) . ? O30 N50 1.19(2) . ? O32 N55 1.24(2) . ? O33 N55 1.20(2) . ? O35 N60 1.22(3) . ? O36 N60 1.21(2) . ? O37 C169 1.402(17) . ? O37 C172 1.448(16) . ? O38 C176 1.38(3) . ? O38 C173 1.50(2) . ? N1 C1 1.35(2) . ? N1 N2 1.38(2) . ? N2 C3 1.33(2) . ? N3 C6 1.32(2) . ? N3 N4 1.355(19) . ? N4 C8 1.30(2) . ? N5 C7 1.42(2) . ? N6 C9 1.34(2) . ? N6 N7 1.380(19) . ? N7 C11 1.34(2) . ? N8 C14 1.35(2) . ? N8 N9 1.37(2) . ? N9 C16 1.34(2) . ? N11 C17 1.34(2) . ? N11 N12 1.351(19) . ? N12 C19 1.35(2) . ? N13 C22 1.31(2) . ? N13 N14 1.346(18) . ? N14 C24 1.32(2) . ? N15 C23 1.40(2) . ? N16 C25 1.35(3) . ? N16 N17 1.386(19) . ? N17 C27 1.33(2) . ? N18 C30 1.33(3) . ? N18 N19 1.35(2) . ? N19 C32 1.32(3) . ? N20 C31 1.40(3) . ? N21 C33 1.33(3) . ? N21 N22 1.37(2) . ? N22 C35 1.33(3) . ? N23 C38 1.38(3) . ? N23 N24 1.39(2) . ? N24 C40 1.30(3) . ? N25 C39 1.38(3) . ? N26 C41 1.29(3) . ? N26 N27 1.40(2) . ? N27 C43 1.32(3) . ? N28 C46 1.31(3) . ? N28 N29 1.39(2) . ? N29 C48 1.31(3) . ? N30 C47 1.45(3) . ? N31 C49 1.35(2) . ? N31 N32 1.37(2) . ? N32 C51 1.36(2) . ? N33 C54 1.35(2) . ? N33 N34 1.39(2) . ? N34 C56 1.33(3) . ? N35 C55 1.40(3) . ? N36 C57 1.31(2) . ? N36 N37 1.384(19) . ? N37 C59 1.33(2) . ? N38 C62 1.33(2) . ? N38 N39 1.360(19) . ? N39 C64 1.32(2) . ? N40 C63 1.44(3) . ? N41 C65 1.35(2) . ? N41 N42 1.378(17) . ? N42 C67 1.34(2) . ? N43 C70 1.34(2) . ? N43 N44 1.406(18) . ? N44 C72 1.33(2) . ? N45 C71 1.42(3) . ? N46 C73 1.33(2) . ? N46 N47 1.398(18) . ? N47 C75 1.33(2) . ? N48 N49 1.358(18) . ? N48 C78 1.36(2) . ? N49 C80 1.33(2) . ? N50 C79 1.47(3) . ? N51 C81 1.35(2) . ? N51 N52 1.376(19) . ? N52 C83 1.32(2) . ? N53 C86 1.30(2) . ? N53 N54 1.369(17) . ? N54 C88 1.32(2) . ? N55 C87 1.44(2) . ? N56 C89 1.35(2) . ? N56 N57 1.358(19) . ? N57 C91 1.33(2) . ? N58 C94 1.33(2) . ? N58 N59 1.359(19) . ? N59 C96 1.36(2) . ? N60 C95 1.44(3) . ? N62 O39 1.242(12) . ? N62 O40 1.251(12) . ? N63 P1 1.582(15) . ? N63 P2 1.590(15) . ? N64 P3 1.57(2) . ? N64 P4 1.62(3) . ? C1 C2 1.40(3) . ? C1 C4 1.50(3) . ? C2 C3 1.38(3) . ? C3 C5 1.54(3) . ? C6 C7 1.38(2) . ? C7 C8 1.41(2) . ? C9 C10 1.39(3) . ? C9 C12 1.49(3) . ? C10 C11 1.38(3) . ? C11 C13 1.49(3) . ? C14 C15 1.36(3) . ? C15 C16 1.35(3) . ? C15 N61 1.441(19) . ? C17 C18 1.37(3) . ? C17 C21 1.52(3) . ? C18 C19 1.38(3) . ? C19 C20 1.49(3) . ? C22 C23 1.42(2) . ? C23 C24 1.37(2) . ? C25 C26 1.36(3) . ? C25 C28 1.50(3) . ? C26 C27 1.36(3) . ? C27 C29 1.49(3) . ? C30 C31 1.37(3) . ? C31 C32 1.37(3) . ? C33 C34 1.35(4) . ? C33 C36 1.52(3) . ? C34 C35 1.36(3) . ? C35 C37 1.48(4) . ? C38 C39 1.39(3) . ? C39 C40 1.40(3) . ? C41 C42 1.40(3) . ? C41 C44 1.52(3) . ? C42 C43 1.42(3) . ? C43 C45 1.51(4) . ? C46 C47 1.39(3) . ? C47 C48 1.38(3) . ? C49 C50 1.40(3) . ? C49 C52 1.49(3) . ? C50 C51 1.38(3) . ? C51 C53 1.47(3) . ? C54 C55 1.35(3) . ? C55 C56 1.36(3) . ? C57 C58 1.38(3) . ? C57 C60 1.54(3) . ? C58 C59 1.35(3) . ? C59 C61 1.51(3) . ? C62 C63 1.36(2) . ? C63 C64 1.35(3) . ? C65 C66 1.38(2) . ? C65 C68 1.51(2) . ? C66 C67 1.35(2) . ? C67 C69 1.51(2) . ? C70 C71 1.36(3) . ? C71 C72 1.39(3) . ? C73 C74 1.36(3) . ? C73 C76 1.51(3) . ? C74 C75 1.41(3) . ? C75 C77 1.50(2) . ? C78 C79 1.34(2) . ? C79 C80 1.36(2) . ? C81 C82 1.36(3) . ? C81 C84 1.53(3) . ? C82 C83 1.42(3) . ? C83 C85 1.51(3) . ? C86 C87 1.37(2) . ? C87 C88 1.38(2) . ? C89 C90 1.39(3) . ? C89 C92 1.48(3) . ? C90 C91 1.36(2) . ? C91 C93 1.50(3) . ? C94 C95 1.39(3) . ? C95 C96 1.39(3) . ? C97 C98 1.3900 . ? C97 C102 1.3900 . ? C97 P1 1.7896 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? C100 C101 1.3900 . ? C101 C102 1.3900 . ? C103 C104 1.3899 . ? C103 C108 1.3901 . ? C103 P1 1.8220 . ? C104 C105 1.3901 . ? C105 C106 1.3901 . ? C106 C107 1.3899 . ? C107 C108 1.3901 . ? C109 C110 1.3897 . ? C109 C114 1.3903 . ? C109 P1 1.7900 . ? C110 C111 1.3901 . ? C111 C112 1.3901 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C115 C120 1.3900 . ? C115 C116 1.3900 . ? C115 P2 1.8091 . ? C116 C117 1.3899 . ? C117 C118 1.3901 . ? C118 C119 1.3899 . ? C119 C120 1.3901 . ? C121 C126 1.3898 . ? C121 C122 1.3899 . ? C121 P2 1.7901 . ? C122 C123 1.3901 . ? C123 C124 1.3899 . ? C124 C125 1.3901 . ? C125 C126 1.3900 . ? C127 C132 1.3898 . ? C127 C128 1.3901 . ? C127 P2 1.7970 . ? C128 C129 1.3898 . ? C129 C130 1.3901 . ? C130 C131 1.3899 . ? C131 C132 1.3900 . ? C133 C134 1.3899 . ? C133 C138 1.3900 . ? C133 P3 1.6544 . ? C134 C135 1.3901 . ? C135 C136 1.3900 . ? C136 C137 1.3900 . ? C137 C138 1.3901 . ? C139 C140 1.3899 . ? C139 C144 1.3900 . ? C139 P3 1.7947 . ? C140 C141 1.3900 . ? C141 C142 1.3898 . ? C142 C143 1.3902 . ? C143 C144 1.3901 . ? C145 C146 1.3899 . ? C145 C150 1.3901 . ? C145 P3 1.8009 . ? C146 C147 1.3902 . ? C147 C148 1.3900 . ? C148 C149 1.3897 . ? C149 C150 1.3899 . ? C151 C152 1.3899 . ? C151 C156 1.3901 . ? C151 P4 1.7679 . ? C152 C153 1.3901 . ? C153 C154 1.3900 . ? C154 C155 1.3895 . ? C155 C156 1.3904 . ? C157 C158 1.3900 . ? C157 C162 1.3901 . ? C157 P4 1.7837 . ? C158 C159 1.3900 . ? C159 C160 1.3901 . ? C160 C161 1.3900 . ? C161 C162 1.3900 . ? C163 C168 1.3897 . ? C163 C164 1.3900 . ? C163 P4 1.7771 . ? C164 C165 1.3900 . ? C165 C166 1.3900 . ? C166 C167 1.3898 . ? C167 C168 1.3904 . ? C169 C170 1.5150 . ? C170 C171 1.5475 . ? C171 C172 1.4848 . ? C173 C174 1.5675 . ? C174 C175 1.5196 . ? C175 C176 1.4471 . ? O42 N65 1.2719 . ? 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 O34 Co1 O1 96.5(5) . . ? O34 Co1 N58 86.7(5) . . ? O1 Co1 N58 87.9(5) . . ? O34 Co1 N4 87.9(5) . . ? O1 Co1 N4 87.5(5) . . ? N58 Co1 N4 172.4(6) . . ? O34 Co1 N56 83.6(5) . . ? O1 Co1 N56 178.9(6) . . ? N58 Co1 N56 93.3(6) . . ? N4 Co1 N56 91.4(6) . . ? O34 Co1 N2 177.6(6) . . ? O1 Co1 N2 83.3(5) . . ? N58 Co1 N2 91.0(6) . . ? N4 Co1 N2 94.5(6) . . ? N56 Co1 N2 96.7(6) . . ? N9 Co2 O4 87.5(5) . . ? N9 Co2 O1 90.2(6) . . ? O4 Co2 O1 94.8(5) . . ? N9 Co2 N3 176.4(6) . . ? O4 Co2 N3 89.7(5) . . ? O1 Co2 N3 87.7(5) . . ? N9 Co2 N1 90.6(6) . . ? O4 Co2 N1 178.0(5) . . ? O1 Co2 N1 84.4(5) . . ? N3 Co2 N1 92.1(6) . . ? N9 Co2 N7 92.8(6) . . ? O4 Co2 N7 83.2(5) . . ? O1 Co2 N7 176.3(5) . . ? N3 Co2 N7 89.2(6) . . ? N1 Co2 N7 97.7(6) . . ? N8 Co3 O4 87.3(5) . . ? N8 Co3 O7 90.8(6) . . ? O4 Co3 O7 97.7(4) . . ? N8 Co3 N14 173.6(6) . . ? O4 Co3 N14 88.4(5) . . ? O7 Co3 N14 85.1(5) . . ? N8 Co3 N6 93.0(6) . . ? O4 Co3 N6 82.5(5) . . ? O7 Co3 N6 176.3(6) . . ? N14 Co3 N6 91.2(6) . . ? N8 Co3 N12 90.0(6) . . ? O4 Co3 N12 176.7(5) . . ? O7 Co3 N12 84.1(5) . . ? N14 Co3 N12 94.5(6) . . ? N6 Co3 N12 95.8(6) . . ? N13 Co4 N19 171.2(6) . . ? N13 Co4 N11 95.2(6) . . ? N19 Co4 N11 91.7(6) . . ? N13 Co4 O10 86.8(5) . . ? N19 Co4 O10 86.4(6) . . ? N11 Co4 O10 178.0(5) . . ? N13 Co4 O7 86.1(5) . . ? N19 Co4 O7 89.3(6) . . ? N11 Co4 O7 82.5(5) . . ? O10 Co4 O7 98.0(5) . . ? N13 Co4 N17 90.3(6) . . ? N19 Co4 N17 94.5(7) . . ? N11 Co4 N17 95.6(6) . . ? O10 Co4 N17 84.1(5) . . ? O7 Co4 N17 175.7(6) . . ? O13 Co5 O10 93.5(5) . . ? O13 Co5 N22 83.5(6) . . ? O10 Co5 N22 175.4(8) . . ? O13 Co5 N24 88.9(7) . . ? O10 Co5 N24 89.3(6) . . ? N22 Co5 N24 94.0(8) . . ? O13 Co5 N16 176.2(7) . . ? O10 Co5 N16 87.2(5) . . ? N22 Co5 N16 96.1(6) . . ? N24 Co5 N16 87.4(7) . . ? O13 Co5 N18 89.9(7) . . ? O10 Co5 N18 85.5(6) . . ? N22 Co5 N18 91.0(8) . . ? N24 Co5 N18 174.6(6) . . ? N16 Co5 N18 93.9(7) . . ? N29 Co6 O16 85.4(6) . . ? N29 Co6 O13 90.3(7) . . ? O16 Co6 O13 91.3(6) . . ? N29 Co6 N23 178.2(7) . . ? O16 Co6 N23 93.9(6) . . ? O13 Co6 N23 88.1(6) . . ? N29 Co6 N27 93.0(8) . . ? O16 Co6 N27 86.3(7) . . ? O13 Co6 N27 175.8(7) . . ? N23 Co6 N27 88.6(8) . . ? N29 Co6 N21 88.6(8) . . ? O16 Co6 N21 172.3(8) . . ? O13 Co6 N21 83.8(7) . . ? N23 Co6 N21 92.0(7) . . ? N27 Co6 N21 98.9(8) . . ? O16 Co7 O19 92.0(9) . . ? O16 Co7 N28 85.1(6) . . ? O19 Co7 N28 91.7(9) . . ? O16 Co7 N32 173.5(8) . . ? O19 Co7 N32 84.3(10) . . ? N28 Co7 N32 89.7(7) . . ? O16 Co7 N26 87.2(7) . . ? O19 Co7 N26 175.6(9) . . ? N28 Co7 N26 92.6(8) . . ? N32 Co7 N26 96.9(7) . . ? O16 Co7 N34 91.8(6) . . ? O19 Co7 N34 87.8(8) . . ? N28 Co7 N34 176.9(6) . . ? N32 Co7 N34 93.3(7) . . ? N26 Co7 N34 87.8(8) . . ? O19 Co8 N39 90.9(9) . . ? O19 Co8 O22 93.8(9) . . ? N39 Co8 O22 86.9(6) . . ? O19 Co8 N37 174.9(9) . . ? N39 Co8 N37 94.1(7) . . ? O22 Co8 N37 85.4(5) . . ? O19 Co8 N31 84.5(9) . . ? N39 Co8 N31 90.9(7) . . ? O22 Co8 N31 177.2(7) . . ? N37 Co8 N31 96.5(6) . . ? O19 Co8 N33 86.9(9) . . ? N39 Co8 N33 176.4(6) . . ? O22 Co8 N33 90.4(6) . . ? N37 Co8 N33 88.0(7) . . ? N31 Co8 N33 91.7(7) . . ? N44 Co9 O25 87.0(5) . . ? N44 Co9 N38 172.1(6) . . ? O25 Co9 N38 89.5(5) . . ? N44 Co9 O22 87.5(6) . . ? O25 Co9 O22 97.9(5) . . ? N38 Co9 O22 85.9(6) . . ? N44 Co9 N42 96.2(6) . . ? O25 Co9 N42 84.2(5) . . ? N38 Co9 N42 90.5(6) . . ? O22 Co9 N42 175.8(5) . . ? N44 Co9 N36 89.7(6) . . ? O25 Co9 N36 176.5(5) . . ? N38 Co9 N36 93.9(6) . . ? O22 Co9 N36 83.2(6) . . ? N42 Co9 N36 94.8(6) . . ? N43 Co10 O28 88.6(5) . . ? N43 Co10 N47 89.8(6) . . ? O28 Co10 N47 82.6(5) . . ? N43 Co10 N49 173.4(6) . . ? O28 Co10 N49 86.5(5) . . ? N47 Co10 N49 93.9(6) . . ? N43 Co10 O25 86.9(5) . . ? O28 Co10 O25 97.9(4) . . ? N47 Co10 O25 176.7(6) . . ? N49 Co10 O25 89.4(5) . . ? N43 Co10 N41 94.4(6) . . ? O28 Co10 N41 176.8(5) . . ? N47 Co10 N41 96.3(6) . . ? N49 Co10 N41 90.6(6) . . ? O25 Co10 N41 83.4(5) . . ? O28 Co11 O31 94.3(5) . . ? O28 Co11 N48 87.2(5) . . ? O31 Co11 N48 90.6(6) . . ? O28 Co11 N54 90.6(5) . . ? O31 Co11 N54 87.4(5) . . ? N48 Co11 N54 176.9(6) . . ? O28 Co11 N46 84.6(5) . . ? O31 Co11 N46 177.1(5) . . ? N48 Co11 N46 92.0(6) . . ? N54 Co11 N46 90.0(6) . . ? O28 Co11 N52 175.4(5) . . ? O31 Co11 N52 83.2(5) . . ? N48 Co11 N52 89.0(6) . . ? N54 Co11 N52 93.1(6) . . ? N46 Co11 N52 98.2(6) . . ? O31 Co12 N59 90.4(5) . . ? O31 Co12 O34 94.9(5) . . ? N59 Co12 O34 85.3(6) . . ? O31 Co12 N53 88.4(5) . . ? N59 Co12 N53 174.1(6) . . ? O34 Co12 N53 89.0(5) . . ? O31 Co12 N51 82.9(5) . . ? N59 Co12 N51 91.7(6) . . ? O34 Co12 N51 176.3(6) . . ? N53 Co12 N51 93.9(6) . . ? O31 Co12 N57 176.2(6) . . ? N59 Co12 N57 93.3(6) . . ? O34 Co12 N57 85.6(5) . . ? N53 Co12 N57 87.8(6) . . ? N51 Co12 N57 96.8(5) . . ? Co1 O1 Co2 109.2(5) . . ? Co3 O4 Co2 110.4(5) . . ? Co3 O7 Co4 109.2(6) . . ? Co5 O10 Co4 108.8(5) . . ? Co5 O13 Co6 109.9(7) . . ? Co6 O16 Co7 110.5(6) . . ? Co8 O19 Co7 110.0(16) . . ? Co8 O22 Co9 109.4(5) . . ? Co9 O25 Co10 109.1(5) . . ? Co10 O28 Co11 110.6(5) . . ? Co12 O31 Co11 110.2(5) . . ? Co1 O34 Co12 109.9(5) . . ? C169 O37 C172 109.6(10) . . ? C176 O38 C173 108.0(19) . . ? C1 N1 N2 108.8(15) . . ? C1 N1 Co2 133.1(13) . . ? N2 N1 Co2 116.5(10) . . ? C3 N2 N1 107.3(14) . . ? C3 N2 Co1 135.2(13) . . ? N1 N2 Co1 117.1(9) . . ? C6 N3 N4 109.9(14) . . ? C6 N3 Co2 132.0(11) . . ? N4 N3 Co2 116.9(11) . . ? C8 N4 N3 109.8(14) . . ? C8 N4 Co1 131.6(12) . . ? N3 N4 Co1 117.6(11) . . ? O3 N5 O2 123.8(14) . . ? O3 N5 C7 119.3(15) . . ? O2 N5 C7 116.9(15) . . ? C9 N6 N7 107.9(14) . . ? C9 N6 Co3 133.5(12) . . ? N7 N6 Co3 117.8(10) . . ? C11 N7 N6 108.5(15) . . ? C11 N7 Co2 133.9(13) . . ? N6 N7 Co2 115.9(10) . . ? C14 N8 N9 106.3(14) . . ? C14 N8 Co3 134.0(13) . . ? N9 N8 Co3 119.0(10) . . ? C16 N9 N8 108.0(15) . . ? C16 N9 Co2 135.4(14) . . ? N8 N9 Co2 116.3(11) . . ? C17 N11 N12 109.1(15) . . ? C17 N11 Co4 133.9(12) . . ? N12 N11 Co4 116.7(10) . . ? C19 N12 N11 108.5(15) . . ? C19 N12 Co3 131.2(13) . . ? N11 N12 Co3 118.0(10) . . ? C22 N13 N14 110.5(14) . . ? C22 N13 Co4 125.9(11) . . ? N14 N13 Co4 117.8(11) . . ? C24 N14 N13 108.3(14) . . ? C24 N14 Co3 132.0(12) . . ? N13 N14 Co3 117.5(11) . . ? O8 N15 O9 124.3(15) . . ? O8 N15 C23 119.0(15) . . ? O9 N15 C23 116.7(15) . . ? C25 N16 N17 106.6(15) . . ? C25 N16 Co5 136.2(13) . . ? N17 N16 Co5 115.7(11) . . ? C27 N17 N16 108.6(15) . . ? C27 N17 Co4 133.8(13) . . ? N16 N17 Co4 117.1(11) . . ? C30 N18 N19 109.2(18) . . ? C30 N18 Co5 133.6(15) . . ? N19 N18 Co5 116.5(12) . . ? C32 N19 N18 108.2(16) . . ? C32 N19 Co4 132.7(15) . . ? N18 N19 Co4 117.7(13) . . ? O11 N20 O12 124(2) . . ? O11 N20 C31 117(3) . . ? O12 N20 C31 119(2) . . ? C33 N21 N22 107.1(17) . . ? C33 N21 Co6 133.6(15) . . ? N22 N21 Co6 116.4(10) . . ? C35 N22 N21 108.3(15) . . ? C35 N22 Co5 135.8(15) . . ? N21 N22 Co5 115.9(10) . . ? C38 N23 N24 109.0(17) . . ? C38 N23 Co6 135.8(14) . . ? N24 N23 Co6 115.2(14) . . ? C40 N24 N23 108.1(18) . . ? C40 N24 Co5 134.1(14) . . ? N23 N24 Co5 117.6(14) . . ? O15 N25 O14 121(3) . . ? O15 N25 C39 119(2) . . ? O14 N25 C39 119(3) . . ? C41 N26 N27 107.4(19) . . ? C41 N26 Co7 134.9(16) . . ? N27 N26 Co7 116.4(14) . . ? C43 N27 N26 109.9(19) . . ? C43 N27 Co6 133.2(15) . . ? N26 N27 Co6 116.0(14) . . ? C46 N28 N29 109.2(18) . . ? C46 N28 Co7 135.0(14) . . ? N29 N28 Co7 115.7(13) . . ? C48 N29 N28 108.3(18) . . ? C48 N29 Co6 133.2(14) . . ? N28 N29 Co6 118.4(14) . . ? O17 N30 O18 123(2) . . ? O17 N30 C47 119(2) . . ? O18 N30 C47 118(2) . . ? C49 N31 N32 108.3(14) . . ? C49 N31 Co8 133.8(14) . . ? N32 N31 Co8 116.6(11) . . ? C51 N32 N31 108.4(15) . . ? C51 N32 Co7 132.6(13) . . ? N31 N32 Co7 117.8(10) . . ? C54 N33 N34 105.8(17) . . ? C54 N33 Co8 134.7(13) . . ? N34 N33 Co8 119.0(14) . . ? C56 N34 N33 109.3(18) . . ? C56 N34 Co7 136.4(16) . . ? N33 N34 Co7 114.2(15) . . ? O20 N35 O21 122(2) . . ? O20 N35 C55 119(2) . . ? O21 N35 C55 118(2) . . ? C57 N36 N37 110.0(14) . . ? C57 N36 Co9 131.7(13) . . ? N37 N36 Co9 117.3(11) . . ? C59 N37 N36 106.1(14) . . ? C59 N37 Co8 136.4(13) . . ? N36 N37 Co8 116.3(10) . . ? C62 N38 N39 108.1(14) . . ? C62 N38 Co9 132.6(11) . . ? N39 N38 Co9 118.7(12) . . ? C64 N39 N38 108.6(16) . . ? C64 N39 Co8 134.5(14) . . ? N38 N39 Co8 116.4(11) . . ? O23 N40 O24 123.0(19) . . ? O23 N40 C63 119.8(18) . . ? O24 N40 C63 117(2) . . ? C65 N41 N42 107.8(12) . . ? C65 N41 Co10 133.9(11) . . ? N42 N41 Co10 117.7(10) . . ? C67 N42 N41 108.8(13) . . ? C67 N42 Co9 134.6(11) . . ? N41 N42 Co9 116.0(9) . . ? C70 N43 N44 106.3(14) . . ? C70 N43 Co10 133.2(12) . . ? N44 N43 Co10 118.0(10) . . ? C72 N44 N43 109.0(14) . . ? C72 N44 Co9 133.8(12) . . ? N43 N44 Co9 115.9(11) . . ? O26 N45 O27 124.1(19) . . ? O26 N45 C71 117.7(18) . . ? O27 N45 C71 118.1(17) . . ? C73 N46 N47 107.7(14) . . ? C73 N46 Co11 135.0(11) . . ? N47 N46 Co11 115.3(9) . . ? C75 N47 N46 107.3(13) . . ? C75 N47 Co10 134.2(12) . . ? N46 N47 Co10 118.0(10) . . ? N49 N48 C78 108.5(13) . . ? N49 N48 Co11 117.3(11) . . ? C78 N48 Co11 133.6(12) . . ? C80 N49 N48 106.4(14) . . ? C80 N49 Co10 135.5(11) . . ? N48 N49 Co10 117.8(10) . . ? O30 N50 O29 127(2) . . ? O30 N50 C79 119.3(18) . . ? O29 N50 C79 114.0(17) . . ? C81 N51 N52 108.5(14) . . ? C81 N51 Co12 135.3(13) . . ? N52 N51 Co12 115.7(10) . . ? C83 N52 N51 108.7(14) . . ? C83 N52 Co11 132.2(13) . . ? N51 N52 Co11 117.4(10) . . ? C86 N53 N54 108.7(13) . . ? C86 N53 Co12 134.0(11) . . ? N54 N53 Co12 116.9(10) . . ? C88 N54 N53 108.3(13) . . ? C88 N54 Co11 134.6(11) . . ? N53 N54 Co11 117.1(10) . . ? O33 N55 O32 123.4(19) . . ? O33 N55 C87 119.4(17) . . ? O32 N55 C87 117.2(17) . . ? C89 N56 N57 108.4(14) . . ? C89 N56 Co1 133.1(12) . . ? N57 N56 Co1 118.3(10) . . ? C91 N57 N56 109.3(13) . . ? C91 N57 Co12 133.4(12) . . ? N56 N57 Co12 115.4(10) . . ? C94 N58 N59 108.9(14) . . ? C94 N58 Co1 132.2(14) . . ? N59 N58 Co1 117.1(11) . . ? C96 N59 N58 109.1(14) . . ? C96 N59 Co12 133.2(13) . . ? N58 N59 Co12 117.4(10) . . ? O36 N60 O35 126(2) . . ? O36 N60 C95 116.3(19) . . ? O35 N60 C95 118.0(19) . . ? O39 N62 O40 107.3(8) . . ? P1 N63 P2 133.0(9) . . ? P3 N64 P4 143(2) . . ? N1 C1 C2 108.2(19) . . ? N1 C1 C4 124(2) . . ? C2 C1 C4 128(2) . . ? C3 C2 C1 105.2(17) . . ? N2 C3 C2 110.5(17) . . ? N2 C3 C5 124.6(18) . . ? C2 C3 C5 124.8(18) . . ? N3 C6 C7 106.3(14) . . ? C6 C7 C8 107.3(14) . . ? C6 C7 N5 126.2(16) . . ? C8 C7 N5 126.2(15) . . ? N4 C8 C7 106.7(14) . . ? N6 C9 C10 108.6(16) . . ? N6 C9 C12 124.8(17) . . ? C10 C9 C12 126.5(18) . . ? C11 C10 C9 106.2(16) . . ? N7 C11 C10 108.8(16) . . ? N7 C11 C13 124.7(18) . . ? C10 C11 C13 126.4(17) . . ? N8 C14 C15 109.8(17) . . ? C16 C15 C14 106.3(18) . . ? C16 C15 N61 126.9(17) . . ? C14 C15 N61 126.8(16) . . ? N9 C16 C15 109.5(18) . . ? N11 C17 C18 107.6(18) . . ? N11 C17 C21 123.8(18) . . ? C18 C17 C21 129(2) . . ? C17 C18 C19 108(2) . . ? N12 C19 C18 107.2(17) . . ? N12 C19 C20 126.6(18) . . ? C18 C19 C20 126.0(19) . . ? N13 C22 C23 106.5(15) . . ? C24 C23 N15 129.7(16) . . ? C24 C23 C22 105.5(15) . . ? N15 C23 C22 124.6(15) . . ? N14 C24 C23 109.1(15) . . ? N16 C25 C26 108.7(18) . . ? N16 C25 C28 125.0(19) . . ? C26 C25 C28 126(2) . . ? C25 C26 C27 108(2) . . ? N17 C27 C26 108.1(17) . . ? N17 C27 C29 123.9(18) . . ? C26 C27 C29 127.9(19) . . ? N18 C30 C31 107.5(19) . . ? C30 C31 C32 107(2) . . ? C30 C31 N20 126(2) . . ? C32 C31 N20 127(3) . . ? N19 C32 C31 108(2) . . ? N21 C33 C34 109(2) . . ? N21 C33 C36 124(2) . . ? C34 C33 C36 126(3) . . ? C33 C34 C35 107(3) . . ? N22 C35 C34 108(2) . . ? N22 C35 C37 125(2) . . ? C34 C35 C37 126(2) . . ? N23 C38 C39 105.8(19) . . ? N25 C39 C38 125(2) . . ? N25 C39 C40 128(2) . . ? C38 C39 C40 107(2) . . ? N24 C40 C39 109.5(18) . . ? N26 C41 C42 111(2) . . ? N26 C41 C44 127(2) . . ? C42 C41 C44 122(2) . . ? C41 C42 C43 105(2) . . ? N27 C43 C42 107(2) . . ? N27 C43 C45 125(2) . . ? C42 C43 C45 128(2) . . ? N28 C46 C47 107.0(18) . . ? C48 C47 C46 108(2) . . ? C48 C47 N30 127(2) . . ? C46 C47 N30 125(2) . . ? N29 C48 C47 108(2) . . ? N31 C49 C50 108.3(17) . . ? N31 C49 C52 125.6(18) . . ? C50 C49 C52 126.0(18) . . ? C51 C50 C49 106.3(17) . . ? N32 C51 C50 108.5(18) . . ? N32 C51 C53 124.3(18) . . ? C50 C51 C53 127.2(18) . . ? N33 C54 C55 109.0(18) . . ? C54 C55 C56 108(2) . . ? C54 C55 N35 126(2) . . ? C56 C55 N35 126(2) . . ? N34 C56 C55 108(2) . . ? N36 C57 C58 106.7(17) . . ? N36 C57 C60 125.9(17) . . ? C58 C57 C60 127.3(18) . . ? C59 C58 C57 107.7(18) . . ? N37 C59 C58 109.3(17) . . ? N37 C59 C61 123.4(17) . . ? C58 C59 C61 126.8(19) . . ? N38 C62 C63 107.0(16) . . ? C64 C63 C62 108.4(17) . . ? C64 C63 N40 126.7(18) . . ? C62 C63 N40 125.0(18) . . ? N39 C64 C63 107.8(17) . . ? N41 C65 C66 107.0(14) . . ? N41 C65 C68 123.3(15) . . ? C66 C65 C68 129.7(16) . . ? C67 C66 C65 108.8(15) . . ? N42 C67 C66 107.7(14) . . ? N42 C67 C69 124.9(16) . . ? C66 C67 C69 127.3(16) . . ? N43 C70 C71 109.8(16) . . ? C70 C71 C72 107.2(17) . . ? C70 C71 N45 127.1(17) . . ? C72 C71 N45 125.7(18) . . ? N44 C72 C71 107.7(16) . . ? N46 C73 C74 110.7(16) . . ? N46 C73 C76 124.3(17) . . ? C74 C73 C76 124.9(18) . . ? C73 C74 C75 105.0(17) . . ? N47 C75 C74 109.2(16) . . ? N47 C75 C77 124.1(16) . . ? C74 C75 C77 126.5(18) . . ? C79 C78 N48 108.1(16) . . ? C78 C79 C80 106.7(17) . . ? C78 C79 N50 126.5(17) . . ? C80 C79 N50 126.8(16) . . ? N49 C80 C79 110.3(14) . . ? N51 C81 C82 108.4(18) . . ? N51 C81 C84 122.8(19) . . ? C82 C81 C84 129(2) . . ? C81 C82 C83 106.7(19) . . ? N52 C83 C82 107.6(17) . . ? N52 C83 C85 127.2(18) . . ? C82 C83 C85 125.1(19) . . ? N53 C86 C87 108.5(14) . . ? C86 C87 C88 106.9(16) . . ? C86 C87 N55 126.4(15) . . ? C88 C87 N55 126.7(17) . . ? N54 C88 C87 107.5(16) . . ? N56 C89 C90 106.2(15) . . ? N56 C89 C92 125.1(16) . . ? C90 C89 C92 128.7(16) . . ? C91 C90 C89 108.3(16) . . ? N57 C91 C90 107.6(17) . . ? N57 C91 C93 125.2(17) . . ? C90 C91 C93 126.9(18) . . ? N58 C94 C95 108.1(18) . . ? C94 C95 C96 107.2(18) . . ? C94 C95 N60 126.0(19) . . ? C96 C95 N60 126.8(19) . . ? N59 C96 C95 106.5(18) . . ? C98 C97 C102 120.0 . . ? C98 C97 P1 121.0 . . ? C102 C97 P1 119.0 . . ? C99 C98 C97 120.0 . . ? C98 C99 C100 120.0 . . ? C101 C100 C99 120.0 . . ? C100 C101 C102 120.0 . . ? C101 C102 C97 120.0 . . ? C104 C103 C108 120.0 . . ? C104 C103 P1 117.9 . . ? C108 C103 P1 122.0 . . ? C103 C104 C105 120.0 . . ? C106 C105 C104 120.0 . . ? C107 C106 C105 120.0 . . ? C106 C107 C108 120.0 . . ? C103 C108 C107 120.0 . . ? C110 C109 C114 120.0 . . ? C110 C109 P1 122.7 . . ? C114 C109 P1 117.2 . . ? C109 C110 C111 120.0 . . ? C112 C111 C110 120.0 . . ? C113 C112 C111 120.0 . . ? C112 C113 C114 120.0 . . ? C113 C114 C109 120.0 . . ? C120 C115 C116 120.0 . . ? C120 C115 P2 121.5 . . ? C116 C115 P2 118.5 . . ? C117 C116 C115 120.0 . . ? C116 C117 C118 120.0 . . ? C119 C118 C117 120.0 . . ? C118 C119 C120 120.0 . . ? C115 C120 C119 120.0 . . ? C126 C121 C122 120.0 . . ? C126 C121 P2 121.4 . . ? C122 C121 P2 118.1 . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C123 C124 C125 120.0 . . ? C126 C125 C124 120.0 . . ? C121 C126 C125 120.0 . . ? C132 C127 C128 120.0 . . ? C132 C127 P2 121.5 . . ? C128 C127 P2 118.2 . . ? C129 C128 C127 120.0 . . ? C128 C129 C130 120.0 . . ? C131 C130 C129 120.0 . . ? C130 C131 C132 120.0 . . ? C127 C132 C131 120.0 . . ? C134 C133 C138 120.0 . . ? C134 C133 P3 121.0 . . ? C138 C133 P3 118.8 . . ? C133 C134 C135 120.0 . . ? C136 C135 C134 120.0 . . ? C137 C136 C135 120.0 . . ? C136 C137 C138 120.0 . . ? C133 C138 C137 120.0 . . ? C140 C139 C144 120.0 . . ? C140 C139 P3 122.0 . . ? C144 C139 P3 118.0 . . ? C139 C140 C141 120.0 . . ? C142 C141 C140 120.0 . . ? C141 C142 C143 120.0 . . ? C144 C143 C142 120.0 . . ? C139 C144 C143 120.0 . . ? C146 C145 C150 120.0 . . ? C146 C145 P3 121.4 . . ? C150 C145 P3 118.5 . . ? C145 C146 C147 120.0 . . ? C148 C147 C146 120.0 . . ? C149 C148 C147 120.0 . . ? C148 C149 C150 120.0 . . ? C149 C150 C145 120.0 . . ? C152 C151 C156 120.0 . . ? C152 C151 P4 115.1 . . ? C156 C151 P4 122.7 . . ? C151 C152 C153 120.0 . . ? C154 C153 C152 120.0 . . ? C155 C154 C153 120.0 . . ? C154 C155 C156 120.0 . . ? C151 C156 C155 120.0 . . ? C158 C157 C162 120.0 . . ? C158 C157 P4 119.6 . . ? C162 C157 P4 120.3 . . ? C159 C158 C157 120.0 . . ? C158 C159 C160 120.0 . . ? C161 C160 C159 120.0 . . ? C162 C161 C160 120.0 . . ? C161 C162 C157 120.0 . . ? C168 C163 C164 120.0 . . ? C168 C163 P4 122.4 . . ? C164 C163 P4 117.4 . . ? C165 C164 C163 120.0 . . ? C164 C165 C166 120.0 . . ? C167 C166 C165 120.0 . . ? C166 C167 C168 120.0 . . ? C163 C168 C167 120.0 . . ? O37 C169 C170 108.3(6) . . ? C169 C170 C171 105.6 . . ? C172 C171 C170 104.0 . . ? O37 C172 C171 108.3(7) . . ? O38 C173 C174 100.5(11) . . ? C175 C174 C173 100.9 . . ? C176 C175 C174 109.4 . . ? O38 C176 C175 99.3(11) . . ? N63 P1 C97 109.6(6) . . ? N63 P1 C109 113.9(5) . . ? C97 P1 C109 109.9 . . ? N63 P1 C103 109.5(6) . . ? C97 P1 C103 104.8 . . ? C109 P1 C103 108.7 . . ? N63 P2 C121 110.3(6) . . ? N63 P2 C127 114.3(5) . . ? C121 P2 C127 110.5 . . ? N63 P2 C115 109.3(5) . . ? C121 P2 C115 105.4 . . ? C127 P2 C115 106.5 . . ? N64 P3 C133 112.6(11) . . ? N64 P3 C139 112.8(14) . . ? C133 P3 C139 102.8 . . ? N64 P3 C145 111.2(9) . . ? C133 P3 C145 111.2 . . ? C139 P3 C145 105.9 . . ? N64 P4 C151 110.4(9) . . ? N64 P4 C163 118.0(10) . . ? C151 P4 C163 109.5 . . ? N64 P4 C157 107.9(13) . . ? C151 P4 C157 105.5 . . ? C163 P4 C157 104.7 . . ? O42 N65 O41 123.3(10) . . ? O6 N61 O5 124.8(14) . . ? O6 N61 C15 116.6(13) . . ? O5 N61 C15 118.5(12) . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 28.66 _diffrn_measured_fraction_theta_full 0.840 _refine_diff_density_max 3.412 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.154 # Attachment 'Co3.cif' data_Co3 _database_code_depnum_ccdc_archive 'CCDC 767216' #TrackingRef 'Co3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H83 Co3 N23 O19' _chemical_formula_weight 1487.18 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.702(2) _cell_length_b 15.116(3) _cell_length_c 26.292(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.689(15) _cell_angle_gamma 90.00 _cell_volume 6889(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 931 _cell_measurement_theta_min 4.685 _cell_measurement_theta_max 49.411 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3108 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The low completeness of the data set reulted due to poor diffraction of the crystal. Several crystallisation effort didn't afforded any better crystals. Theta max used for this data set was 28.40. Lowering the theta max value did not improve the completeness. ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44232 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.40 _reflns_number_total 15458 _reflns_number_gt 8210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Some large and small thermal ellipsoids resulted in the disordered TBA counter ions, which in some cases could not be modeled properly even after applying common thermal restrains (like SIMU, DELU). ; _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^)+(0.0681P)^2^+0.0200P] 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 15458 _refine_ls_number_parameters 856 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1405 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.984 _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 C39 C 0.8519(3) 0.0140(4) 0.4521(3) 0.096(2) Uani 1 1 d D . . H39A H 0.9060 0.0279 0.4548 0.115 Uiso 1 1 calc R . . H39B H 0.8386 0.0319 0.4846 0.115 Uiso 1 1 calc R . . C40 C 0.8452(4) -0.0797(5) 0.4493(3) 0.125(3) Uani 1 1 d D . . H40A H 0.8581 -0.1004 0.4172 0.150 Uiso 1 1 calc R . . H40B H 0.7923 -0.0967 0.4492 0.150 Uiso 1 1 calc R . . C41 C 0.8984(5) -0.1228(6) 0.4949(4) 0.175(5) Uani 1 1 d DU . . H41A H 0.9495 -0.1272 0.4871 0.210 Uiso 1 1 calc R . . H41B H 0.9021 -0.0848 0.5250 0.210 Uiso 1 1 calc R . . C42 C 0.8760(7) -0.2047(8) 0.5073(6) 0.314(10) Uani 1 1 d DU . . H42A H 0.8210 -0.2101 0.4964 0.471 Uiso 1 1 calc R . . H42B H 0.8902 -0.2131 0.5442 0.471 Uiso 1 1 calc R . . H42C H 0.9008 -0.2487 0.4901 0.471 Uiso 1 1 calc R . . C47 C 0.8460(4) 0.0633(4) 0.3637(2) 0.103(2) Uani 1 1 d D . . H47A H 0.9004 0.0760 0.3758 0.124 Uiso 1 1 calc R . . H47B H 0.8424 0.0014 0.3536 0.124 Uiso 1 1 calc R . . C48 C 0.8208(5) 0.1138(4) 0.3175(3) 0.122(3) Uani 1 1 d D . . H48A H 0.8201 0.1759 0.3268 0.146 Uiso 1 1 calc R . . H48B H 0.7685 0.0966 0.3020 0.146 Uiso 1 1 calc R . . C49 C 0.8704(6) 0.1026(6) 0.2781(3) 0.168(4) Uani 1 1 d DU . . H49A H 0.9234 0.1081 0.2967 0.202 Uiso 1 1 calc R . . H49B H 0.8638 0.0419 0.2661 0.202 Uiso 1 1 calc R . . C50 C 0.8641(11) 0.1514(8) 0.2370(5) 0.340(10) Uani 1 1 d DU . . H50A H 0.8274 0.1961 0.2308 0.408 Uiso 1 1 calc R . . H50B H 0.8964 0.1416 0.2137 0.408 Uiso 1 1 calc R . . C31 C 0.3490(3) -0.0783(3) 0.93114(18) 0.0553(12) Uani 1 1 d D . . H31A H 0.3979 -0.0913 0.9214 0.066 Uiso 1 1 calc R . . H31B H 0.3575 -0.0812 0.9687 0.066 Uiso 1 1 calc R . . C32 C 0.2928(3) -0.1500(4) 0.9093(2) 0.0792(16) Uani 1 1 d D . . H32A H 0.2419 -0.1337 0.9144 0.095 Uiso 1 1 calc R . . H32B H 0.2905 -0.1545 0.8722 0.095 Uiso 1 1 calc R . . C33 C 0.3140(4) -0.2387(4) 0.9338(3) 0.096(2) Uani 1 1 d D . . H33A H 0.3638 -0.2562 0.9270 0.115 Uiso 1 1 calc R . . H33B H 0.3196 -0.2330 0.9711 0.115 Uiso 1 1 calc R . . C34 C 0.2575(4) -0.3101(4) 0.9154(3) 0.123(3) Uani 1 1 d D . . H34A H 0.2102 -0.2978 0.9265 0.185 Uiso 1 1 calc R . . H34B H 0.2779 -0.3657 0.9296 0.185 Uiso 1 1 calc R . . H34C H 0.2479 -0.3129 0.8782 0.185 Uiso 1 1 calc R . . C23 C 0.3902(3) 0.0764(3) 0.94307(17) 0.0575(13) Uani 1 1 d D . . H23A H 0.3938 0.0688 0.9801 0.069 Uiso 1 1 calc R . . H23B H 0.4388 0.0570 0.9352 0.069 Uiso 1 1 calc R . . C24 C 0.3804(4) 0.1741(4) 0.9305(2) 0.0846(17) Uani 1 1 d D . . H24A H 0.3291 0.1930 0.9333 0.101 Uiso 1 1 calc R . . H24B H 0.3865 0.1845 0.8951 0.101 Uiso 1 1 calc R . . C25 C 0.4417(6) 0.2287(5) 0.9688(3) 0.167(4) Uani 1 1 d DU . . H25A H 0.4896 0.1956 0.9771 0.200 Uiso 1 1 calc R . . H25B H 0.4518 0.2837 0.9524 0.200 Uiso 1 1 calc R . . C26 C 0.4162(10) 0.2469(8) 1.0140(4) 0.361(14) Uani 1 1 d D . . H26A H 0.4017 0.3081 1.0143 0.541 Uiso 1 1 calc R . . H26B H 0.4568 0.2350 1.0434 0.541 Uiso 1 1 calc R . . H26C H 0.3725 0.2103 1.0158 0.541 Uiso 1 1 calc R . . Co1 Co 0.25980(3) 0.17825(3) 0.219986(19) 0.03265(14) Uani 1 1 d . . . Co2 Co 0.20852(3) -0.01807(4) 0.22222(2) 0.03440(14) Uani 1 1 d . . . Co3 Co 0.27743(3) 0.07839(4) 0.324648(19) 0.03331(14) Uani 1 1 d . . . C1 C 0.0618(2) 0.0555(3) 0.15773(14) 0.0400(10) Uani 1 1 d . . . H1 H 0.0323 0.0042 0.1532 0.048 Uiso 1 1 calc R . . C2 C 0.0376(2) 0.1395(3) 0.14010(15) 0.0410(10) Uani 1 1 d . . . C3 C 0.0993(2) 0.1960(3) 0.15532(14) 0.0390(10) Uani 1 1 d . . . H3 H 0.0992 0.2565 0.1490 0.047 Uiso 1 1 calc R . . C4 C 0.1378(2) 0.0011(3) 0.35667(16) 0.0414(10) Uani 1 1 d . . . H4 H 0.1469 0.0213 0.3908 0.050 Uiso 1 1 calc R . . C5 C 0.0749(2) -0.0466(3) 0.33274(17) 0.0439(10) Uani 1 1 d . . . C6 C 0.0843(2) -0.0625(3) 0.28307(16) 0.0413(10) Uani 1 1 d . . . H6 H 0.0501 -0.0933 0.2577 0.050 Uiso 1 1 calc R . . C7 C 0.1699(2) 0.3044(3) 0.27409(16) 0.0403(10) Uani 1 1 d . . . H7 H 0.1557 0.3456 0.2476 0.048 Uiso 1 1 calc R . . C8 C 0.1466(2) 0.3049(3) 0.32096(16) 0.0441(11) Uani 1 1 d . . . C9 C 0.1809(2) 0.2320(3) 0.34871(16) 0.0418(10) Uani 1 1 d . . . H9 H 0.1752 0.2150 0.3817 0.050 Uiso 1 1 calc R . . C10 C 0.3156(2) -0.0362(3) 0.14644(15) 0.0442(11) Uani 1 1 d . . . H10 H 0.3109 -0.0968 0.1405 0.053 Uiso 1 1 calc R . . C11 C 0.3632(2) 0.0207(3) 0.12634(15) 0.0452(11) Uani 1 1 d . . . C12 C 0.3532(2) 0.1042(3) 0.14534(15) 0.0411(10) Uani 1 1 d . . . H12 H 0.3784 0.1554 0.1385 0.049 Uiso 1 1 calc R . . C13 C 0.3801(2) -0.0844(3) 0.33928(17) 0.0476(11) Uani 1 1 d . . . H13 H 0.4128 -0.0696 0.3705 0.057 Uiso 1 1 calc R . . C14 C 0.3829(3) -0.1614(3) 0.31205(18) 0.0515(12) Uani 1 1 d . . . C15 C 0.3245(2) -0.1563(3) 0.26878(17) 0.0476(11) Uani 1 1 d . . . H15 H 0.3120 -0.1997 0.2434 0.057 Uiso 1 1 calc R . . C16 C 0.4241(2) 0.2309(3) 0.26672(17) 0.0442(10) Uani 1 1 d . . . H16 H 0.4342 0.2670 0.2403 0.053 Uiso 1 1 calc R . . C17 C 0.4749(2) 0.2110(3) 0.31214(18) 0.0473(11) Uani 1 1 d . . . C18 C 0.4372(2) 0.1553(3) 0.34001(17) 0.0452(11) Uani 1 1 d . . . H18 H 0.4580 0.1305 0.3722 0.054 Uiso 1 1 calc R . . C19 C 0.2491(2) 0.0402(4) 0.92824(17) 0.0590(13) Uani 1 1 d . . . H19A H 0.2361 0.1001 0.9165 0.071 Uiso 1 1 calc R . . H19B H 0.2099 0.0014 0.9088 0.071 Uiso 1 1 calc R . . C20 C 0.2449(3) 0.0345(4) 0.98503(19) 0.0739(16) Uani 1 1 d . . . H20A H 0.2549 -0.0258 0.9971 0.089 Uiso 1 1 calc R . . H20B H 0.2840 0.0723 1.0053 0.089 Uiso 1 1 calc R . . C21 C 0.1670(3) 0.0626(5) 0.9928(2) 0.091(2) Uani 1 1 d . . . H21A H 0.1286 0.0212 0.9750 0.109 Uiso 1 1 calc R . . H21B H 0.1550 0.1204 0.9772 0.109 Uiso 1 1 calc R . . C22 C 0.1619(3) 0.0667(5) 1.0493(2) 0.114(3) Uani 1 1 d . . . H22A H 0.1776 0.0110 1.0656 0.171 Uiso 1 1 calc R . . H22B H 0.1098 0.0791 1.0521 0.171 Uiso 1 1 calc R . . H22C H 0.1953 0.1127 1.0662 0.171 Uiso 1 1 calc R . . C27 C 0.3170(3) 0.0272(4) 0.85661(16) 0.0592(13) Uani 1 1 d . . . H27A H 0.2777 -0.0140 0.8399 0.071 Uiso 1 1 calc R . . H27B H 0.2978 0.0865 0.8476 0.071 Uiso 1 1 calc R . . C28 C 0.3882(3) 0.0133(4) 0.83426(17) 0.0652(14) Uani 1 1 d . . . H28A H 0.4275 0.0557 0.8495 0.078 Uiso 1 1 calc R . . H28B H 0.4084 -0.0456 0.8430 0.078 Uiso 1 1 calc R . . C29 C 0.3704(4) 0.0243(4) 0.77637(19) 0.0883(19) Uani 1 1 d . . . H29A H 0.3488 0.0827 0.7679 0.106 Uiso 1 1 calc R . . H29B H 0.3316 -0.0189 0.7613 0.106 Uiso 1 1 calc R . . C30 C 0.4407(4) 0.0129(5) 0.7523(2) 0.110(2) Uani 1 1 d . . . H30A H 0.4779 0.0580 0.7652 0.164 Uiso 1 1 calc R . . H30B H 0.4258 0.0177 0.7152 0.164 Uiso 1 1 calc R . . H30C H 0.4632 -0.0443 0.7613 0.164 Uiso 1 1 calc R . . C35 C 0.7253(4) 0.0391(5) 0.3947(3) 0.103(2) Uani 1 1 d . . . H35A H 0.6987 0.0760 0.3664 0.124 Uiso 1 1 calc R . . H35B H 0.7267 -0.0205 0.3813 0.124 Uiso 1 1 calc R . . C36 C 0.6807(4) 0.0379(5) 0.4344(3) 0.110(2) Uani 1 1 d . . . H36A H 0.6707 0.0982 0.4440 0.132 Uiso 1 1 calc R . . H36B H 0.7096 0.0083 0.4650 0.132 Uiso 1 1 calc R . . C37 C 0.6018(4) -0.0115(5) 0.4150(3) 0.112(2) Uani 1 1 d . . . H37A H 0.5742 0.0160 0.3833 0.135 Uiso 1 1 calc R . . H37B H 0.6117 -0.0727 0.4074 0.135 Uiso 1 1 calc R . . C38 C 0.5570(4) -0.0081(7) 0.4527(3) 0.163(4) Uani 1 1 d . . . H38A H 0.5865 -0.0295 0.4851 0.244 Uiso 1 1 calc R . . H38B H 0.5120 -0.0442 0.4422 0.244 Uiso 1 1 calc R . . H38C H 0.5416 0.0520 0.4569 0.244 Uiso 1 1 calc R . . C43 C 0.8089(4) 0.1672(4) 0.4280(2) 0.0866(18) Uani 1 1 d . . . H43A H 0.7762 0.2008 0.4006 0.104 Uiso 1 1 calc R . . H43B H 0.7855 0.1701 0.4583 0.104 Uiso 1 1 calc R . . C44 C 0.8834(4) 0.2113(5) 0.4408(3) 0.103(2) Uani 1 1 d . . . H44A H 0.9048 0.2169 0.4098 0.124 Uiso 1 1 calc R . . H44B H 0.9188 0.1761 0.4659 0.124 Uiso 1 1 calc R . . C45 C 0.8747(4) 0.3043(5) 0.4637(3) 0.103(2) Uani 1 1 d . . . H45A H 0.8357 0.3376 0.4401 0.123 Uiso 1 1 calc R . . H45B H 0.8582 0.2985 0.4965 0.123 Uiso 1 1 calc R . . C46 C 0.9497(4) 0.3524(5) 0.4718(3) 0.128(3) Uani 1 1 d . . . H46A H 0.9871 0.3217 0.4972 0.192 Uiso 1 1 calc R . . H46B H 0.9430 0.4113 0.4838 0.192 Uiso 1 1 calc R . . H46C H 0.9672 0.3551 0.4396 0.192 Uiso 1 1 calc R . . N1 N 0.15826(17) 0.1495(2) 0.18039(11) 0.0339(7) Uani 1 1 d . . . N2 N 0.13495(16) 0.0619(2) 0.18222(11) 0.0339(7) Uani 1 1 d . . . N3 N -0.0376(2) 0.1628(3) 0.11293(15) 0.0597(11) Uani 1 1 d . . . N4 N 0.15003(17) -0.0269(2) 0.27727(12) 0.0368(8) Uani 1 1 d . . . N5 N 0.18330(17) 0.0138(2) 0.32323(12) 0.0352(8) Uani 1 1 d . . . N6 N 0.0120(2) -0.0718(3) 0.35574(18) 0.0561(10) Uani 1 1 d . . . N7 N 0.22339(17) 0.1908(2) 0.31945(12) 0.0339(7) Uani 1 1 d . . . N8 N 0.21568(17) 0.2354(2) 0.27291(12) 0.0348(8) Uani 1 1 d . . . N9 N 0.0974(2) 0.3682(3) 0.33795(17) 0.0579(11) Uani 1 1 d . . . N10 N 0.30129(16) 0.0981(2) 0.17502(11) 0.0353(8) Uani 1 1 d . . . N11 N 0.27766(17) 0.0108(2) 0.17566(12) 0.0365(8) Uani 1 1 d . . . N12 N 0.4125(2) -0.0027(4) 0.09226(15) 0.0623(12) Uani 1 1 d . . . N13 N 0.28931(18) -0.0797(2) 0.26939(12) 0.0395(8) Uani 1 1 d . . . N14 N 0.32335(17) -0.0350(2) 0.31392(12) 0.0378(8) Uani 1 1 d . . . N15 N 0.4347(3) -0.2333(4) 0.3252(2) 0.0813(14) Uani 1 1 d . . . N16 N 0.36655(16) 0.1432(2) 0.31332(12) 0.0358(8) Uani 1 1 d . . . N17 N 0.35841(17) 0.1896(2) 0.26714(12) 0.0358(8) Uani 1 1 d . . . N18 N 0.5523(2) 0.2430(3) 0.32818(19) 0.0667(12) Uani 1 1 d . . . N19 N 0.1661(2) -0.1226(2) 0.18598(13) 0.0479(9) Uani 1 1 d . . . N20 N 0.3078(2) 0.0776(2) 0.39910(13) 0.0444(9) Uani 1 1 d . . . N21 N 0.2715(2) 0.2848(3) 0.18198(14) 0.0475(9) Uani 1 1 d . . . N22 N 0.3266(2) 0.0162(3) 0.91468(13) 0.0514(9) Uani 1 1 d . . . N23 N 0.8076(2) 0.0723(3) 0.41078(16) 0.0639(11) Uani 1 1 d . . . O1 O -0.0497(2) 0.2406(3) 0.10030(17) 0.0946(14) Uani 1 1 d . . . O2 O -0.08563(18) 0.1049(3) 0.10257(14) 0.0798(11) Uani 1 1 d . . . O3 O -0.04334(18) -0.1080(2) 0.32885(14) 0.0711(10) Uani 1 1 d . . . O4 O 0.0151(2) -0.0534(3) 0.40176(15) 0.0786(11) Uani 1 1 d . . . O5 O 0.07798(19) 0.3556(3) 0.37906(14) 0.0797(11) Uani 1 1 d . . . O6 O 0.0774(2) 0.4323(3) 0.30978(15) 0.0818(12) Uani 1 1 d . . . O7 O 0.4517(2) 0.0550(3) 0.07743(14) 0.0773(11) Uani 1 1 d . . . O8 O 0.4126(2) -0.0793(3) 0.07771(16) 0.0980(14) Uani 1 1 d . . . O9 O 0.4239(3) -0.3006(3) 0.29937(19) 0.1096(16) Uani 1 1 d . . . O10 O 0.4877(3) -0.2240(3) 0.3621(2) 0.1260(19) Uani 1 1 d . . . O11 O 0.5931(2) 0.2093(3) 0.36564(19) 0.1041(15) Uani 1 1 d . . . O12 O 0.5732(2) 0.3026(3) 0.30329(16) 0.0967(14) Uani 1 1 d . . . O13 O 0.09750(19) -0.1401(2) 0.17996(13) 0.0672(9) Uani 1 1 d . . . O14 O 0.2092(2) -0.1736(2) 0.16825(14) 0.0745(10) Uani 1 1 d . . . O15 O 0.26418(19) 0.1029(2) 0.42711(11) 0.0663(10) Uani 1 1 d . . . O16 O 0.37218(18) 0.0515(2) 0.41980(12) 0.0706(10) Uani 1 1 d . . . O17 O 0.2232(2) 0.3439(2) 0.17707(14) 0.0695(10) Uani 1 1 d . . . O18 O 0.3289(2) 0.2970(2) 0.16385(15) 0.0813(11) Uani 1 1 d . . . O19 O 0.24913(13) 0.07967(16) 0.25519(9) 0.0333(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C39 0.066(4) 0.094(5) 0.122(5) 0.044(4) 0.005(3) 0.011(4) C40 0.091(5) 0.110(7) 0.174(8) 0.070(6) 0.028(5) 0.020(5) C41 0.111(6) 0.141(8) 0.255(11) 0.117(8) -0.008(7) 0.005(6) C42 0.231(13) 0.35(2) 0.40(2) 0.263(17) 0.158(14) 0.114(14) C47 0.159(6) 0.082(5) 0.071(4) -0.003(4) 0.027(4) -0.014(5) C48 0.208(8) 0.063(5) 0.098(5) 0.005(4) 0.040(6) 0.005(5) C49 0.336(13) 0.118(7) 0.076(5) 0.031(5) 0.100(7) 0.082(8) C50 0.73(3) 0.169(12) 0.215(13) -0.009(10) 0.312(18) -0.013(16) C31 0.054(3) 0.057(3) 0.055(3) 0.005(2) 0.012(2) 0.007(3) C32 0.070(4) 0.080(5) 0.089(4) -0.004(3) 0.017(3) -0.001(3) C33 0.111(5) 0.058(4) 0.125(5) -0.001(4) 0.037(4) -0.004(4) C34 0.130(6) 0.072(5) 0.183(8) -0.011(5) 0.069(6) -0.016(5) C23 0.054(3) 0.069(4) 0.049(3) 0.000(2) 0.008(2) -0.002(3) C24 0.107(5) 0.064(4) 0.080(4) 0.002(3) 0.012(3) -0.005(3) C25 0.320(13) 0.067(6) 0.106(6) -0.012(5) 0.028(8) -0.022(7) C26 0.75(4) 0.137(11) 0.144(10) 0.001(9) -0.041(17) -0.076(17) Co1 0.0283(3) 0.0313(3) 0.0393(3) 0.0005(2) 0.0090(2) 0.0002(2) Co2 0.0341(3) 0.0308(3) 0.0385(3) -0.0024(2) 0.0079(2) -0.0005(2) Co3 0.0278(3) 0.0344(3) 0.0374(3) -0.0003(2) 0.0058(2) -0.0019(2) C1 0.033(2) 0.047(3) 0.041(2) -0.004(2) 0.0083(17) -0.006(2) C2 0.030(2) 0.049(3) 0.043(2) 0.001(2) 0.0030(17) 0.005(2) C3 0.036(2) 0.038(3) 0.042(2) 0.0011(19) 0.0068(18) 0.0081(19) C4 0.042(2) 0.041(3) 0.044(2) 0.0024(19) 0.0142(19) 0.000(2) C5 0.033(2) 0.046(3) 0.056(3) 0.008(2) 0.0136(19) -0.004(2) C6 0.033(2) 0.036(3) 0.053(3) 0.001(2) 0.0056(18) -0.0047(19) C7 0.035(2) 0.034(3) 0.049(2) -0.0073(19) 0.0016(18) 0.0039(19) C8 0.034(2) 0.048(3) 0.048(2) -0.015(2) 0.0054(19) 0.007(2) C9 0.037(2) 0.047(3) 0.042(2) -0.009(2) 0.0070(18) -0.005(2) C10 0.046(2) 0.047(3) 0.039(2) -0.008(2) 0.0088(19) 0.014(2) C11 0.043(2) 0.059(3) 0.037(2) 0.002(2) 0.0163(19) 0.015(2) C12 0.034(2) 0.051(3) 0.040(2) 0.006(2) 0.0115(18) 0.003(2) C13 0.038(2) 0.053(3) 0.049(2) 0.006(2) 0.0031(19) 0.004(2) C14 0.052(3) 0.041(3) 0.064(3) 0.014(2) 0.019(2) 0.018(2) C15 0.052(3) 0.037(3) 0.059(3) -0.003(2) 0.022(2) 0.008(2) C16 0.036(2) 0.041(3) 0.058(3) -0.002(2) 0.016(2) -0.005(2) C17 0.028(2) 0.046(3) 0.067(3) -0.005(2) 0.009(2) -0.007(2) C18 0.034(2) 0.045(3) 0.053(3) -0.003(2) 0.0012(19) 0.002(2) C19 0.047(3) 0.073(4) 0.056(3) 0.002(2) 0.008(2) 0.018(2) C20 0.060(3) 0.102(5) 0.064(3) 0.009(3) 0.022(3) 0.023(3) C21 0.064(3) 0.151(6) 0.059(3) 0.000(4) 0.018(3) 0.024(4) C22 0.088(4) 0.197(8) 0.061(4) 0.000(4) 0.023(3) 0.052(5) C27 0.064(3) 0.071(4) 0.040(2) 0.006(2) 0.004(2) 0.010(3) C28 0.078(3) 0.071(4) 0.050(3) 0.003(3) 0.020(3) 0.006(3) C29 0.105(5) 0.112(5) 0.050(3) 0.009(3) 0.021(3) -0.010(4) C30 0.151(6) 0.116(6) 0.076(4) 0.003(4) 0.055(4) -0.004(5) C35 0.076(4) 0.109(6) 0.114(5) 0.026(4) -0.007(4) 0.003(4) C36 0.093(5) 0.130(7) 0.105(5) 0.028(5) 0.013(4) 0.020(5) C37 0.075(4) 0.147(7) 0.107(5) 0.012(5) -0.001(4) 0.004(5) C38 0.107(6) 0.299(13) 0.082(5) 0.044(6) 0.015(5) 0.035(7) C43 0.088(4) 0.086(5) 0.088(4) -0.009(4) 0.021(3) -0.004(4) C44 0.093(5) 0.123(6) 0.087(4) -0.016(4) 0.004(4) 0.009(4) C45 0.122(6) 0.092(5) 0.088(4) -0.024(4) 0.006(4) -0.011(4) C46 0.133(6) 0.128(7) 0.132(6) -0.039(5) 0.048(5) -0.022(6) N1 0.0339(17) 0.030(2) 0.0378(18) -0.0008(14) 0.0075(14) 0.0020(15) N2 0.0267(16) 0.037(2) 0.0382(17) -0.0021(15) 0.0080(13) -0.0004(15) N3 0.038(2) 0.072(3) 0.064(3) -0.001(2) -0.0011(18) 0.004(2) N4 0.0341(18) 0.033(2) 0.0413(18) -0.0020(15) 0.0042(14) -0.0049(15) N5 0.0308(16) 0.038(2) 0.0371(17) 0.0004(15) 0.0079(14) -0.0067(15) N6 0.044(2) 0.049(3) 0.080(3) 0.006(2) 0.023(2) -0.006(2) N7 0.0315(17) 0.033(2) 0.0370(17) -0.0039(15) 0.0070(14) -0.0002(15) N8 0.0339(17) 0.029(2) 0.0416(18) -0.0013(15) 0.0090(14) -0.0003(15) N9 0.043(2) 0.070(3) 0.059(3) -0.024(2) 0.007(2) 0.012(2) N10 0.0301(16) 0.040(2) 0.0388(18) -0.0002(15) 0.0135(14) 0.0033(15) N11 0.0330(17) 0.036(2) 0.0408(18) -0.0035(15) 0.0085(14) 0.0024(16) N12 0.056(2) 0.084(4) 0.051(2) -0.001(2) 0.020(2) 0.024(3) N13 0.0398(18) 0.032(2) 0.047(2) -0.0018(16) 0.0101(15) 0.0028(16) N14 0.0318(17) 0.036(2) 0.0451(19) 0.0033(16) 0.0062(15) 0.0006(15) N15 0.083(3) 0.073(4) 0.089(4) 0.023(3) 0.019(3) 0.041(3) N16 0.0279(17) 0.035(2) 0.0436(19) 0.0015(15) 0.0055(14) -0.0044(14) N17 0.0298(17) 0.034(2) 0.0447(19) -0.0011(15) 0.0097(14) -0.0038(15) N18 0.037(2) 0.072(3) 0.088(3) -0.011(3) 0.007(2) -0.018(2) N19 0.050(2) 0.038(2) 0.054(2) -0.0061(18) 0.0071(18) -0.0040(19) N20 0.040(2) 0.051(2) 0.0412(19) -0.0017(17) 0.0042(17) -0.0079(18) N21 0.041(2) 0.047(3) 0.057(2) 0.0081(19) 0.0163(18) 0.0006(19) N22 0.047(2) 0.059(3) 0.050(2) 0.0036(19) 0.0110(17) 0.0085(19) N23 0.060(3) 0.064(3) 0.065(3) 0.003(2) 0.006(2) 0.007(2) O1 0.065(2) 0.066(3) 0.131(3) 0.010(3) -0.029(2) 0.017(2) O2 0.0412(19) 0.088(3) 0.099(3) 0.005(2) -0.0129(18) -0.016(2) O3 0.0468(19) 0.071(3) 0.097(3) 0.002(2) 0.0165(18) -0.0253(18) O4 0.080(2) 0.089(3) 0.081(3) -0.009(2) 0.050(2) -0.021(2) O5 0.068(2) 0.112(3) 0.065(2) -0.018(2) 0.0280(19) 0.025(2) O6 0.085(3) 0.074(3) 0.085(3) -0.004(2) 0.014(2) 0.044(2) O7 0.067(2) 0.101(3) 0.075(2) 0.017(2) 0.0423(19) 0.019(2) O8 0.117(3) 0.089(3) 0.106(3) -0.024(3) 0.067(3) 0.021(3) O9 0.153(4) 0.057(3) 0.120(4) 0.005(3) 0.028(3) 0.049(3) O10 0.115(4) 0.110(4) 0.132(4) 0.008(3) -0.022(3) 0.071(3) O11 0.043(2) 0.112(4) 0.140(4) 0.023(3) -0.025(2) -0.017(2) O12 0.068(2) 0.118(4) 0.103(3) 0.002(3) 0.015(2) -0.057(3) O13 0.060(2) 0.056(2) 0.082(2) -0.0194(18) 0.0051(18) -0.0139(18) O14 0.076(2) 0.049(2) 0.099(3) -0.031(2) 0.020(2) -0.0021(19) O15 0.063(2) 0.093(3) 0.0423(18) -0.0069(17) 0.0093(16) 0.0022(19) O16 0.055(2) 0.094(3) 0.055(2) 0.0032(18) -0.0083(16) 0.0139(19) O17 0.072(2) 0.047(2) 0.095(3) 0.0233(19) 0.0283(19) 0.0117(19) O18 0.079(2) 0.066(3) 0.112(3) 0.030(2) 0.050(2) 0.004(2) O19 0.0384(14) 0.0280(15) 0.0338(13) -0.0042(11) 0.0079(11) -0.0026(12) _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 C39 C40 1.423(8) . ? C39 N23 1.491(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.514(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.359(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C47 C48 1.428(8) . ? C47 N23 1.533(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.497(9) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.294(11) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9300 . ? C50 H50B 0.9300 . ? C31 C32 1.504(6) . ? C31 N22 1.522(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.503(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.484(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C23 C24 1.516(7) . ? C23 N22 1.520(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.558(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.382(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? Co1 O19 1.784(2) . ? Co1 N21 1.928(4) . ? Co1 N8 1.932(3) . ? Co1 N17 1.933(3) . ? Co1 N1 1.935(3) . ? Co1 N10 1.938(3) . ? Co2 O19 1.788(2) . ? Co2 N19 1.918(4) . ? Co2 N2 1.926(3) . ? Co2 N13 1.932(3) . ? Co2 N4 1.947(3) . ? Co2 N11 1.948(3) . ? Co3 O19 1.793(2) . ? Co3 N20 1.922(3) . ? Co3 N5 1.925(3) . ? Co3 N16 1.931(3) . ? Co3 N7 1.941(3) . ? Co3 N14 1.942(3) . ? C1 N2 1.327(4) . ? C1 C2 1.389(6) . ? C1 H1 0.9300 . ? C2 C3 1.380(5) . ? C2 N3 1.422(5) . ? C3 N1 1.319(4) . ? C3 H3 0.9300 . ? C4 N5 1.322(5) . ? C4 C5 1.367(5) . ? C4 H4 0.9300 . ? C5 C6 1.371(6) . ? C5 N6 1.423(5) . ? C6 N4 1.318(5) . ? C6 H6 0.9300 . ? C7 N8 1.325(5) . ? C7 C8 1.376(6) . ? C7 H7 0.9300 . ? C8 C9 1.391(6) . ? C8 N9 1.426(5) . ? C9 N7 1.334(5) . ? C9 H9 0.9300 . ? C10 N11 1.325(5) . ? C10 C11 1.382(6) . ? C10 H10 0.9300 . ? C11 C12 1.382(6) . ? C11 N12 1.417(5) . ? C12 N10 1.324(5) . ? C12 H12 0.9300 . ? C13 N14 1.319(5) . ? C13 C14 1.372(6) . ? C13 H13 0.9300 . ? C14 C15 1.376(6) . ? C14 N15 1.418(6) . ? C15 N13 1.316(5) . ? C15 H15 0.9300 . ? C16 N17 1.321(5) . ? C16 C17 1.375(6) . ? C16 H16 0.9300 . ? C17 C18 1.374(6) . ? C17 N18 1.433(5) . ? C18 N16 1.318(5) . ? C18 H18 0.9300 . ? C19 C20 1.512(6) . ? C19 N22 1.530(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.496(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.508(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C27 C28 1.511(6) . ? C27 N22 1.511(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.500(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.517(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C35 C36 1.431(9) . ? C35 N23 1.518(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.574(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.391(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C43 C44 1.457(8) . ? C43 N23 1.503(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.549(8) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.490(9) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? N1 N2 1.390(4) . ? N3 O2 1.213(5) . ? N3 O1 1.229(5) . ? N4 N5 1.378(4) . ? N6 O3 1.216(5) . ? N6 O4 1.231(5) . ? N7 N8 1.380(4) . ? N9 O5 1.214(5) . ? N9 O6 1.227(5) . ? N10 N11 1.386(4) . ? N12 O8 1.219(5) . ? N12 O7 1.226(5) . ? N13 N14 1.380(4) . ? N15 O10 1.214(6) . ? N15 O9 1.216(6) . ? N16 N17 1.384(4) . ? N18 O11 1.210(5) . ? N18 O12 1.214(5) . ? N19 O13 1.221(4) . ? N19 O14 1.241(4) . ? N20 O16 1.225(4) . ? N20 O15 1.230(4) . ? N21 O18 1.221(4) . ? N21 O17 1.224(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 C39 N23 121.6(6) . . ? C40 C39 H39A 106.9 . . ? N23 C39 H39A 106.9 . . ? C40 C39 H39B 106.9 . . ? N23 C39 H39B 106.9 . . ? H39A C39 H39B 106.7 . . ? C39 C40 C41 110.8(7) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 114.6(9) . . ? C42 C41 H41A 108.6 . . ? C40 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? C40 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C47 N23 121.7(6) . . ? C48 C47 H47A 106.9 . . ? N23 C47 H47A 106.9 . . ? C48 C47 H47B 106.9 . . ? N23 C47 H47B 106.9 . . ? H47A C47 H47B 106.7 . . ? C47 C48 C49 113.8(7) . . ? C47 C48 H48A 108.8 . . ? C49 C48 H48A 108.8 . . ? C47 C48 H48B 108.8 . . ? C49 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 123.5(10) . . ? C50 C49 H49A 106.5 . . ? C48 C49 H49A 106.5 . . ? C50 C49 H49B 106.5 . . ? C48 C49 H49B 106.5 . . ? H49A C49 H49B 106.5 . . ? C49 C50 H50A 120.0 . . ? C49 C50 H50B 120.0 . . ? H50A C50 H50B 120.0 . . ? C32 C31 N22 116.9(4) . . ? C32 C31 H31A 108.1 . . ? N22 C31 H31A 108.1 . . ? C32 C31 H31B 108.1 . . ? N22 C31 H31B 108.1 . . ? H31A C31 H31B 107.3 . . ? C33 C32 C31 113.0(5) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 114.5(6) . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C24 C23 N22 115.9(4) . . ? C24 C23 H23A 108.3 . . ? N22 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? N22 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 C25 110.0(5) . . ? C23 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? C23 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 110.8(10) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O19 Co1 N21 179.92(17) . . ? O19 Co1 N8 84.21(12) . . ? N21 Co1 N8 95.80(15) . . ? O19 Co1 N17 85.31(12) . . ? N21 Co1 N17 94.62(14) . . ? N8 Co1 N17 86.71(13) . . ? O19 Co1 N1 84.67(12) . . ? N21 Co1 N1 95.41(14) . . ? N8 Co1 N1 91.20(13) . . ? N17 Co1 N1 169.92(14) . . ? O19 Co1 N10 83.56(12) . . ? N21 Co1 N10 96.43(15) . . ? N8 Co1 N10 167.77(14) . . ? N17 Co1 N10 92.42(13) . . ? N1 Co1 N10 87.54(13) . . ? O19 Co2 N19 178.99(15) . . ? O19 Co2 N2 84.66(12) . . ? N19 Co2 N2 95.30(15) . . ? O19 Co2 N13 85.12(13) . . ? N19 Co2 N13 94.94(15) . . ? N2 Co2 N13 169.74(14) . . ? O19 Co2 N4 85.33(12) . . ? N19 Co2 N4 95.67(15) . . ? N2 Co2 N4 92.66(13) . . ? N13 Co2 N4 85.74(13) . . ? O19 Co2 N11 82.96(12) . . ? N19 Co2 N11 96.03(15) . . ? N2 Co2 N11 87.57(13) . . ? N13 Co2 N11 91.94(13) . . ? N4 Co2 N11 168.22(13) . . ? O19 Co3 N20 179.74(15) . . ? O19 Co3 N5 85.63(12) . . ? N20 Co3 N5 94.50(14) . . ? O19 Co3 N16 84.59(12) . . ? N20 Co3 N16 95.28(14) . . ? N5 Co3 N16 170.22(13) . . ? O19 Co3 N7 83.50(12) . . ? N20 Co3 N7 96.27(15) . . ? N5 Co3 N7 91.73(13) . . ? N16 Co3 N7 87.22(13) . . ? O19 Co3 N14 84.29(12) . . ? N20 Co3 N14 95.95(15) . . ? N5 Co3 N14 86.31(13) . . ? N16 Co3 N14 92.66(13) . . ? N7 Co3 N14 167.74(13) . . ? N2 C1 C2 107.4(4) . . ? N2 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? C3 C2 C1 107.2(3) . . ? C3 C2 N3 126.6(4) . . ? C1 C2 N3 126.1(4) . . ? N1 C3 C2 108.3(4) . . ? N1 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? N5 C4 C5 108.6(4) . . ? N5 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? C4 C5 C6 106.7(4) . . ? C4 C5 N6 125.4(4) . . ? C6 C5 N6 127.9(4) . . ? N4 C6 C5 108.6(4) . . ? N4 C6 H6 125.7 . . ? C5 C6 H6 125.7 . . ? N8 C7 C8 108.7(4) . . ? N8 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? C7 C8 C9 106.7(4) . . ? C7 C8 N9 126.6(4) . . ? C9 C8 N9 126.6(4) . . ? N7 C9 C8 107.7(4) . . ? N7 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? N11 C10 C11 107.9(4) . . ? N11 C10 H10 126.0 . . ? C11 C10 H10 126.0 . . ? C10 C11 C12 107.3(4) . . ? C10 C11 N12 126.1(5) . . ? C12 C11 N12 126.6(4) . . ? N10 C12 C11 107.8(4) . . ? N10 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? N14 C13 C14 108.7(4) . . ? N14 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? C13 C14 C15 106.5(4) . . ? C13 C14 N15 127.8(5) . . ? C15 C14 N15 125.8(5) . . ? N13 C15 C14 108.5(4) . . ? N13 C15 H15 125.7 . . ? C14 C15 H15 125.7 . . ? N17 C16 C17 108.2(4) . . ? N17 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? C18 C17 C16 107.1(3) . . ? C18 C17 N18 126.0(4) . . ? C16 C17 N18 126.9(4) . . ? N16 C18 C17 108.2(4) . . ? N16 C18 H18 125.9 . . ? C17 C18 H18 125.9 . . ? C20 C19 N22 116.3(4) . . ? C20 C19 H19A 108.2 . . ? N22 C19 H19A 108.2 . . ? C20 C19 H19B 108.2 . . ? N22 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? C21 C20 C19 110.4(4) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 112.7(4) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C27 N22 116.4(4) . . ? C28 C27 H27A 108.2 . . ? N22 C27 H27A 108.2 . . ? C28 C27 H27B 108.2 . . ? N22 C27 H27B 108.2 . . ? H27A C27 H27B 107.3 . . ? C29 C28 C27 111.0(4) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 112.8(5) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C35 N23 116.2(6) . . ? C36 C35 H35A 108.2 . . ? N23 C35 H35A 108.2 . . ? C36 C35 H35B 108.2 . . ? N23 C35 H35B 108.2 . . ? H35A C35 H35B 107.4 . . ? C35 C36 C37 110.7(6) . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 110.3(7) . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C43 N23 117.6(5) . . ? C44 C43 H43A 107.9 . . ? N23 C43 H43A 107.9 . . ? C44 C43 H43B 107.9 . . ? N23 C43 H43B 107.9 . . ? H43A C43 H43B 107.2 . . ? C43 C44 C45 110.4(6) . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C44 110.0(6) . . ? C46 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? C46 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C3 N1 N2 108.3(3) . . ? C3 N1 Co1 134.8(3) . . ? N2 N1 Co1 116.4(2) . . ? C1 N2 N1 108.7(3) . . ? C1 N2 Co2 134.7(3) . . ? N1 N2 Co2 116.4(2) . . ? O2 N3 O1 123.6(4) . . ? O2 N3 C2 118.5(4) . . ? O1 N3 C2 117.9(4) . . ? C6 N4 N5 108.2(3) . . ? C6 N4 Co2 136.8(3) . . ? N5 N4 Co2 115.1(2) . . ? C4 N5 N4 108.0(3) . . ? C4 N5 Co3 134.7(3) . . ? N4 N5 Co3 117.3(2) . . ? O3 N6 O4 122.9(4) . . ? O3 N6 C5 118.8(4) . . ? O4 N6 C5 118.3(4) . . ? C9 N7 N8 108.5(3) . . ? C9 N7 Co3 134.1(3) . . ? N8 N7 Co3 116.7(2) . . ? C7 N8 N7 108.4(3) . . ? C7 N8 Co1 135.0(3) . . ? N7 N8 Co1 116.0(2) . . ? O5 N9 O6 124.2(4) . . ? O5 N9 C8 118.4(5) . . ? O6 N9 C8 117.4(4) . . ? C12 N10 N11 108.7(3) . . ? C12 N10 Co1 135.3(3) . . ? N11 N10 Co1 115.8(2) . . ? C10 N11 N10 108.3(3) . . ? C10 N11 Co2 134.5(3) . . ? N10 N11 Co2 116.8(2) . . ? O8 N12 O7 122.7(4) . . ? O8 N12 C11 118.4(5) . . ? O7 N12 C11 118.9(5) . . ? C15 N13 N14 108.3(3) . . ? C15 N13 Co2 135.0(3) . . ? N14 N13 Co2 116.6(2) . . ? C13 N14 N13 108.0(3) . . ? C13 N14 Co3 136.4(3) . . ? N13 N14 Co3 115.6(2) . . ? O10 N15 O9 123.4(5) . . ? O10 N15 C14 117.6(6) . . ? O9 N15 C14 119.0(5) . . ? C18 N16 N17 108.4(3) . . ? C18 N16 Co3 134.9(3) . . ? N17 N16 Co3 116.7(2) . . ? C16 N17 N16 108.1(3) . . ? C16 N17 Co1 135.9(3) . . ? N16 N17 Co1 115.9(2) . . ? O11 N18 O12 123.7(4) . . ? O11 N18 C17 118.4(5) . . ? O12 N18 C17 118.0(5) . . ? O13 N19 O14 119.1(4) . . ? O13 N19 Co2 121.5(3) . . ? O14 N19 Co2 119.4(3) . . ? O16 N20 O15 118.3(3) . . ? O16 N20 Co3 119.8(3) . . ? O15 N20 Co3 121.9(3) . . ? O18 N21 O17 117.8(4) . . ? O18 N21 Co1 120.9(3) . . ? O17 N21 Co1 121.2(3) . . ? C27 N22 C23 110.6(4) . . ? C27 N22 C31 111.2(3) . . ? C23 N22 C31 107.3(3) . . ? C27 N22 C19 106.6(3) . . ? C23 N22 C19 110.7(3) . . ? C31 N22 C19 110.5(4) . . ? C39 N23 C43 111.8(5) . . ? C39 N23 C35 110.0(4) . . ? C43 N23 C35 110.7(4) . . ? C39 N23 C47 106.3(4) . . ? C43 N23 C47 110.2(4) . . ? C35 N23 C47 107.7(5) . . ? Co1 O19 Co2 120.85(13) . . ? Co1 O19 Co3 120.02(13) . . ? Co2 O19 Co3 119.12(14) . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 0.754 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.073