# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_qll _database_code_depnum_ccdc_archive 'CCDC 895802' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H32 Co N4 O7' _chemical_formula_sum 'C46 H34 Co N4 O7' _chemical_formula_weight 813.70 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 Hexagonal _symmetry_space_group_name_H-M 'P6(5) ' _symmetry_space_group_name_hall P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 13.5091(7) _cell_length_b 13.5091(7) _cell_length_c 36.8157(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5818.6(5) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10631 _cell_measurement_theta_min 2.404 _cell_measurement_theta_max 26.184 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2526 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8723 _exptl_absorpt_correction_T_max 0.8976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33619 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7694 _reflns_number_gt 6593 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^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 constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(7) _refine_ls_number_reflns 7694 _refine_ls_number_parameters 523 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.98885(19) 0.69614(19) 0.10715(6) 0.0364(5) Uani 1 1 d . . . H1 H 1.0365 0.7751 0.1068 0.044 Uiso 1 1 calc R . . C2 C 0.97066(18) 0.64061(18) 0.13971(6) 0.0330(5) Uani 1 1 d . . . H2 H 1.0051 0.6815 0.1608 0.040 Uiso 1 1 calc R . . C3 C 0.90077(17) 0.52344(17) 0.14102(5) 0.0274(5) Uani 1 1 d . . . C4 C 0.85423(18) 0.46733(18) 0.10848(6) 0.0321(5) Uani 1 1 d . . . H4 H 0.8086 0.3882 0.1080 0.039 Uiso 1 1 calc R . . C5 C 0.87602(18) 0.52938(17) 0.07704(6) 0.0318(5) Uani 1 1 d . . . H5 H 0.8435 0.4905 0.0555 0.038 Uiso 1 1 calc R . . C6 C 0.87850(17) 0.46131(17) 0.17615(6) 0.0297(5) Uani 1 1 d . . . C7 C 0.86904(18) 0.51111(18) 0.20826(6) 0.0330(5) Uani 1 1 d . . . H7 H 0.8778 0.5839 0.2081 0.040 Uiso 1 1 calc R . . C8 C 0.84653(18) 0.45075(18) 0.24010(6) 0.0326(5) Uani 1 1 d . . . C9 C 0.83610(17) 0.34459(18) 0.24188(5) 0.0317(5) Uani 1 1 d . . . H9 H 0.8248 0.3079 0.2641 0.038 Uiso 1 1 calc R . . C10 C 0.84253(17) 0.29204(17) 0.21021(5) 0.0288(5) Uani 1 1 d . . . C11 C 0.86280(17) 0.35091(16) 0.17739(5) 0.0283(5) Uani 1 1 d . . . H11 H 0.8659 0.3161 0.1560 0.034 Uiso 1 1 calc R . . C12 C 0.81971(17) 0.17283(17) 0.21008(5) 0.0281(5) Uani 1 1 d . . . C13 C 0.85767(18) 0.12741(19) 0.23693(6) 0.0345(5) Uani 1 1 d . . . H13 H 0.9009 0.1726 0.2563 0.041 Uiso 1 1 calc R . . C14 C 0.83082(19) 0.01518(18) 0.23461(6) 0.0343(5) Uani 1 1 d . . . H14 H 0.8569 -0.0139 0.2528 0.041 Uiso 1 1 calc R . . C15 C 0.73205(18) -0.01077(18) 0.18198(6) 0.0332(5) Uani 1 1 d . . . H15 H 0.6887 -0.0578 0.1630 0.040 Uiso 1 1 calc R . . C16 C 0.75492(18) 0.10103(18) 0.18234(5) 0.0314(5) Uani 1 1 d . . . H16 H 0.7268 0.1276 0.1640 0.038 Uiso 1 1 calc R . . C17 C 0.71384(19) 0.44923(17) 0.28066(6) 0.0358(5) Uani 1 1 d . . . C18 C 0.6873(2) 0.43596(18) 0.31731(6) 0.0370(5) Uani 1 1 d . . . H18 H 0.7450 0.4595 0.3346 0.044 Uiso 1 1 calc R . . C19 C 0.5735(2) 0.38714(18) 0.32821(6) 0.0382(6) Uani 1 1 d . . . C20 C 0.4892(2) 0.35247(19) 0.30197(6) 0.0399(6) Uani 1 1 d . . . H20 H 0.4131 0.3186 0.3092 0.048 Uiso 1 1 calc R . . C21 C 0.5155(2) 0.36706(18) 0.26502(6) 0.0359(5) Uani 1 1 d . . . C22 C 0.6289(2) 0.41648(18) 0.25473(6) 0.0381(5) Uani 1 1 d . . . H22 H 0.6482 0.4278 0.2302 0.046 Uiso 1 1 calc R . . C23 C 0.4235(2) 0.32873(19) 0.23725(6) 0.0401(6) Uani 1 1 d . . . C24 C 0.3135(2) 0.2406(2) 0.24386(7) 0.0481(6) Uani 1 1 d . . . H24 H 0.2946 0.2048 0.2664 0.058 Uiso 1 1 calc R . . C25 C 0.2315(3) 0.2057(2) 0.21674(9) 0.0562(8) Uani 1 1 d . . . H25 H 0.1581 0.1470 0.2222 0.067 Uiso 1 1 calc R . . C26 C 0.3565(2) 0.3348(2) 0.17715(8) 0.0562(7) Uani 1 1 d . . . H26 H 0.3729 0.3681 0.1542 0.067 Uiso 1 1 calc R . . C27 C 0.4445(2) 0.3767(2) 0.20258(7) 0.0481(6) Uani 1 1 d . . . H27 H 0.5169 0.4361 0.1965 0.058 Uiso 1 1 calc R . . C28 C 0.5445(2) 0.37217(19) 0.36743(6) 0.0401(5) Uani 1 1 d . . . C29 C 0.6178(3) 0.4468(2) 0.39306(6) 0.0520(7) Uani 1 1 d . . . H29 H 0.6874 0.5088 0.3860 0.062 Uiso 1 1 calc R . . C30 C 0.5878(3) 0.4295(2) 0.42960(7) 0.0592(8) Uani 1 1 d . . . H30 H 0.6382 0.4816 0.4465 0.071 Uiso 1 1 calc R . . C31 C 0.4203(2) 0.2712(2) 0.41669(7) 0.0542(7) Uani 1 1 d . . . H31 H 0.3513 0.2099 0.4245 0.065 Uiso 1 1 calc R . . C32 C 0.4425(2) 0.2819(2) 0.37984(6) 0.0468(6) Uani 1 1 d . . . H32 H 0.3896 0.2293 0.3636 0.056 Uiso 1 1 calc R . . C33 C 0.9658(2) 0.62285(19) -0.01809(6) 0.0357(5) Uani 1 1 d . . . C34 C 0.97302(19) 0.56347(18) -0.05123(6) 0.0336(5) Uani 1 1 d . . . C35 C 1.0719(2) 0.6156(2) -0.07216(7) 0.0427(6) Uani 1 1 d . . . H35 H 1.1342 0.6840 -0.0645 0.051 Uiso 1 1 calc R . . C36 C 1.46147(19) 1.58016(18) 0.10390(6) 0.0372(5) Uani 1 1 d . . . H36 H 1.4265 1.6120 0.1176 0.045 Uiso 1 1 calc R . . C37 C 1.4115(2) 1.52307(19) 0.07227(6) 0.0414(6) Uani 1 1 d . . . H37 H 1.3421 1.5149 0.0647 0.050 Uiso 1 1 calc R . . C38 C 1.4644(2) 1.47828(18) 0.05193(6) 0.0402(6) Uani 1 1 d . . . C39 C 1.5663(2) 1.4884(2) 0.06242(7) 0.0467(6) Uani 1 1 d . . . H39 H 1.6017 1.4584 0.0481 0.056 Uiso 1 1 calc R . . C40 C 1.33352(18) 1.30918(17) 0.02197(6) 0.0347(5) Uani 1 1 d . . . C41 C 1.31332(19) 1.24668(18) 0.05365(6) 0.0392(6) Uani 1 1 d . . . H41 H 1.3530 1.2817 0.0748 0.047 Uiso 1 1 calc R . . C42 C 1.23309(18) 1.13130(18) 0.05328(6) 0.0354(5) Uani 1 1 d . . . H42 H 1.2198 1.0886 0.0744 0.042 Uiso 1 1 calc R . . C43 C 1.17237(17) 1.07834(17) 0.02223(6) 0.0282(5) Uani 1 1 d . . . C44 C 1.19287(17) 1.14328(17) -0.00911(6) 0.0313(5) Uani 1 1 d . . . H44 H 1.1514 1.1090 -0.0301 0.038 Uiso 1 1 calc R . . C45 C 1.27391(18) 1.25796(18) -0.00946(6) 0.0349(5) Uani 1 1 d . . . H45 H 1.2883 1.3004 -0.0307 0.042 Uiso 1 1 calc R . . C46 C 1.08962(17) 0.95432(17) 0.02234(6) 0.0297(5) Uani 1 1 d . . . Co1 Co 0.96116(2) 0.74437(2) 0.031111(7) 0.02847(7) Uani 1 1 d U . . N1 N 0.94188(14) 0.64316(14) 0.07587(4) 0.0292(4) Uani 1 1 d . . . N2 N 0.4902(2) 0.3418(2) 0.44159(6) 0.0570(6) Uani 1 1 d . . . N3 N 0.25015(19) 0.25011(19) 0.18344(7) 0.0571(6) Uani 1 1 d . . . N4 N 0.76878(14) -0.05458(14) 0.20740(4) 0.0301(4) Uani 1 1 d . . . O1 O 0.82811(13) 0.49712(12) 0.27169(4) 0.0399(4) Uani 1 1 d . . . O2 O 1.41482(14) 1.42330(13) 0.01924(4) 0.0488(4) Uani 1 1 d . . . O3 O 0.86938(13) 0.60112(13) -0.00625(4) 0.0411(4) Uani 1 1 d U . . O4 O 1.05573(14) 0.69693(13) -0.00288(4) 0.0477(4) Uani 1 1 d . . . O5 O 1.02540(12) 0.90720(12) -0.00428(4) 0.0353(3) Uani 1 1 d . . . O6 O 1.08650(12) 0.89684(11) 0.05032(4) 0.0359(4) Uani 1 1 d . . . O1W O 0.03118(19) 0.1359(2) 0.14240(6) 0.1011(9) Uani 1 1 d . . . H1WD H 0.0782 0.1523 0.1598 0.121 Uiso 1 1 d R . . H1WA H -0.0259 0.0694 0.1457 0.152 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 C1 0.0411(13) 0.0252(12) 0.0404(13) -0.0012(10) -0.0019(10) 0.0147(10) C2 0.0403(13) 0.0266(12) 0.0311(12) -0.0010(9) -0.0014(10) 0.0160(10) C3 0.0286(11) 0.0265(11) 0.0317(12) 0.0020(9) 0.0039(9) 0.0171(9) C4 0.0318(12) 0.0220(11) 0.0387(13) 0.0012(9) 0.0021(10) 0.0106(10) C5 0.0335(12) 0.0267(11) 0.0339(12) -0.0029(9) -0.0031(10) 0.0141(10) C6 0.0290(11) 0.0268(11) 0.0317(11) 0.0014(9) 0.0036(9) 0.0128(9) C7 0.0352(12) 0.0249(11) 0.0367(12) 0.0013(9) 0.0066(10) 0.0135(10) C8 0.0296(11) 0.0309(12) 0.0296(11) -0.0042(9) 0.0034(9) 0.0095(10) C9 0.0318(12) 0.0320(12) 0.0245(11) 0.0024(9) 0.0031(9) 0.0109(10) C10 0.0289(11) 0.0267(11) 0.0283(11) 0.0006(8) 0.0019(9) 0.0120(9) C11 0.0313(11) 0.0271(11) 0.0245(11) 0.0000(9) 0.0054(9) 0.0130(9) C12 0.0300(11) 0.0293(11) 0.0246(10) 0.0043(8) 0.0060(8) 0.0145(9) C13 0.0370(13) 0.0346(13) 0.0276(11) 0.0004(9) -0.0049(9) 0.0147(10) C14 0.0365(13) 0.0374(13) 0.0307(12) 0.0068(10) -0.0016(10) 0.0198(11) C15 0.0397(13) 0.0345(12) 0.0263(11) -0.0011(9) -0.0035(9) 0.0192(11) C16 0.0392(12) 0.0338(12) 0.0255(11) 0.0052(9) 0.0005(9) 0.0216(10) C17 0.0434(14) 0.0256(11) 0.0348(13) -0.0020(9) 0.0076(11) 0.0147(11) C18 0.0523(15) 0.0308(12) 0.0294(12) 0.0013(9) 0.0075(10) 0.0218(12) C19 0.0566(16) 0.0301(12) 0.0323(12) 0.0023(10) 0.0110(11) 0.0251(12) C20 0.0472(14) 0.0286(12) 0.0448(14) 0.0032(10) 0.0148(11) 0.0196(11) C21 0.0471(14) 0.0289(12) 0.0314(12) 0.0002(9) 0.0066(10) 0.0187(11) C22 0.0510(15) 0.0312(12) 0.0283(12) -0.0003(9) 0.0096(11) 0.0177(11) C23 0.0473(15) 0.0314(13) 0.0425(14) -0.0020(10) 0.0072(11) 0.0204(12) C24 0.0522(16) 0.0374(14) 0.0499(16) 0.0029(12) 0.0087(13) 0.0187(13) C25 0.0510(17) 0.0344(15) 0.074(2) 0.0007(14) 0.0033(15) 0.0141(13) C26 0.0641(19) 0.0466(16) 0.0468(16) 0.0032(13) 0.0029(14) 0.0193(15) C27 0.0510(15) 0.0387(14) 0.0434(15) 0.0029(12) 0.0041(12) 0.0140(12) C28 0.0585(15) 0.0359(13) 0.0345(13) 0.0075(11) 0.0108(12) 0.0302(12) C29 0.0748(19) 0.0408(15) 0.0367(14) 0.0064(12) 0.0176(13) 0.0261(14) C30 0.085(2) 0.0565(18) 0.0380(15) 0.0058(13) 0.0130(14) 0.0366(17) C31 0.0618(18) 0.0589(18) 0.0463(16) 0.0206(14) 0.0196(14) 0.0334(15) C32 0.0578(17) 0.0495(15) 0.0391(14) 0.0094(11) 0.0140(12) 0.0312(14) C33 0.0370(13) 0.0310(12) 0.0447(14) 0.0065(10) 0.0048(11) 0.0213(11) C34 0.0378(13) 0.0287(12) 0.0407(13) 0.0056(9) 0.0049(10) 0.0214(11) C35 0.0402(14) 0.0305(13) 0.0578(16) -0.0002(11) 0.0082(11) 0.0181(11) C36 0.0363(13) 0.0311(12) 0.0441(14) 0.0013(10) 0.0057(10) 0.0169(10) C37 0.0318(13) 0.0331(13) 0.0530(16) 0.0016(11) -0.0026(11) 0.0114(11) C38 0.0386(14) 0.0219(11) 0.0430(14) -0.0006(10) 0.0029(11) 0.0022(10) C39 0.0403(14) 0.0332(13) 0.0606(17) -0.0112(12) 0.0048(12) 0.0139(12) C40 0.0310(12) 0.0228(11) 0.0409(13) -0.0015(9) 0.0032(10) 0.0063(9) C41 0.0383(13) 0.0309(12) 0.0374(13) -0.0048(10) -0.0066(10) 0.0091(11) C42 0.0337(12) 0.0281(12) 0.0397(13) 0.0029(10) 0.0001(10) 0.0119(10) C43 0.0250(11) 0.0258(10) 0.0346(12) -0.0011(9) 0.0021(9) 0.0134(9) C44 0.0317(12) 0.0311(12) 0.0283(11) -0.0032(9) 0.0023(9) 0.0137(10) C45 0.0387(13) 0.0317(12) 0.0295(12) 0.0041(9) 0.0069(10) 0.0140(10) C46 0.0255(11) 0.0297(11) 0.0347(13) 0.0018(9) 0.0046(9) 0.0144(9) Co1 0.02711(15) 0.02406(15) 0.03306(15) 0.00216(12) -0.00130(12) 0.01192(13) N1 0.0296(9) 0.0240(9) 0.0332(10) 0.0024(8) -0.0011(8) 0.0127(8) N2 0.0766(17) 0.0655(16) 0.0383(12) 0.0155(12) 0.0197(12) 0.0427(14) N3 0.0562(15) 0.0415(13) 0.0648(16) -0.0028(12) -0.0044(12) 0.0177(12) N4 0.0304(10) 0.0331(10) 0.0283(10) 0.0056(8) 0.0055(7) 0.0170(8) O1 0.0428(10) 0.0355(9) 0.0325(9) -0.0070(7) 0.0087(7) 0.0128(8) O2 0.0529(11) 0.0276(8) 0.0400(9) -0.0002(7) 0.0004(8) 0.0006(8) O3 0.0387(9) 0.0503(10) 0.0401(9) -0.0086(7) -0.0031(7) 0.0265(8) O4 0.0399(10) 0.0361(9) 0.0606(12) -0.0075(8) 0.0074(8) 0.0140(8) O5 0.0326(8) 0.0292(8) 0.0371(9) -0.0020(7) -0.0013(7) 0.0101(7) O6 0.0328(8) 0.0254(8) 0.0448(9) 0.0040(7) -0.0058(7) 0.0109(7) O1W 0.0766(16) 0.0953(18) 0.125(2) 0.0601(16) -0.0029(14) 0.0386(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(3) . ? C1 C2 1.370(3) . ? C1 H1 0.9300 . ? C2 C3 1.380(3) . ? C2 H2 0.9300 . ? C3 C4 1.389(3) . ? C3 C6 1.488(3) . ? C4 C5 1.372(3) . ? C4 H4 0.9300 . ? C5 N1 1.337(2) . ? C5 H5 0.9300 . ? C6 C7 1.397(3) . ? C6 C11 1.398(3) . ? C7 C8 1.372(3) . ? C7 H7 0.9300 . ? C8 C9 1.371(3) . ? C8 O1 1.401(2) . ? C9 C10 1.390(3) . ? C9 H9 0.9300 . ? C10 C11 1.396(3) . ? C10 C12 1.480(3) . ? C11 H11 0.9300 . ? C12 C16 1.379(3) . ? C12 C13 1.390(3) . ? C13 C14 1.374(3) . ? C13 H13 0.9300 . ? C14 N4 1.343(3) . ? C14 H14 0.9300 . ? C15 N4 1.329(2) . ? C15 C16 1.382(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O1 1.383(3) . ? C17 C22 1.384(3) . ? C17 C18 1.385(3) . ? C18 C19 1.395(3) . ? C18 H18 0.9300 . ? C19 C20 1.384(3) . ? C19 C28 1.483(3) . ? C20 C21 1.395(3) . ? C20 H20 0.9300 . ? C21 C22 1.383(3) . ? C21 C23 1.488(3) . ? C22 H22 0.9300 . ? C23 C24 1.384(3) . ? C23 C27 1.395(3) . ? C24 C25 1.387(4) . ? C24 H24 0.9300 . ? C25 N3 1.332(3) . ? C25 H25 0.9300 . ? C26 N3 1.336(3) . ? C26 C27 1.392(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.375(3) . ? C28 C32 1.384(3) . ? C29 C30 1.391(3) . ? C29 H29 0.9300 . ? C30 N2 1.331(3) . ? C30 H30 0.9300 . ? C31 N2 1.320(3) . ? C31 C32 1.381(3) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O4 1.255(3) . ? C33 O3 1.261(2) . ? C33 C34 1.490(3) . ? C34 C36 1.381(3) 6_644 ? C34 C35 1.390(3) . ? C35 C39 1.378(3) 6_644 ? C35 H35 0.9300 . ? C36 C37 1.373(3) . ? C36 C34 1.381(3) 5_675 ? C36 H36 0.9300 . ? C37 C38 1.368(3) . ? C37 H37 0.9300 . ? C38 C39 1.369(3) . ? C38 O2 1.397(2) . ? C39 C35 1.378(3) 5_675 ? C39 H39 0.9300 . ? C40 O2 1.378(2) . ? C40 C45 1.382(3) . ? C40 C41 1.385(3) . ? C41 C42 1.384(3) . ? C41 H41 0.9300 . ? C42 C43 1.380(3) . ? C42 H42 0.9300 . ? C43 C44 1.391(3) . ? C43 C46 1.478(3) . ? C44 C45 1.379(3) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 O5 1.252(2) . ? C46 O6 1.278(2) . ? C46 Co1 2.498(2) . ? Co1 O6 2.0303(14) . ? Co1 N1 2.0728(17) . ? Co1 N4 2.0770(17) 6_554 ? Co1 O4 2.1040(15) . ? Co1 O3 2.1851(15) . ? Co1 O5 2.3196(14) . ? N4 Co1 2.0770(17) 5 ? O1W H1WD 0.8498 . ? O1W H1WA 0.8500 . ? 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 N1 C1 C2 123.6(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 117.33(19) . . ? C2 C3 C6 120.45(18) . . ? C4 C3 C6 122.21(19) . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.1(2) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C11 118.96(19) . . ? C7 C6 C3 120.33(18) . . ? C11 C6 C3 120.68(18) . . ? C8 C7 C6 118.88(19) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 122.6(2) . . ? C9 C8 O1 118.67(19) . . ? C7 C8 O1 118.65(19) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 118.65(19) . . ? C9 C10 C12 121.73(18) . . ? C11 C10 C12 119.45(18) . . ? C10 C11 C6 121.18(18) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? C16 C12 C13 117.44(19) . . ? C16 C12 C10 118.76(18) . . ? C13 C12 C10 123.78(19) . . ? C14 C13 C12 119.4(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? N4 C14 C13 123.26(19) . . ? N4 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? N4 C15 C16 123.4(2) . . ? N4 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C12 C16 C15 119.48(19) . . ? C12 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? O1 C17 C22 122.55(19) . . ? O1 C17 C18 116.7(2) . . ? C22 C17 C18 120.7(2) . . ? C17 C18 C19 119.6(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.0(2) . . ? C20 C19 C28 121.1(2) . . ? C18 C19 C28 119.9(2) . . ? C19 C20 C21 121.6(2) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 118.5(2) . . ? C22 C21 C23 120.7(2) . . ? C20 C21 C23 120.7(2) . . ? C17 C22 C21 120.4(2) . . ? C17 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C27 116.3(2) . . ? C24 C23 C21 121.9(2) . . ? C27 C23 C21 121.7(2) . . ? C23 C24 C25 119.8(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N3 C25 C24 124.8(3) . . ? N3 C25 H25 117.6 . . ? C24 C25 H25 117.6 . . ? N3 C26 C27 124.5(3) . . ? N3 C26 H26 117.8 . . ? C27 C26 H26 117.8 . . ? C26 C27 C23 119.5(2) . . ? C26 C27 H27 120.3 . . ? C23 C27 H27 120.3 . . ? C29 C28 C32 117.0(2) . . ? C29 C28 C19 121.6(2) . . ? C32 C28 C19 121.3(2) . . ? C28 C29 C30 119.8(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? N2 C30 C29 123.1(3) . . ? N2 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N2 C31 C32 124.5(3) . . ? N2 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C31 C32 C28 119.0(3) . . ? C31 C32 H32 120.5 . . ? C28 C32 H32 120.5 . . ? O4 C33 O3 120.5(2) . . ? O4 C33 C34 119.8(2) . . ? O3 C33 C34 119.7(2) . . ? C36 C34 C35 119.4(2) 6_644 . ? C36 C34 C33 121.4(2) 6_644 . ? C35 C34 C33 119.1(2) . . ? C39 C35 C34 120.3(2) 6_644 . ? C39 C35 H35 119.9 6_644 . ? C34 C35 H35 119.9 . . ? C37 C36 C34 120.2(2) . 5_675 ? C37 C36 H36 119.9 . . ? C34 C36 H36 119.9 5_675 . ? C38 C37 C36 119.6(2) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 121.5(2) . . ? C37 C38 O2 119.3(2) . . ? C39 C38 O2 119.1(2) . . ? C38 C39 C35 119.0(2) . 5_675 ? C38 C39 H39 120.5 . . ? C35 C39 H39 120.5 5_675 . ? O2 C40 C45 115.98(19) . . ? O2 C40 C41 123.2(2) . . ? C45 C40 C41 120.82(19) . . ? C42 C41 C40 118.9(2) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C41 121.3(2) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 118.74(19) . . ? C42 C43 C46 120.13(19) . . ? C44 C43 C46 121.11(19) . . ? C45 C44 C43 120.8(2) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C40 119.4(2) . . ? C44 C45 H45 120.3 . . ? C40 C45 H45 120.3 . . ? O5 C46 O6 121.22(19) . . ? O5 C46 C43 120.90(19) . . ? O6 C46 C43 117.89(19) . . ? O5 C46 Co1 67.18(11) . . ? O6 C46 Co1 54.03(10) . . ? C43 C46 Co1 171.91(16) . . ? O6 Co1 N1 99.11(6) . . ? O6 Co1 N4 97.97(6) . 6_554 ? N1 Co1 N4 98.17(6) . 6_554 ? O6 Co1 O4 100.99(6) . . ? N1 Co1 O4 99.62(7) . . ? N4 Co1 O4 151.48(7) 6_554 . ? O6 Co1 O3 159.04(6) . . ? N1 Co1 O3 95.04(6) . . ? N4 Co1 O3 95.23(6) 6_554 . ? O4 Co1 O3 61.18(6) . . ? O6 Co1 O5 60.44(5) . . ? N1 Co1 O5 159.41(6) . . ? N4 Co1 O5 83.41(6) 6_554 . ? O4 Co1 O5 87.62(6) . . ? O3 Co1 O5 105.30(6) . . ? O6 Co1 C46 30.62(6) . . ? N1 Co1 C46 129.69(7) . . ? N4 Co1 C46 90.62(6) 6_554 . ? O4 Co1 C46 94.94(6) . . ? O3 Co1 C46 133.53(7) . . ? O5 Co1 C46 29.82(6) . . ? C1 N1 C5 116.90(18) . . ? C1 N1 Co1 117.53(14) . . ? C5 N1 Co1 125.15(14) . . ? C31 N2 C30 116.4(2) . . ? C25 N3 C26 115.2(2) . . ? C15 N4 C14 116.97(18) . . ? C15 N4 Co1 116.88(14) . 5 ? C14 N4 Co1 125.57(14) . 5 ? C17 O1 C8 113.29(16) . . ? C40 O2 C38 115.72(16) . . ? C33 O3 Co1 87.06(13) . . ? C33 O4 Co1 90.85(13) . . ? C46 O5 Co1 82.99(12) . . ? C46 O6 Co1 95.35(12) . . ? H1WD O1W H1WA 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.242 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.036 data_ql1 _database_code_depnum_ccdc_archive 'CCDC 895803' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C112 H82 Co5 N10 O21' _chemical_formula_sum 'C112 H82 Co5 N10 O21' _chemical_formula_weight 2198.53 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 'C2/c ' _symmetry_space_group_name_hall ' -C 2yc' 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 27.4499(17) _cell_length_b 17.0811(10) _cell_length_c 29.4964(18) _cell_angle_alpha 90.00 _cell_angle_beta 108.5660(10) _cell_angle_gamma 90.00 _cell_volume 13110.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9429 _cell_measurement_theta_min 2.208 _cell_measurement_theta_max 26.364 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4508 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8326 _exptl_absorpt_correction_T_max 0.8649 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58499 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.53 _reflns_number_total 14987 _reflns_number_gt 10940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^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 constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14987 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.88268(9) 0.80089(15) 0.88245(8) 0.0361(6) Uani 1 1 d . . . H1 H 0.8686 0.8488 0.8866 0.043 Uiso 1 1 calc R . . C2 C 0.86675(9) 0.76720(15) 0.83769(9) 0.0412(6) Uani 1 1 d . . . H2 H 0.8425 0.7922 0.8124 0.049 Uiso 1 1 calc R . . C3 C 0.88705(9) 0.69605(15) 0.83059(8) 0.0351(5) Uani 1 1 d . . . C4 C 0.92141(9) 0.66024(14) 0.87024(8) 0.0366(6) Uani 1 1 d . . . H4 H 0.9351 0.6114 0.8674 0.044 Uiso 1 1 calc R . . C5 C 0.93504(9) 0.69759(14) 0.91381(8) 0.0338(5) Uani 1 1 d . . . H5 H 0.9577 0.6724 0.9401 0.041 Uiso 1 1 calc R . . C6 C 0.87329(9) 0.65717(15) 0.78348(8) 0.0373(6) Uani 1 1 d . . . C7 C 0.82273(10) 0.65530(16) 0.75376(9) 0.0460(7) Uani 1 1 d . . . H7 H 0.7977 0.6833 0.7620 0.055 Uiso 1 1 calc R . . C8 C 0.80913(9) 0.61183(15) 0.71165(9) 0.0403(6) Uani 1 1 d . . . C9 C 0.84628(9) 0.57115(14) 0.69887(8) 0.0380(6) Uani 1 1 d . . . H9 H 0.8374 0.5410 0.6712 0.046 Uiso 1 1 calc R . . C10 C 0.89696(9) 0.57600(13) 0.72799(8) 0.0319(5) Uani 1 1 d . . . C11 C 0.91069(9) 0.61756(14) 0.76972(8) 0.0350(5) Uani 1 1 d . . . H11 H 0.9449 0.6194 0.7889 0.042 Uiso 1 1 calc R . . C12 C 0.75422(9) 0.60948(15) 0.68136(9) 0.0415(6) Uani 1 1 d . . . C13 C 0.72847(10) 0.67693(16) 0.66286(10) 0.0521(7) Uani 1 1 d . . . H13 H 0.7453 0.7250 0.6689 0.062 Uiso 1 1 calc R . . C14 C 0.67781(10) 0.67308(16) 0.63539(10) 0.0484(7) Uani 1 1 d . . . H14 H 0.6612 0.7195 0.6229 0.058 Uiso 1 1 calc R . . C15 C 0.67594(10) 0.54267(16) 0.64433(10) 0.0486(7) Uani 1 1 d . . . H15 H 0.6579 0.4956 0.6391 0.058 Uiso 1 1 calc R . . C16 C 0.72695(11) 0.54112(16) 0.67103(10) 0.0559(8) Uani 1 1 d . . . H16 H 0.7430 0.4937 0.6821 0.067 Uiso 1 1 calc R . . C17 C 0.93204(9) 0.45961(13) 0.70976(8) 0.0325(5) Uani 1 1 d . . . C18 C 0.92964(10) 0.42802(14) 0.66632(8) 0.0364(5) Uani 1 1 d . . . H18 H 0.9292 0.4605 0.6409 0.044 Uiso 1 1 calc R . . C19 C 0.92791(10) 0.34720(14) 0.66065(8) 0.0365(6) Uani 1 1 d . . . C20 C 0.92897(10) 0.30009(15) 0.69929(8) 0.0389(6) Uani 1 1 d . . . H20 H 0.9272 0.2460 0.6955 0.047 Uiso 1 1 calc R . . C21 C 0.93263(10) 0.33210(14) 0.74348(8) 0.0362(5) Uani 1 1 d . . . C22 C 0.93372(9) 0.41323(14) 0.74830(8) 0.0357(5) Uani 1 1 d . . . H22 H 0.9356 0.4359 0.7775 0.043 Uiso 1 1 calc R . . C23 C 0.92704(10) 0.31230(14) 0.61434(8) 0.0385(6) Uani 1 1 d . . . C24 C 0.95377(12) 0.34673(16) 0.58681(10) 0.0513(7) Uani 1 1 d . . . H24 H 0.9696 0.3951 0.5955 0.062 Uiso 1 1 calc R . . C25 C 0.95679(12) 0.30919(15) 0.54664(9) 0.0473(7) Uani 1 1 d . . . H25 H 0.9757 0.3328 0.5292 0.057 Uiso 1 1 calc R . . C26 C 0.90601(11) 0.21039(16) 0.55653(9) 0.0428(6) Uani 1 1 d . . . H26 H 0.8883 0.1641 0.5457 0.051 Uiso 1 1 calc R . . C27 C 0.90174(11) 0.24321(16) 0.59724(9) 0.0469(7) Uani 1 1 d . . . H27 H 0.8818 0.2191 0.6135 0.056 Uiso 1 1 calc R . . C28 C 0.93611(10) 0.28081(14) 0.78553(8) 0.0366(5) Uani 1 1 d . . . C29 C 0.94918(14) 0.20290(18) 0.78742(10) 0.0620(9) Uani 1 1 d . . . H29 H 0.9570 0.1805 0.7618 0.074 Uiso 1 1 calc R . . C30 C 0.95088(14) 0.15747(17) 0.82625(10) 0.0595(9) Uani 1 1 d . . . H30 H 0.9591 0.1048 0.8255 0.071 Uiso 1 1 calc R . . C31 C 0.93177(13) 0.26077(16) 0.86399(9) 0.0559(8) Uani 1 1 d . . . H31 H 0.9268 0.2827 0.8911 0.067 Uiso 1 1 calc R . . C32 C 0.92853(14) 0.30952(17) 0.82609(9) 0.0566(8) Uani 1 1 d . . . H32 H 0.9211 0.3623 0.8280 0.068 Uiso 1 1 calc R . . C33 C 0.88507(8) 0.97300(13) 0.97280(7) 0.0247(4) Uani 1 1 d . . . C34 C 0.83037(8) 0.99684(13) 0.96523(8) 0.0299(5) Uani 1 1 d . . . C35 C 0.81631(9) 1.07446(15) 0.96622(9) 0.0384(6) Uani 1 1 d . . . H35 H 0.8414 1.1132 0.9742 0.046 Uiso 1 1 calc R . . C36 C 0.76510(10) 1.09471(16) 0.95544(10) 0.0480(7) Uani 1 1 d . . . H36 H 0.7557 1.1469 0.9558 0.058 Uiso 1 1 calc R . . C37 C 0.72859(9) 1.03754(17) 0.94424(10) 0.0473(7) Uani 1 1 d . . . C38 C 0.74142(10) 0.96030(17) 0.94332(11) 0.0519(7) Uani 1 1 d . . . H38 H 0.7160 0.9220 0.9356 0.062 Uiso 1 1 calc R . . C39 C 0.79235(9) 0.93994(15) 0.95401(10) 0.0447(6) Uani 1 1 d . . . H39 H 0.8014 0.8875 0.9537 0.054 Uiso 1 1 calc R . . C40 C 0.65424(9) 1.10795(16) 0.94990(10) 0.0440(7) Uani 1 1 d . . . C41 C 0.67603(10) 1.13934(19) 0.99495(10) 0.0547(8) Uani 1 1 d . . . H41 H 0.7094 1.1259 1.0129 0.066 Uiso 1 1 calc R . . C42 C 0.64846(9) 1.19038(16) 1.01339(9) 0.0436(6) Uani 1 1 d . . . H42 H 0.6637 1.2120 1.0435 0.052 Uiso 1 1 calc R . . C43 C 0.59850(8) 1.20999(13) 0.98781(8) 0.0291(5) Uani 1 1 d . . . C44 C 0.57704(9) 1.17713(14) 0.94254(9) 0.0373(6) Uani 1 1 d . . . H44 H 0.5433 1.1891 0.9249 0.045 Uiso 1 1 calc R . . C45 C 0.60465(9) 1.12752(16) 0.92341(9) 0.0427(6) Uani 1 1 d . . . H45 H 0.5900 1.1073 0.8928 0.051 Uiso 1 1 calc R . . C46 C 0.56745(8) 1.26362(12) 1.00772(7) 0.0245(4) Uani 1 1 d . . . C47 C 1.03553(8) 1.05344(13) 1.10311(7) 0.0260(4) Uani 1 1 d . . . C48 C 1.02799(9) 1.10290(13) 1.14198(8) 0.0303(5) Uani 1 1 d . . . C49 C 1.05274(12) 1.08496(17) 1.18965(9) 0.0539(8) Uani 1 1 d . . . H49 H 1.0752 1.0426 1.1973 0.065 Uiso 1 1 calc R . . C50 C 1.04474(15) 1.12828(18) 1.22541(9) 0.0677(10) Uani 1 1 d . . . H50 H 1.0626 1.1169 1.2572 0.081 Uiso 1 1 calc R . . C51 C 1.00999(13) 1.18914(15) 1.21419(9) 0.0508(8) Uani 1 1 d . . . C52 C 0.98622(12) 1.20970(15) 1.16768(9) 0.0454(7) Uani 1 1 d . . . H52 H 0.9641 1.2525 1.1604 0.055 Uiso 1 1 calc R . . C53 C 0.99513(10) 1.16678(14) 1.13163(8) 0.0386(6) Uani 1 1 d . . . H53 H 0.9789 1.1808 1.0999 0.046 Uiso 1 1 calc R . . Co1 Co 1.0000 1.0000 1.0000 0.02069(10) Uani 1 2 d S . . Co2 Co 0.957324(10) 0.832066(16) 0.983004(9) 0.02103(8) Uani 1 1 d . . . Co3 Co 1.071209(11) 0.891170(17) 1.080895(10) 0.02508(8) Uani 1 1 d . . . N1 N 0.91741(7) 0.76798(11) 0.92025(6) 0.0286(4) Uani 1 1 d . . . N2 N 0.65086(7) 0.60674(11) 0.62555(7) 0.0337(4) Uani 1 1 d . . . N3 N 0.93416(8) 0.24068(11) 0.53121(7) 0.0332(4) Uani 1 1 d . . . N4 N 0.94149(8) 0.18411(12) 0.86473(7) 0.0359(5) Uani 1 1 d . . . O1 O 0.93557(6) 0.54017(9) 0.71406(6) 0.0358(4) Uani 1 1 d . . . O2 O 0.67613(6) 1.05267(13) 0.92847(8) 0.0663(7) Uani 1 1 d . . . O3 O 1.0000 1.23340(15) 1.2500 0.0692(10) Uani 1 2 d S . . O4 O 0.89341(5) 0.90116(8) 0.97242(5) 0.0278(3) Uani 1 1 d . . . O5 O 0.91863(5) 1.02607(9) 0.97857(5) 0.0269(3) Uani 1 1 d . . . O6 O 0.59044(6) 1.29968(9) 1.04572(5) 0.0309(4) Uani 1 1 d . . . O7 O 0.52053(5) 1.26870(9) 0.98500(5) 0.0317(4) Uani 1 1 d . . . O8 O 1.06204(6) 0.99225(9) 1.11597(5) 0.0332(4) Uani 1 1 d . . . O9 O 1.01460(5) 1.07504(8) 1.06019(5) 0.0251(3) Uani 1 1 d . . . O10 O 0.99669(5) 0.90343(8) 1.03866(5) 0.0221(3) Uani 1 1 d . . . O11 O 0.93732(14) 1.0460(2) 0.59674(14) 0.1170(13) Uani 1 1 d . . . C56 C 0.9119(2) 0.9880(5) 0.5912(2) 0.139(3) Uani 1 1 d . . . H56 H 0.9121 0.9556 0.5659 0.166 Uiso 1 1 calc R . . N5 N 0.8822(3) 0.9642(5) 0.6187(4) 0.238(5) Uani 1 1 d . . . C55 C 0.8523(4) 0.8875(6) 0.6054(4) 0.271(6) Uani 1 1 d . . . H55A H 0.8645 0.8590 0.5831 0.325 Uiso 1 1 calc R . . H55B H 0.8164 0.8988 0.5910 0.325 Uiso 1 1 calc R . . H55C H 0.8572 0.8566 0.6337 0.325 Uiso 1 1 calc R . . C54 C 0.8907(7) 1.0275(10) 0.6658(5) 0.493(16) Uani 1 1 d . . . H54A H 0.9261 1.0273 0.6854 0.592 Uiso 1 1 calc R . . H54B H 0.8696 1.0112 0.6846 0.592 Uiso 1 1 calc R . . H54C H 0.8810 1.0794 0.6539 0.592 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 C1 0.0303(12) 0.0390(14) 0.0327(12) -0.0096(10) 0.0013(10) 0.0067(10) C2 0.0321(13) 0.0481(16) 0.0325(12) -0.0108(11) -0.0052(11) 0.0093(11) C3 0.0240(11) 0.0467(15) 0.0315(12) -0.0136(10) 0.0045(10) -0.0003(10) C4 0.0363(13) 0.0352(14) 0.0337(12) -0.0120(10) 0.0047(11) 0.0029(10) C5 0.0364(13) 0.0333(13) 0.0271(11) -0.0022(9) 0.0034(10) 0.0017(10) C6 0.0306(12) 0.0440(15) 0.0298(12) -0.0144(10) -0.0011(10) 0.0048(10) C7 0.0334(13) 0.0561(17) 0.0394(14) -0.0188(12) -0.0013(11) 0.0103(12) C8 0.0313(13) 0.0443(15) 0.0342(13) -0.0086(11) -0.0056(11) 0.0028(10) C9 0.0422(14) 0.0385(14) 0.0262(11) -0.0098(10) 0.0010(11) -0.0002(11) C10 0.0367(13) 0.0279(12) 0.0288(11) -0.0020(9) 0.0073(10) 0.0014(9) C11 0.0285(12) 0.0404(14) 0.0288(12) -0.0054(10) -0.0011(10) 0.0041(10) C12 0.0318(13) 0.0501(16) 0.0319(12) -0.0125(11) -0.0050(11) 0.0035(11) C13 0.0400(15) 0.0432(16) 0.0568(17) -0.0016(13) -0.0075(13) -0.0085(12) C14 0.0405(15) 0.0398(15) 0.0515(16) 0.0048(12) -0.0043(13) -0.0044(11) C15 0.0415(15) 0.0380(16) 0.0526(16) -0.0006(12) -0.0042(13) -0.0064(11) C16 0.0488(17) 0.0370(16) 0.0607(18) -0.0023(13) -0.0123(14) 0.0028(12) C17 0.0343(13) 0.0327(13) 0.0316(12) -0.0025(9) 0.0122(10) 0.0047(10) C18 0.0498(15) 0.0339(14) 0.0285(12) 0.0024(10) 0.0165(11) 0.0043(11) C19 0.0501(15) 0.0338(14) 0.0293(12) 0.0008(10) 0.0178(11) 0.0069(11) C20 0.0552(16) 0.0315(13) 0.0341(13) 0.0020(10) 0.0202(12) 0.0060(11) C21 0.0428(14) 0.0390(14) 0.0294(12) 0.0026(10) 0.0151(11) 0.0078(11) C22 0.0409(14) 0.0405(14) 0.0267(11) -0.0015(10) 0.0121(11) 0.0068(11) C23 0.0537(16) 0.0350(14) 0.0301(12) 0.0009(10) 0.0179(12) 0.0061(11) C24 0.084(2) 0.0345(15) 0.0455(15) -0.0104(12) 0.0342(16) -0.0141(14) C25 0.074(2) 0.0378(15) 0.0379(14) -0.0058(11) 0.0292(14) -0.0144(13) C26 0.0548(16) 0.0414(15) 0.0394(14) -0.0101(11) 0.0251(13) -0.0106(12) C27 0.0663(19) 0.0427(16) 0.0443(15) -0.0057(12) 0.0356(14) -0.0106(13) C28 0.0441(14) 0.0380(14) 0.0291(12) 0.0027(10) 0.0135(11) 0.0063(11) C29 0.108(3) 0.0477(18) 0.0464(16) 0.0062(13) 0.0480(18) 0.0201(17) C30 0.099(3) 0.0405(17) 0.0531(17) 0.0099(13) 0.0444(18) 0.0195(16) C31 0.102(2) 0.0402(17) 0.0304(13) -0.0021(11) 0.0275(15) -0.0012(15) C32 0.104(3) 0.0363(16) 0.0366(14) 0.0017(11) 0.0323(16) 0.0083(15) C33 0.0244(11) 0.0313(12) 0.0187(10) 0.0004(8) 0.0071(9) 0.0062(9) C34 0.0237(11) 0.0352(13) 0.0316(12) -0.0005(9) 0.0099(10) 0.0083(9) C35 0.0309(12) 0.0381(14) 0.0476(15) -0.0055(11) 0.0144(11) 0.0089(10) C36 0.0392(15) 0.0411(16) 0.0653(18) -0.0118(13) 0.0187(14) 0.0180(12) C37 0.0255(13) 0.0620(19) 0.0548(16) -0.0178(14) 0.0135(12) 0.0127(12) C38 0.0263(13) 0.0514(18) 0.080(2) -0.0152(15) 0.0192(14) 0.0021(11) C39 0.0305(13) 0.0343(14) 0.0712(18) -0.0039(13) 0.0189(13) 0.0073(10) C40 0.0246(12) 0.0530(17) 0.0543(16) -0.0206(13) 0.0123(12) 0.0112(10) C41 0.0254(13) 0.077(2) 0.0525(16) -0.0201(15) 0.0003(12) 0.0212(13) C42 0.0275(13) 0.0569(17) 0.0406(14) -0.0162(12) 0.0027(11) 0.0073(11) C43 0.0236(11) 0.0302(12) 0.0342(12) -0.0024(9) 0.0104(10) 0.0059(9) C44 0.0242(12) 0.0469(15) 0.0373(13) -0.0076(11) 0.0046(10) 0.0155(10) C45 0.0293(13) 0.0542(17) 0.0396(14) -0.0173(12) 0.0039(11) 0.0131(11) C46 0.0233(11) 0.0264(11) 0.0242(10) 0.0019(8) 0.0082(9) 0.0045(8) C47 0.0265(11) 0.0294(12) 0.0234(10) -0.0014(9) 0.0098(9) 0.0022(9) C48 0.0427(13) 0.0283(12) 0.0238(11) -0.0002(9) 0.0158(10) 0.0019(9) C49 0.088(2) 0.0462(17) 0.0259(13) 0.0001(11) 0.0151(14) 0.0205(15) C50 0.129(3) 0.0536(19) 0.0204(12) -0.0012(12) 0.0241(16) 0.0204(19) C51 0.108(2) 0.0264(14) 0.0340(13) -0.0015(10) 0.0446(16) 0.0006(14) C52 0.078(2) 0.0315(14) 0.0388(14) 0.0043(11) 0.0354(14) 0.0118(13) C53 0.0573(16) 0.0373(14) 0.0260(12) 0.0018(10) 0.0201(12) 0.0085(11) Co1 0.0216(2) 0.0225(2) 0.01724(18) 0.00098(14) 0.00508(16) 0.00427(15) Co2 0.01989(14) 0.02338(15) 0.01950(14) -0.00155(10) 0.00581(11) 0.00438(10) Co3 0.02523(16) 0.02773(17) 0.01901(14) -0.00021(11) 0.00242(12) 0.00668(11) N1 0.0269(10) 0.0326(11) 0.0256(9) -0.0055(8) 0.0073(8) 0.0003(8) N2 0.0321(10) 0.0356(11) 0.0269(10) -0.0013(8) 0.0004(8) -0.0055(8) N3 0.0411(11) 0.0306(11) 0.0305(10) -0.0012(8) 0.0149(9) -0.0004(8) N4 0.0416(12) 0.0383(12) 0.0272(10) 0.0040(8) 0.0099(9) 0.0057(9) O1 0.0390(9) 0.0333(9) 0.0388(9) -0.0051(7) 0.0175(8) 0.0005(7) O2 0.0253(9) 0.0849(16) 0.0802(15) -0.0462(12) 0.0047(10) 0.0209(9) O3 0.162(3) 0.0287(14) 0.0454(16) 0.000 0.074(2) 0.000 O4 0.0231(8) 0.0256(8) 0.0349(8) 0.0010(6) 0.0095(7) 0.0074(6) O5 0.0219(8) 0.0283(8) 0.0304(8) 0.0008(6) 0.0081(6) 0.0052(6) O6 0.0294(8) 0.0329(9) 0.0267(8) -0.0050(6) 0.0038(7) 0.0102(6) O7 0.0219(8) 0.0350(9) 0.0351(8) -0.0087(7) 0.0047(7) 0.0114(6) O8 0.0398(9) 0.0354(9) 0.0213(7) -0.0032(6) 0.0053(7) 0.0129(7) O9 0.0303(8) 0.0272(8) 0.0176(7) -0.0008(6) 0.0075(6) 0.0044(6) O10 0.0233(7) 0.0228(8) 0.0189(7) 0.0013(5) 0.0046(6) 0.0038(5) O11 0.124(3) 0.108(3) 0.151(3) 0.054(2) 0.089(3) 0.025(2) C56 0.092(4) 0.213(8) 0.119(4) 0.076(5) 0.044(4) 0.036(4) N5 0.161(5) 0.230(8) 0.381(11) 0.190(8) 0.167(7) 0.056(5) C55 0.187(9) 0.313(14) 0.304(12) 0.159(11) 0.066(9) -0.018(9) C54 0.78(3) 0.49(2) 0.421(19) 0.175(18) 0.49(2) 0.39(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.338(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9300 . ? C2 C3 1.381(3) . ? C2 H2 0.9300 . ? C3 C4 1.389(3) . ? C3 C6 1.477(3) . ? C4 C5 1.376(3) . ? C4 H4 0.9300 . ? C5 N1 1.332(3) . ? C5 H5 0.9300 . ? C6 C7 1.386(3) . ? C6 C11 1.394(3) . ? C7 C8 1.392(3) . ? C7 H7 0.9300 . ? C8 C9 1.382(3) . ? C8 C12 1.488(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.366(3) . ? C10 O1 1.394(3) . ? C11 H11 0.9300 . ? C12 C16 1.368(4) . ? C12 C13 1.371(4) . ? C13 C14 1.370(4) . ? C13 H13 0.9300 . ? C14 N2 1.334(3) . ? C14 H14 0.9300 . ? C15 N2 1.317(3) . ? C15 C16 1.371(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.372(3) . ? C17 C22 1.374(3) . ? C17 O1 1.382(3) . ? C18 C19 1.390(3) . ? C18 H18 0.9300 . ? C19 C20 1.388(3) . ? C19 C23 1.483(3) . ? C20 C21 1.387(3) . ? C20 H20 0.9300 . ? C21 C22 1.392(3) . ? C21 C28 1.496(3) . ? C22 H22 0.9300 . ? C23 C27 1.381(4) . ? C23 C24 1.387(4) . ? C24 C25 1.373(3) . ? C24 H24 0.9300 . ? C25 N3 1.335(3) . ? C25 H25 0.9300 . ? C26 N3 1.338(3) . ? C26 C27 1.364(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C32 1.369(3) . ? C28 C29 1.375(4) . ? C29 C30 1.372(4) . ? C29 H29 0.9300 . ? C30 N4 1.322(3) . ? C30 H30 0.9300 . ? C31 N4 1.335(3) . ? C31 C32 1.374(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O4 1.249(2) . ? C33 O5 1.265(3) . ? C33 C34 1.502(3) . ? C34 C35 1.384(3) . ? C34 C39 1.387(3) . ? C35 C36 1.383(3) . ? C35 H35 0.9300 . ? C36 C37 1.362(4) . ? C36 H36 0.9300 . ? C37 C38 1.368(4) . ? C37 O2 1.389(3) . ? C38 C39 1.376(3) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O2 1.376(3) . ? C40 C45 1.378(3) . ? C40 C41 1.380(4) . ? C41 C42 1.375(3) . ? C41 H41 0.9300 . ? C42 C43 1.380(3) . ? C42 H42 0.9300 . ? C43 C44 1.394(3) . ? C43 C46 1.493(3) . ? C44 C45 1.372(3) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 O7 1.251(2) . ? C46 O6 1.258(2) . ? C47 O8 1.261(2) . ? C47 O9 1.267(2) . ? C47 C48 1.491(3) . ? C48 C53 1.386(3) . ? C48 C49 1.387(3) . ? C49 C50 1.362(4) . ? C49 H49 0.9300 . ? C50 C51 1.378(4) . ? C50 H50 0.9300 . ? C51 C52 1.364(4) . ? C51 O3 1.395(3) . ? C52 C53 1.376(3) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? Co1 O10 2.0237(14) 5_777 ? Co1 O10 2.0237(14) . ? Co1 O9 2.1218(14) 5_777 ? Co1 O9 2.1218(14) . ? Co1 O5 2.1650(14) . ? Co1 O5 2.1650(14) 5_777 ? Co2 O7 2.0299(14) 3_545 ? Co2 O10 2.0539(14) . ? Co2 O4 2.0541(14) . ? Co2 N1 2.1293(17) . ? Co2 N3 2.1321(19) 6_566 ? Co2 O9 2.3151(15) 5_777 ? Co3 O6 2.0361(15) 3_545 ? Co3 O10 2.0390(14) . ? Co3 O8 2.0689(15) . ? Co3 N2 2.1640(19) 8_566 ? Co3 N4 2.169(2) 5_767 ? Co3 O5 2.3374(15) 5_777 ? N2 Co3 2.1640(19) 8_465 ? N3 Co2 2.1321(19) 6_565 ? N4 Co3 2.169(2) 5_767 ? O3 C51 1.395(3) 2_757 ? O5 Co3 2.3374(15) 5_777 ? O6 Co3 2.0361(15) 3_455 ? O7 Co2 2.0299(14) 3_455 ? O9 Co2 2.3151(15) 5_777 ? O11 C56 1.193(8) . ? C56 N5 1.380(7) . ? C56 H56 0.9300 . ? N5 C55 1.530(11) . ? N5 C54 1.719(16) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? 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 N1 C1 C2 123.2(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.5(2) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 117.3(2) . . ? C2 C3 C6 123.0(2) . . ? C4 C3 C6 119.7(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 123.3(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C6 C11 119.1(2) . . ? C7 C6 C3 120.7(2) . . ? C11 C6 C3 120.1(2) . . ? C6 C7 C8 120.4(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.0(2) . . ? C9 C8 C12 121.1(2) . . ? C7 C8 C12 118.9(2) . . ? C8 C9 C10 118.9(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 121.6(2) . . ? C11 C10 O1 118.4(2) . . ? C9 C10 O1 119.92(19) . . ? C10 C11 C6 119.8(2) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C16 C12 C13 116.9(2) . . ? C16 C12 C8 122.3(2) . . ? C13 C12 C8 120.8(2) . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N2 C14 C13 123.9(2) . . ? N2 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? N2 C15 C16 124.0(2) . . ? N2 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C12 C16 C15 119.9(3) . . ? C12 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C22 121.6(2) . . ? C18 C17 O1 117.3(2) . . ? C22 C17 O1 121.0(2) . . ? C17 C18 C19 119.5(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.1(2) . . ? C20 C19 C23 120.9(2) . . ? C18 C19 C23 120.0(2) . . ? C21 C20 C19 121.3(2) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 118.7(2) . . ? C20 C21 C28 120.9(2) . . ? C22 C21 C28 120.3(2) . . ? C17 C22 C21 119.7(2) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C27 C23 C24 116.5(2) . . ? C27 C23 C19 122.6(2) . . ? C24 C23 C19 120.8(2) . . ? C25 C24 C23 119.7(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? N3 C25 C24 123.7(2) . . ? N3 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N3 C26 C27 124.0(2) . . ? N3 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C26 C27 C23 119.9(2) . . ? C26 C27 H27 120.0 . . ? C23 C27 H27 120.0 . . ? C32 C28 C29 114.9(2) . . ? C32 C28 C21 121.8(2) . . ? C29 C28 C21 123.2(2) . . ? C30 C29 C28 121.4(3) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? N4 C30 C29 123.9(3) . . ? N4 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? N4 C31 C32 124.6(2) . . ? N4 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C28 C32 C31 120.4(3) . . ? C28 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? O4 C33 O5 125.27(19) . . ? O4 C33 C34 116.3(2) . . ? O5 C33 C34 118.46(19) . . ? C35 C34 C39 118.9(2) . . ? C35 C34 C33 121.9(2) . . ? C39 C34 C33 119.1(2) . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 119.5(2) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 121.5(2) . . ? C36 C37 O2 123.5(3) . . ? C38 C37 O2 114.7(2) . . ? C37 C38 C39 119.2(3) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C34 120.7(2) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? O2 C40 C45 113.8(2) . . ? O2 C40 C41 126.2(2) . . ? C45 C40 C41 119.9(2) . . ? C42 C41 C40 120.2(2) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.9(2) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C44 118.0(2) . . ? C42 C43 C46 121.8(2) . . ? C44 C43 C46 120.25(19) . . ? C45 C44 C43 121.5(2) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C44 C45 C40 119.5(2) . . ? C44 C45 H45 120.3 . . ? C40 C45 H45 120.3 . . ? O7 C46 O6 125.57(19) . . ? O7 C46 C43 116.81(18) . . ? O6 C46 C43 117.62(18) . . ? O8 C47 O9 125.20(19) . . ? O8 C47 C48 116.53(18) . . ? O9 C47 C48 118.27(18) . . ? C53 C48 C49 118.1(2) . . ? C53 C48 C47 121.1(2) . . ? C49 C48 C47 120.7(2) . . ? C50 C49 C48 121.1(3) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 119.6(3) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120.6(2) . . ? C52 C51 O3 118.4(2) . . ? C50 C51 O3 121.0(2) . . ? C51 C52 C53 119.6(2) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C48 120.8(2) . . ? C52 C53 H53 119.6 . . ? C48 C53 H53 119.6 . . ? O10 Co1 O10 180.000(1) 5_777 . ? O10 Co1 O9 92.94(5) 5_777 5_777 ? O10 Co1 O9 87.06(5) . 5_777 ? O10 Co1 O9 87.06(5) 5_777 . ? O10 Co1 O9 92.94(5) . . ? O9 Co1 O9 180.0 5_777 . ? O10 Co1 O5 83.97(5) 5_777 . ? O10 Co1 O5 96.03(6) . . ? O9 Co1 O5 88.71(5) 5_777 . ? O9 Co1 O5 91.29(5) . . ? O10 Co1 O5 96.03(6) 5_777 5_777 ? O10 Co1 O5 83.97(5) . 5_777 ? O9 Co1 O5 91.29(5) 5_777 5_777 ? O9 Co1 O5 88.71(5) . 5_777 ? O5 Co1 O5 180.0 . 5_777 ? O7 Co2 O10 93.78(6) 3_545 . ? O7 Co2 O4 172.55(6) 3_545 . ? O10 Co2 O4 89.26(6) . . ? O7 Co2 N1 87.11(6) 3_545 . ? O10 Co2 N1 173.75(6) . . ? O4 Co2 N1 89.14(6) . . ? O7 Co2 N3 95.94(7) 3_545 6_566 ? O10 Co2 N3 90.32(6) . 6_566 ? O4 Co2 N3 90.84(7) . 6_566 ? N1 Co2 N3 95.74(7) . 6_566 ? O7 Co2 O9 87.15(6) 3_545 5_777 ? O10 Co2 O9 81.40(5) . 5_777 ? O4 Co2 O9 86.58(5) . 5_777 ? N1 Co2 O9 92.48(6) . 5_777 ? N3 Co2 O9 171.35(6) 6_566 5_777 ? O6 Co3 O10 98.04(6) 3_545 . ? O6 Co3 O8 171.05(7) 3_545 . ? O10 Co3 O8 87.81(6) . . ? O6 Co3 N2 86.98(7) 3_545 8_566 ? O10 Co3 N2 173.15(7) . 8_566 ? O8 Co3 N2 86.67(7) . 8_566 ? O6 Co3 N4 92.89(7) 3_545 5_767 ? O10 Co3 N4 98.43(7) . 5_767 ? O8 Co3 N4 92.94(7) . 5_767 ? N2 Co3 N4 85.91(8) 8_566 5_767 ? O6 Co3 O5 88.26(6) 3_545 5_777 ? O10 Co3 O5 79.37(5) . 5_777 ? O8 Co3 O5 86.16(6) . 5_777 ? N2 Co3 O5 96.20(6) 8_566 5_777 ? N4 Co3 O5 177.65(6) 5_767 5_777 ? C5 N1 C1 117.08(19) . . ? C5 N1 Co2 118.57(14) . . ? C1 N1 Co2 122.76(15) . . ? C15 N2 C14 115.8(2) . . ? C15 N2 Co3 124.13(16) . 8_465 ? C14 N2 Co3 120.08(16) . 8_465 ? C25 N3 C26 115.9(2) . . ? C25 N3 Co2 122.21(17) . 6_565 ? C26 N3 Co2 119.66(16) . 6_565 ? C30 N4 C31 114.6(2) . . ? C30 N4 Co3 123.50(18) . 5_767 ? C31 N4 Co3 121.02(17) . 5_767 ? C17 O1 C10 115.24(18) . . ? C40 O2 C37 122.1(2) . . ? C51 O3 C51 114.4(3) . 2_757 ? C33 O4 Co2 135.51(14) . . ? C33 O5 Co1 122.10(13) . . ? C33 O5 Co3 126.04(13) . 5_777 ? Co1 O5 Co3 89.15(5) . 5_777 ? C46 O6 Co3 133.77(14) . 3_455 ? C46 O7 Co2 140.99(14) . 3_455 ? C47 O8 Co3 133.76(14) . . ? C47 O9 Co1 124.39(13) . . ? C47 O9 Co2 128.67(14) . 5_777 ? Co1 O9 Co2 87.76(5) . 5_777 ? Co1 O10 Co3 102.22(6) . . ? Co1 O10 Co2 98.05(6) . . ? Co3 O10 Co2 126.69(7) . . ? O11 C56 N5 126.4(8) . . ? O11 C56 H56 116.8 . . ? N5 C56 H56 116.8 . . ? C56 N5 C55 118.1(10) . . ? C56 N5 C54 109.7(9) . . ? C55 N5 C54 132.0(8) . . ? N5 C55 H55A 109.5 . . ? N5 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N5 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? 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 -0.001 0.493 -0.006 4456 922 ' ' 2 0.000 0.956 0.250 19 1 ' ' 3 0.000 0.044 0.750 19 1 ' ' 4 0.500 0.456 0.250 19 1 ' ' 5 0.500 0.544 0.750 19 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.617 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.061