# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H76 Co4 N8 O18 S8' _chemical_formula_sum 'C23 H35 Co N2 O12.5 S2' _chemical_formula_weight 622.59 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' S S 0.1246 0.1234 '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 13.6908(15) _cell_length_b 34.250(4) _cell_length_c 14.9404(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.863(2) _cell_angle_gamma 90.00 _cell_volume 6668.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3452 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 23.88 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7912 _exptl_absorpt_correction_T_max 0.9069 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18286 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.1351 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 26.08 _reflns_number_total 6596 _reflns_number_gt 3048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 experimental data have been refined, and the restraints we have done are as follow: We have refined the bpe ligand containing N1 and N2 in the aspect of the disorder with the limit of the distance and thermal parameters (each pyridine ring along the link between N atom and contrapuntal C atom is symmetrical, and the shapes of two pyridine rings are similar at the same time) to make sure that all the atoms on each pyridine ring are coplanar with C21/C22. We also made the restraints to the thiophene ring, the distances between C-C double bond atoms in all the thiophene ring are equal, the distances between C-C single bond atoms are similar, the thiophene ring along the link between S atom and the center of meta-position C atoms is symmetrical, and at the same time, the shapes of all the thiophene ring are similar. We have made a limit of thermal parameters to all the atoms in each btdc ligand to ensure the atoms' ellipsoid shape are similar. Besides the limit above, we have also made a thermal parameters isotropic limit for part of the atoms whose thermal parameters are abnormal (c29 c31 c31' c39 c3 c13 c10). dfix 1.53 c23 c24 c23' c24 sadi c20 c24 c20' c24 flat n2 > c23 flat n2' > c23' dfix 1.49 c23 c20 c23' c20' sadi c23 c19 c23 c21 c23' c19' c23' c21' SIZE 0.37 0.24 0.15 flat s1 > c5 c1' flat s1' > c5' c1 flat c4 > o2 flat c4' > o2' simu .01 s1 > o2' simu .005 .005 5 s1 s1' simu .01 n2 > c23' TEMP -100 same n2 c22 < c18 same n2' > c22' same n2' c22' < c18' ; _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^)+(0.0128P)^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 6596 _refine_ls_number_parameters 434 _refine_ls_number_restraints 279 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.012 _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 N2 N -0.0606(13) 0.0989(5) 1.0279(13) 0.049(4) Uani 0.50 1 d PDU . . C18 C -0.1399(11) 0.0822(3) 0.9626(10) 0.058(3) Uani 0.50 1 d PDU . . H18A H -0.2081 0.0893 0.9614 0.070 Uiso 0.50 1 d PR . . C19 C -0.1282(9) 0.0559(3) 0.8970(8) 0.071(3) Uani 0.50 1 d PDU . . H19A H -0.1859 0.0447 0.8500 0.085 Uiso 0.50 1 d PR . . C20 C -0.0342(9) 0.0444(5) 0.8945(10) 0.086(4) Uani 0.50 1 d PDU . . C21 C 0.0445(10) 0.0630(5) 0.9534(9) 0.096(4) Uani 0.50 1 d PDU . . H21A H 0.1135 0.0576 0.9541 0.115 Uiso 0.50 1 d PR . . C22 C 0.0315(13) 0.0902(5) 1.0174(11) 0.088(5) Uani 0.50 1 d PDU . . H22A H 0.0885 0.1027 1.0622 0.105 Uiso 0.50 1 d PR . . C23 C -0.0221(9) 0.0155(3) 0.8211(8) 0.090(4) Uani 0.50 1 d PDU . . H23A H -0.0766 -0.0033 0.8064 0.108 Uiso 0.50 1 d PR . . H23B H 0.0421 0.0020 0.8444 0.108 Uiso 0.50 1 d PR . . C24 C -0.0281(10) 0.0376(2) 0.7325(8) 0.087(3) Uani 0.50 1 d PDU . . H24A H 0.0332 0.0530 0.7454 0.104 Uiso 0.50 1 d PR . . H24B H -0.0856 0.0551 0.7183 0.104 Uiso 0.50 1 d PR . . N2' N 0.0633(15) 0.0930(6) 0.4638(13) 0.054(4) Uani 0.50 1 d PDU . . C18' C 0.1268(12) 0.0680(4) 0.5240(11) 0.077(4) Uani 0.50 1 d PDU . . H18B H 0.1976 0.0706 0.5272 0.092 Uiso 0.50 1 d PR . . C19' C 0.0962(10) 0.0423(4) 0.5798(10) 0.088(4) Uani 0.50 1 d PDU . . H19B H 0.1478 0.0260 0.6212 0.106 Uiso 0.50 1 d PR . . C20' C 0.0005(10) 0.0396(4) 0.5798(8) 0.076(3) Uani 0.50 1 d PDU . . C21' C -0.0682(11) 0.0600(4) 0.5139(8) 0.070(3) Uani 0.50 1 d PDU . . H21B H -0.1394 0.0559 0.5075 0.084 Uiso 0.50 1 d PR . . C22' C -0.0359(13) 0.0864(5) 0.4580(9) 0.058(3) Uani 0.50 1 d PDU . . H22B H -0.0870 0.1012 0.4121 0.070 Uiso 0.50 1 d PR . . C23' C -0.0348(10) 0.0118(3) 0.6455(8) 0.099(4) Uani 0.50 1 d PDU . . H23C H -0.1037 0.0025 0.6182 0.119 Uiso 0.50 1 d PR . . H23D H 0.0112 -0.0101 0.6620 0.119 Uiso 0.50 1 d PR . . S1 S 0.3793(12) 0.0437(5) 0.4764(10) 0.091(3) Uani 0.50 1 d PDU . . C1 C 0.4420(9) 0.0006(4) 0.4744(9) 0.112(5) Uani 0.50 1 d PDU . . C2 C 0.4009(8) -0.0184(3) 0.3925(9) 0.137(5) Uani 0.50 1 d PDU . . H2A H 0.4242 -0.0435 0.3790 0.164 Uiso 0.50 1 d PR . . C3 C 0.3170(9) 0.0015(4) 0.3301(9) 0.130(5) Uani 0.50 1 d PDU . . H3A H 0.2798 -0.0071 0.2679 0.156 Uiso 0.50 1 d PR . . C4 C 0.2956(11) 0.0351(4) 0.3676(11) 0.101(5) Uani 0.50 1 d PDU . . C5 C 0.220(2) 0.0636(7) 0.325(2) 0.076(4) Uani 0.50 1 d PDU . . O1 O 0.216(2) 0.0974(9) 0.369(2) 0.056(5) Uani 0.50 1 d PDU . . O2 O 0.1508(14) 0.0531(4) 0.2481(14) 0.086(5) Uani 0.50 1 d PDU . . S1' S 0.6069(13) -0.0472(5) 0.5413(11) 0.101(3) Uani 0.50 1 d PDU . . C1' C 0.5266(9) -0.0120(4) 0.5570(9) 0.097(4) Uani 0.50 1 d PDU . . C2' C 0.5551(7) 0.0002(3) 0.6464(8) 0.093(3) Uani 0.50 1 d PDU . . H2'A H 0.5181 0.0201 0.6679 0.111 Uiso 0.50 1 d PR . . C3' C 0.6431(7) -0.0188(3) 0.7053(8) 0.083(3) Uani 0.50 1 d PDU . . H3'A H 0.6713 -0.0140 0.7715 0.100 Uiso 0.50 1 d PR . . C4' C 0.6811(10) -0.0451(4) 0.6566(10) 0.071(4) Uani 0.50 1 d PDU . . C5' C 0.7770(18) -0.0708(6) 0.6871(19) 0.051(3) Uani 0.50 1 d PDU . . O1' O 0.7821(19) -0.0918(9) 0.624(2) 0.041(4) Uani 0.50 1 d PDU . . O2' O 0.8341(12) -0.0672(4) 0.7668(12) 0.062(3) Uani 0.50 1 d PDU . . C6 C -0.2432(3) 0.23953(12) 0.4602(3) 0.0667(13) Uani 1 1 d . . . C7 C -0.3117(3) 0.23360(15) 0.3731(3) 0.1014(19) Uani 1 1 d . . . H7 H -0.3799 0.2434 0.3551 0.122 Uiso 1 1 calc R . . C8 C -0.2726(3) 0.21177(13) 0.3126(3) 0.0829(16) Uani 1 1 d . . . H8 H -0.3108 0.2059 0.2494 0.100 Uiso 1 1 calc R . . C9 C -0.1730(3) 0.19972(10) 0.3543(3) 0.0482(11) Uani 1 1 d . . . C10 C -0.1079(3) 0.17568(10) 0.3148(3) 0.0375(9) Uani 1 1 d . . . C11 C 0.3025(3) 0.17076(12) 0.4706(3) 0.0675(14) Uani 1 1 d . . . H11 H 0.3236 0.1571 0.4243 0.081 Uiso 1 1 calc R . . C12 C 0.3736(3) 0.19344(13) 0.5352(3) 0.0710(14) Uani 1 1 d . . . H12 H 0.4419 0.1947 0.5323 0.085 Uiso 1 1 calc R . . C13 C 0.3484(3) 0.21420(11) 0.6032(3) 0.0518(12) Uani 1 1 d . . . C14 C 0.2473(3) 0.21122(11) 0.6015(3) 0.0653(13) Uani 1 1 d . . . H14 H 0.2238 0.2253 0.6456 0.078 Uiso 1 1 calc R . . C15 C 0.1802(3) 0.18757(12) 0.5352(3) 0.0640(13) Uani 1 1 d . . . H15 H 0.1113 0.1859 0.5362 0.077 Uiso 1 1 calc R . . C16 C 0.4251(3) 0.23866(11) 0.6756(3) 0.0708(14) Uani 1 1 d . . . H16A H 0.3879 0.2563 0.7065 0.085 Uiso 1 1 calc R . . H16B H 0.4639 0.2551 0.6437 0.085 Uiso 1 1 calc R . . C17 C 0.5000 0.21402(15) 0.7500 0.0642(18) Uani 1 2 d S . . H17A H 0.4612 0.1970 0.7806 0.077 Uiso 0.50 1 calc PR . . H17B H 0.5388 0.1970 0.7194 0.077 Uiso 0.50 1 calc PR . . Co1 Co 0.09862(3) 0.133124(13) 0.36507(3) 0.03561(15) Uani 1 1 d . . . N1 N 0.2059(2) 0.16716(9) 0.4707(2) 0.0455(9) Uani 1 1 d . . . O3 O -0.01868(15) 0.16893(6) 0.36992(16) 0.0450(7) Uani 1 1 d . . . O4 O -0.14448(16) 0.16540(7) 0.23189(17) 0.0451(7) Uani 1 1 d . . . O5 O 0.0000 0.09962(8) 0.2500 0.0390(9) Uani 1 2 d S . . H5A H -0.0375 0.0849 0.2717 0.047 Uiso 1 1 d R . . S2 S -0.12846(7) 0.21752(3) 0.46751(8) 0.0660(4) 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 N2 0.047(6) 0.043(6) 0.050(7) -0.009(5) 0.006(6) -0.006(5) C18 0.068(6) 0.058(7) 0.052(7) -0.025(6) 0.021(5) -0.009(5) C19 0.095(6) 0.059(6) 0.053(7) -0.034(5) 0.014(6) 0.001(5) C20 0.103(7) 0.081(6) 0.067(7) -0.025(6) 0.014(6) 0.026(6) C21 0.093(7) 0.111(8) 0.075(9) -0.038(7) 0.012(6) 0.045(6) C22 0.075(6) 0.096(8) 0.073(9) -0.022(7) -0.005(7) 0.009(6) C23 0.127(8) 0.072(6) 0.069(8) -0.005(5) 0.024(7) 0.036(6) C24 0.150(9) 0.068(5) 0.053(8) 0.011(5) 0.049(7) 0.045(5) N2' 0.066(7) 0.067(8) 0.029(6) 0.000(5) 0.013(6) 0.007(6) C18' 0.090(7) 0.081(8) 0.059(7) 0.020(6) 0.022(6) 0.022(6) C19' 0.126(8) 0.066(7) 0.062(7) 0.026(6) 0.013(7) 0.010(7) C20' 0.123(8) 0.056(6) 0.048(6) 0.008(5) 0.025(6) 0.010(6) C21' 0.111(7) 0.071(6) 0.031(6) 0.004(5) 0.024(6) -0.015(6) C22' 0.085(7) 0.075(7) 0.021(5) 0.003(5) 0.024(5) -0.007(6) C23' 0.160(9) 0.077(6) 0.059(7) 0.029(5) 0.031(7) 0.026(6) S1 0.063(3) 0.096(3) 0.086(5) -0.027(3) -0.017(3) 0.049(3) C1 0.082(8) 0.104(8) 0.107(9) -0.038(6) -0.036(6) 0.068(6) C2 0.103(8) 0.114(8) 0.136(9) -0.040(7) -0.047(7) 0.074(6) C3 0.103(8) 0.107(8) 0.123(9) -0.039(7) -0.050(7) 0.064(6) C4 0.083(7) 0.078(8) 0.094(9) -0.036(6) -0.045(6) 0.049(6) C5 0.070(6) 0.057(7) 0.069(8) -0.017(6) -0.024(6) 0.033(5) O1 0.053(7) 0.040(8) 0.050(8) -0.001(7) -0.020(6) 0.018(5) O2 0.083(7) 0.062(8) 0.076(8) -0.019(6) -0.028(6) 0.035(6) S1' 0.077(4) 0.098(3) 0.093(5) -0.032(4) -0.026(3) 0.049(3) C1' 0.064(6) 0.101(7) 0.098(7) -0.033(6) -0.017(5) 0.053(5) C2' 0.066(6) 0.104(7) 0.091(7) -0.021(6) 0.000(5) 0.049(5) C3' 0.065(6) 0.089(7) 0.080(7) -0.018(5) -0.001(5) 0.045(5) C4' 0.054(6) 0.071(7) 0.065(7) -0.017(5) -0.015(5) 0.036(5) C5' 0.042(5) 0.054(7) 0.050(6) -0.002(6) 0.001(5) 0.022(5) O1' 0.032(6) 0.043(8) 0.046(7) 0.004(6) 0.008(6) 0.015(5) O2' 0.054(5) 0.064(7) 0.051(6) -0.012(6) -0.008(4) 0.029(5) C6 0.051(2) 0.090(3) 0.057(4) -0.025(3) 0.014(3) 0.027(2) C7 0.055(3) 0.168(5) 0.069(4) -0.043(4) 0.002(3) 0.051(3) C8 0.052(3) 0.135(4) 0.051(3) -0.028(3) 0.001(3) 0.033(3) C9 0.045(2) 0.063(3) 0.033(3) -0.010(2) 0.006(2) 0.014(2) C10 0.042(2) 0.036(2) 0.037(3) 0.001(2) 0.016(2) 0.0042(18) C11 0.037(2) 0.099(4) 0.062(3) -0.031(3) 0.009(2) -0.007(2) C12 0.039(2) 0.097(4) 0.071(4) -0.024(3) 0.008(3) -0.013(2) C13 0.051(3) 0.036(2) 0.047(3) 0.002(2) -0.016(2) 0.001(2) C14 0.060(3) 0.077(3) 0.049(3) -0.034(2) 0.002(3) 0.008(2) C15 0.035(2) 0.094(4) 0.051(3) -0.019(3) -0.005(2) -0.005(2) C16 0.067(3) 0.053(3) 0.061(3) -0.010(2) -0.027(3) 0.000(2) C17 0.068(4) 0.053(4) 0.044(4) 0.000 -0.023(3) 0.000 Co1 0.0288(2) 0.0412(3) 0.0309(3) 0.0002(3) 0.0005(2) 0.0025(2) N1 0.0374(18) 0.062(2) 0.032(2) -0.0120(17) 0.0025(17) -0.0009(16) O3 0.0319(13) 0.0581(17) 0.0384(17) -0.0066(13) 0.0008(13) 0.0098(12) O4 0.0422(14) 0.0577(17) 0.0331(17) -0.0044(14) 0.0080(14) 0.0116(12) O5 0.0369(17) 0.040(2) 0.035(2) 0.000 0.0025(17) 0.000 S2 0.0470(6) 0.0968(9) 0.0484(8) -0.0179(7) 0.0062(6) 0.0245(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N2 N2' 0.25(4) 2_556 ? N2 C22' 1.34(3) 2_556 ? N2 C18 1.344(10) . ? N2 C22 1.352(11) . ? N2 C18' 1.45(3) 2_556 ? N2 Co1 2.171(16) 2_556 ? C18 C18' 0.54(2) 2_556 ? C18 N2' 1.32(3) 2_556 ? C18 C19 1.378(10) . ? C18 C19' 1.69(2) 2_556 ? C18 H18A 0.9600 . ? C19 C19' 0.660(16) 2_556 ? C19 C18' 1.25(2) 2_556 ? C19 C20 1.357(10) . ? C19 H19A 0.9602 . ? C20 C20' 0.53(2) 2_556 ? C20 C19' 1.04(2) 2_556 ? C20 C21 1.328(11) . ? C20 C23 1.521(11) . ? C20 C23' 1.69(2) 2_556 ? C21 C21' 0.51(2) 2_556 ? C21 C20' 1.04(2) 2_556 ? C21 C22 1.383(11) . ? C21 C22' 1.58(2) 2_556 ? C21 H21A 0.9601 . ? C22 C22' 0.38(3) 2_556 ? C22 C21' 1.30(3) 2_556 ? C22 N2' 1.41(4) 2_556 ? C22 H22A 0.9599 . ? C23 C23' 0.796(16) 2_556 ? C23 C24 1.42(2) 2_556 ? C23 C24 1.505(11) . ? C23 C20' 1.640(19) 2_556 ? C23 H23A 0.9600 . ? C23 H23B 0.9599 . ? C24 C24 0.79(2) 2_556 ? C24 C23 1.42(2) 2_556 ? C24 C23' 1.551(11) . ? C24 H24A 0.9599 . ? C24 H24B 0.9600 . ? N2' N2 0.25(4) 2_556 ? N2' C18 1.32(3) 2_556 ? N2' C18' 1.349(11) . ? N2' C22' 1.352(11) . ? N2' C22 1.41(4) 2_556 ? N2' Co1 2.177(16) . ? C18' C18 0.54(2) 2_556 ? C18' C19 1.25(2) 2_556 ? C18' C19' 1.364(11) . ? C18' N2 1.45(3) 2_556 ? C18' H18B 0.9601 . ? C19' C19 0.660(16) 2_556 ? C19' C20 1.04(2) 2_556 ? C19' C20' 1.314(11) . ? C19' C18 1.69(2) 2_556 ? C19' H19B 0.9601 . ? C20' C20 0.53(2) 2_556 ? C20' C21 1.04(2) 2_556 ? C20' C21' 1.332(10) . ? C20' C23' 1.548(11) . ? C20' C23 1.640(19) 2_556 ? C21' C21 0.51(2) 2_556 ? C21' C22 1.30(3) 2_556 ? C21' C22' 1.392(10) . ? C21' H21B 0.9601 . ? C22' C22 0.38(3) 2_556 ? C22' N2 1.34(3) 2_556 ? C22' C21 1.58(2) 2_556 ? C22' H22B 0.9600 . ? C23' C23 0.796(16) 2_556 ? C23' C20 1.69(2) 2_556 ? C23' H23C 0.9600 . ? C23' H23D 0.9600 . ? S1 S1' 0.39(4) 5_656 ? S1 C4 1.703(11) . ? S1 C1 1.712(10) . ? S1 C1' 1.87(3) 5_656 ? S1 C4' 1.90(3) 5_656 ? C1 C1' 0.83(2) 5_656 ? C1 C2 1.347(10) . ? C1 C1' 1.475(9) . ? C1 C1 1.54(2) 5_656 ? C1 S1' 1.72(3) 5_656 ? C2 C2' 1.142(15) 5_656 ? C2 C3 1.412(10) . ? C2 C1' 1.48(2) 5_656 ? C2 H2A 0.9600 . ? C3 C3' 1.052(16) 5_656 ? C3 C4 1.351(11) . ? C3 C4' 1.51(2) 5_656 ? C3 C2' 1.677(16) 5_656 ? C3 H3A 0.9600 . ? C4 C4' 0.65(3) 5_656 ? C4 C5 1.43(3) . ? C4 C5' 1.63(3) 5_656 ? C4 S1' 1.64(3) 5_656 ? C4 C3' 1.66(2) 5_656 ? C5 C5' 0.32(3) 5_656 ? C5 O1' 1.23(3) 5_656 ? C5 O2 1.30(3) . ? C5 O1 1.34(5) . ? C5 O2' 1.35(4) 5_656 ? C5 C4' 1.45(3) 5_656 ? O1 O1' 0.21(6) 5_656 ? O1 C5' 1.26(3) 5_656 ? O1 Co1 2.01(3) . ? O2 O2' 0.59(2) 5_656 ? O2 C5' 1.30(4) 5_656 ? S1' S1 0.39(4) 5_656 ? S1' C4 1.64(3) 5_656 ? S1' C1' 1.695(11) . ? S1' C4' 1.712(11) . ? S1' C1 1.72(3) 5_656 ? C1' C1 0.83(2) 5_656 ? C1' C2' 1.339(10) . ? C1' C2 1.48(2) 5_656 ? C1' S1 1.87(3) 5_656 ? C2' C2 1.142(15) 5_656 ? C2' C3' 1.414(9) . ? C2' C3 1.677(16) 5_656 ? C2' H2'A 0.9601 . ? C3' C3 1.052(16) 5_656 ? C3' C4' 1.358(10) . ? C3' C4 1.66(2) 5_656 ? C3' H3'A 0.9600 . ? C4' C4 0.65(3) 5_656 ? C4' C5 1.45(3) 5_656 ? C4' C3 1.51(2) 5_656 ? C4' C5' 1.53(2) . ? C4' S1 1.90(3) 5_656 ? C5' C5 0.32(3) 5_656 ? C5' O1' 1.20(5) . ? C5' O2' 1.22(3) . ? C5' O1 1.26(3) 5_656 ? C5' O2 1.30(4) 5_656 ? C5' C4 1.63(3) 5_656 ? O1' O1 0.21(6) 5_656 ? O1' C5 1.23(3) 5_656 ? O1' Co1 2.13(3) 5_656 ? O2' O2 0.59(2) 5_656 ? O2' C5 1.35(4) 5_656 ? C6 C7 1.366(5) . ? C6 C6 1.448(7) 7_456 ? C6 S2 1.716(4) . ? C7 C8 1.400(5) . ? C7 H7 0.9500 . ? C8 C9 1.377(4) . ? C8 H8 0.9500 . ? C9 C10 1.464(4) . ? C9 S2 1.724(4) . ? C10 O4 1.237(4) . ? C10 O3 1.267(4) . ? C11 N1 1.329(4) . ? C11 C12 1.380(5) . ? C11 H11 0.9500 . ? C12 C13 1.369(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 C16 1.510(4) . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 N1 1.323(4) . ? C15 H15 0.9500 . ? C16 C17 1.516(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C16 1.516(4) 2_656 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? Co1 O3 2.039(2) . ? Co1 O4 2.067(2) 2 ? Co1 O1' 2.13(3) 5_656 ? Co1 N1 2.141(3) . ? Co1 O5 2.1614(15) . ? Co1 N2 2.171(16) 2_556 ? O4 Co1 2.067(2) 2 ? O5 Co1 2.1615(15) 2 ? O5 H5A 0.8499 . ? 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 N2' N2 C22' 87(9) 2_556 2_556 ? N2' N2 C18 79(8) 2_556 . ? C22' N2 C18 121.1(13) 2_556 . ? N2' N2 C22 99(8) 2_556 . ? C22' N2 C22 16.1(13) 2_556 . ? C18 N2 C22 113.4(11) . . ? N2' N2 C18' 60(7) 2_556 2_556 ? C22' N2 C18' 106.0(15) 2_556 2_556 ? C18 N2 C18' 21.6(9) . 2_556 ? C22 N2 C18' 103.2(12) . 2_556 ? N2' N2 Co1 88(7) 2_556 2_556 ? C22' N2 Co1 120.1(13) 2_556 2_556 ? C18 N2 Co1 116.2(10) . 2_556 ? C22 N2 Co1 130.4(10) . 2_556 ? C18' N2 Co1 122.4(14) 2_556 2_556 ? C18' C18 N2' 82(3) 2_556 2_556 ? C18' C18 N2 91(3) 2_556 . ? N2' C18 N2 10.5(18) 2_556 . ? C18' C18 C19 65(3) 2_556 . ? N2' C18 C19 122.7(14) 2_556 . ? N2 C18 C19 123.4(10) . . ? C18' C18 C19' 45(2) 2_556 2_556 ? N2' C18 C19' 104.8(14) 2_556 2_556 ? N2 C18 C19' 108.4(10) . 2_556 ? C19 C18 C19' 21.9(7) . 2_556 ? C18' C18 H18A 116.7 2_556 . ? N2' C18 H18A 117.7 2_556 . ? N2 C18 H18A 118.0 . . ? C19 C18 H18A 118.6 . . ? C19' C18 H18A 130.7 2_556 . ? C19' C19 C18' 86(2) 2_556 2_556 ? C19' C19 C20 48(2) 2_556 . ? C18' C19 C20 112.6(13) 2_556 . ? C19' C19 C18 107(2) 2_556 . ? C18' C19 C18 22.9(10) 2_556 . ? C20 C19 C18 121.9(9) . . ? C19' C19 C20' 38.5(17) 2_556 2_556 ? C18' C19 C20' 101.1(12) 2_556 2_556 ? C20 C19 C20' 12.4(9) . 2_556 ? C18 C19 C20' 113.0(9) . 2_556 ? C19' C19 H19A 111.7 2_556 . ? C18' C19 H19A 126.5 2_556 . ? C20 C19 H19A 116.1 . . ? C18 C19 H19A 122.1 . . ? C20' C19 H19A 124.2 2_556 . ? C20' C20 C19' 110(4) 2_556 2_556 ? C20' C20 C21 47(3) 2_556 . ? C19' C20 C21 112.3(16) 2_556 . ? C20' C20 C19 134(3) 2_556 . ? C19' C20 C19 28.2(10) 2_556 . ? C21 C20 C19 115.2(10) . . ? C20' C20 C23 93(3) 2_556 . ? C19' C20 C23 120.3(17) 2_556 . ? C21 C20 C23 123.0(9) . . ? C19 C20 C23 121.4(9) . . ? C20' C20 C23' 66(2) 2_556 2_556 ? C19' C20 C23' 134.3(19) 2_556 2_556 ? C21 C20 C23' 97.2(9) . 2_556 ? C19 C20 C23' 147.3(11) . 2_556 ? C23 C20 C23' 28.2(6) . 2_556 ? C20' C20 C21' 37(2) 2_556 2_556 ? C19' C20 C21' 106.7(16) 2_556 2_556 ? C21 C20 C21' 12.4(11) . 2_556 ? C19 C20 C21' 115.9(11) . 2_556 ? C23 C20 C21' 122.3(10) . 2_556 ? C23' C20 C21' 94.6(9) 2_556 2_556 ? C21' C21 C20' 114(4) 2_556 2_556 ? C21' C21 C20 134(4) 2_556 . ? C20' C21 C20 21.7(12) 2_556 . ? C21' C21 C22 70(3) 2_556 . ? C20' C21 C22 131.7(17) 2_556 . ? C20 C21 C22 122.1(10) . . ? C21' C21 C22' 59(2) 2_556 2_556 ? C20' C21 C22' 127(2) 2_556 2_556 ? C20 C21 C22' 123.0(14) . 2_556 ? C22 C21 C22' 12.4(14) . 2_556 ? C21' C21 C19' 117(4) 2_556 2_556 ? C20' C21 C19' 37.9(10) 2_556 2_556 ? C20 C21 C19' 29.1(8) . 2_556 ? C22 C21 C19' 95.4(10) . 2_556 ? C22' C21 C19' 94.3(12) 2_556 2_556 ? C21' C21 H21A 67.3 2_556 . ? C20' C21 H21A 107.0 2_556 . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 117.3 . . ? C22' C21 H21A 114.5 2_556 . ? C19' C21 H21A 144.7 2_556 . ? C22' C22 C21' 97(5) 2_556 2_556 ? C22' C22 N2 81(5) 2_556 . ? C21' C22 N2 134.2(15) 2_556 . ? C22' C22 C21 116(5) 2_556 . ? C21' C22 C21 21.5(9) 2_556 . ? N2 C22 C21 123.4(11) . . ? C22' C22 N2' 73(5) 2_556 2_556 ? C21' C22 N2' 127(2) 2_556 2_556 ? N2 C22 N2' 9.9(17) . 2_556 ? C21 C22 N2' 120.3(14) . 2_556 ? C22' C22 H22A 67.6 2_556 . ? C21' C22 H22A 106.7 2_556 . ? N2 C22 H22A 114.0 . . ? C21 C22 H22A 122.3 . . ? N2' C22 H22A 115.5 2_556 . ? C23' C23 C24 83.6(18) 2_556 2_556 ? C23' C23 C24 114(2) 2_556 . ? C24 C23 C24 31.0(10) 2_556 . ? C23' C23 C20 87.5(15) 2_556 . ? C24 C23 C20 103.8(10) 2_556 . ? C24 C23 C20 108.6(8) . . ? C23' C23 C20' 69.2(13) 2_556 2_556 ? C24 C23 C20' 104.8(10) 2_556 2_556 ? C24 C23 C20' 119.2(11) . 2_556 ? C20 C23 C20' 18.7(8) . 2_556 ? C23' C23 H23A 125.3 2_556 . ? C24 C23 H23A 134.7 2_556 . ? C24 C23 H23A 107.9 . . ? C20 C23 H23A 110.7 . . ? C20' C23 H23A 117.3 2_556 . ? C23' C23 H23B 23.5 2_556 . ? C24 C23 H23B 85.0 2_556 . ? C24 C23 H23B 110.9 . . ? C20 C23 H23B 110.0 . . ? C20' C23 H23B 91.3 2_556 . ? H23A C23 H23B 108.7 . . ? C24 C24 C23 80.3(17) 2_556 2_556 ? C24 C24 C23 68.7(15) 2_556 . ? C23 C24 C23 108.9(10) 2_556 . ? C24 C24 C23' 110.6(18) 2_556 . ? C23 C24 C23' 30.7(7) 2_556 . ? C23 C24 C23' 115.1(6) . . ? C24 C24 C23' 47.5(12) 2_556 2_556 ? C23 C24 C23' 97.6(7) 2_556 2_556 ? C23 C24 C23' 21.6(7) . 2_556 ? C23' C24 C23' 114.5(8) . 2_556 ? C24 C24 H24A 41.3 2_556 . ? C23 C24 H24A 82.0 2_556 . ? C23 C24 H24A 106.9 . . ? C23' C24 H24A 107.8 . . ? C23' C24 H24A 87.3 2_556 . ? C24 C24 H24B 135.7 2_556 . ? C23 C24 H24B 135.4 2_556 . ? C23 C24 H24B 109.1 . . ? C23' C24 H24B 109.7 . . ? C23' C24 H24B 125.5 2_556 . ? H24A C24 H24B 108.0 . . ? N2 N2' C18 91(8) 2_556 2_556 ? N2 N2' C18' 110(8) 2_556 . ? C18 N2' C18' 23.1(9) 2_556 . ? N2 N2' C22' 83(8) 2_556 . ? C18 N2' C22' 122.3(15) 2_556 . ? C18' N2' C22' 111.5(11) . . ? N2 N2' C22 71(8) 2_556 2_556 ? C18 N2' C22 111.1(18) 2_556 2_556 ? C18' N2' C22 105.5(13) . 2_556 ? C22' N2' C22 15.5(13) . 2_556 ? N2 N2' Co1 85(7) 2_556 . ? C18 N2' Co1 117.2(14) 2_556 . ? C18' N2' Co1 128.4(11) . . ? C22' N2' Co1 119.3(10) . . ? C22 N2' Co1 125.9(13) 2_556 . ? C18 C18' C19 93(3) 2_556 2_556 ? C18 C18' N2' 75(3) 2_556 . ? C19 C18' N2' 131.5(14) 2_556 . ? C18 C18' C19' 119(3) 2_556 . ? C19 C18' C19' 28.8(7) 2_556 . ? N2' C18' C19' 124.1(11) . . ? C18 C18' N2 68(3) 2_556 2_556 ? C19 C18' N2 125(2) 2_556 2_556 ? N2' C18' N2 9.1(17) . 2_556 ? C19' C18' N2 122.6(14) . 2_556 ? C18 C18' H18B 71.4 2_556 . ? C19 C18' H18B 105.3 2_556 . ? N2' C18' H18B 114.1 . . ? C19' C18' H18B 121.6 . . ? N2 C18' H18B 114.5 2_556 . ? C19 C19' C20 104(3) 2_556 2_556 ? C19 C19' C20' 123(2) 2_556 . ? C20 C19' C20' 22.2(12) 2_556 . ? C19 C19' C18' 66(2) 2_556 . ? C20 C19' C18' 128.5(16) 2_556 . ? C20' C19' C18' 122.6(11) . . ? C19 C19' C18 51.2(16) 2_556 2_556 ? C20 C19' C18 120.5(18) 2_556 2_556 ? C20' C19' C18 121.6(13) . 2_556 ? C18' C19' C18 16.0(10) . 2_556 ? C19 C19' C21 109(2) 2_556 2_556 ? C20 C19' C21 38.6(10) 2_556 2_556 ? C20' C19' C21 29.1(8) . 2_556 ? C18' C19' C21 94.2(10) . 2_556 ? C18 C19' C21 92.6(10) 2_556 2_556 ? C19 C19' H19B 80.3 2_556 . ? C20 C19' H19B 109.0 2_556 . ? C20' C19' H19B 119.8 . . ? C18' C19' H19B 117.7 . . ? C18 C19' H19B 115.7 2_556 . ? C21 C19' H19B 147.2 2_556 . ? C20 C20' C21 112(4) 2_556 2_556 ? C20 C20' C19' 48(3) 2_556 . ? C21 C20' C19' 113.0(16) 2_556 . ? C20 C20' C21' 130(3) 2_556 . ? C21 C20' C21' 20.3(14) 2_556 . ? C19' C20' C21' 116.2(10) . . ? C20 C20' C23' 96(2) 2_556 . ? C21 C20' C23' 121.5(16) 2_556 . ? C19' C20' C23' 123.2(9) . . ? C21' C20' C23' 120.3(9) . . ? C20 C20' C23 68(2) 2_556 2_556 ? C21 C20' C23 137.3(19) 2_556 2_556 ? C19' C20' C23 97.5(10) . 2_556 ? C21' C20' C23 145.3(11) . 2_556 ? C23' C20' C23 28.8(6) . 2_556 ? C20 C20' C19 34(2) 2_556 2_556 ? C21 C20' C19 104.9(15) 2_556 2_556 ? C19' C20' C19 18.2(8) . 2_556 ? C21' C20' C19 114.3(10) . 2_556 ? C23' C20' C19 123.5(9) . 2_556 ? C23 C20' C19 95.0(8) 2_556 2_556 ? C21 C21' C22 89(3) 2_556 2_556 ? C21 C21' C20' 45(3) 2_556 . ? C22 C21' C20' 114.9(14) 2_556 . ? C21 C21' C22' 103(3) 2_556 . ? C22 C21' C22' 15.6(14) 2_556 . ? C20' C21' C22' 120.2(10) . . ? C21 C21' C20 34(3) 2_556 2_556 ? C22 C21' C20 103.0(14) 2_556 2_556 ? C20' C21' C20 13.7(9) . 2_556 ? C22' C21' C20 110.5(10) . 2_556 ? C21 C21' H21B 117.1 2_556 . ? C22 C21' H21B 125.1 2_556 . ? C20' C21' H21B 117.4 . . ? C22' C21' H21B 122.4 . . ? C20 C21' H21B 126.1 2_556 . ? C22 C22' N2 83(5) 2_556 2_556 ? C22 C22' N2' 91(5) 2_556 . ? N2 C22' N2' 10.4(18) 2_556 . ? C22 C22' C21' 68(5) 2_556 . ? N2 C22' C21' 126.2(13) 2_556 . ? N2' C22' C21' 124.5(10) . . ? C22 C22' C21 52(4) 2_556 2_556 ? N2 C22' C21 110.6(15) 2_556 2_556 ? N2' C22' C21 111.2(12) . 2_556 ? C21' C22' C21 18.2(9) . 2_556 ? C22 C22' H22B 112.4 2_556 . ? N2 C22' H22B 114.3 2_556 . ? N2' C22' H22B 117.1 . . ? C21' C22' H22B 118.4 . . ? C21 C22' H22B 129.8 2_556 . ? C23 C23' C20' 82.0(15) 2_556 . ? C23 C23' C24 65.7(17) 2_556 . ? C20' C23' C24 103.3(8) . . ? C23 C23' C20 64.3(13) 2_556 2_556 ? C20' C23' C20 18.1(7) . 2_556 ? C24 C23' C20 91.4(11) . 2_556 ? C23 C23' C24 44.2(14) 2_556 2_556 ? C20' C23' C24 100.2(8) . 2_556 ? C24 C23' C24 22.0(8) . 2_556 ? C20 C23' C24 84.1(7) 2_556 2_556 ? C23 C23' H23C 164.8 2_556 . ? C20' C23' H23C 113.1 . . ? C24 C23' H23C 110.1 . . ? C20 C23' H23C 130.8 2_556 . ? C24 C23' H23C 129.5 2_556 . ? C23 C23' H23D 61.8 2_556 . ? C20' C23' H23D 109.5 . . ? C24 C23' H23D 111.4 . . ? C20 C23' H23D 102.2 2_556 . ? C24 C23' H23D 92.7 2_556 . ? H23C C23' H23D 109.3 . . ? S1' S1 C4 74(4) 5_656 . ? S1' S1 C1 84(5) 5_656 . ? C4 S1 C1 91.6(7) . . ? S1' S1 C1' 58(4) 5_656 5_656 ? C4 S1 C1' 87.8(9) . 5_656 ? C1 S1 C1' 26.2(7) . 5_656 ? S1' S1 C4' 55(4) 5_656 5_656 ? C4 S1 C4' 19.7(8) . 5_656 ? C1 S1 C4' 93.6(8) . 5_656 ? C1' S1 C4' 81.4(9) 5_656 5_656 ? C1' C1 C2 81.8(18) 5_656 . ? C1' C1 C1' 101.6(17) 5_656 . ? C2 C1 C1' 128.3(8) . . ? C1' C1 C1 69.9(16) 5_656 5_656 ? C2 C1 C1 121.2(14) . 5_656 ? C1' C1 C1 31.8(9) . 5_656 ? C1' C1 S1 87.3(19) 5_656 . ? C2 C1 S1 111.1(8) . . ? C1' C1 S1 120.5(7) . . ? C1 C1 S1 117.5(13) 5_656 . ? C1' C1 S1' 74(2) 5_656 5_656 ? C2 C1 S1' 106.7(11) . 5_656 ? C1' C1 S1' 124.1(9) . 5_656 ? C1 C1 S1' 113.2(16) 5_656 5_656 ? S1 C1 S1' 13.0(12) . 5_656 ? C1' C1 C2' 43.0(14) 5_656 5_656 ? C2 C1 C2' 38.8(7) . 5_656 ? C1' C1 C2' 125.1(8) . 5_656 ? C1 C1 C2' 99.2(12) 5_656 5_656 ? S1 C1 C2' 101.2(8) . 5_656 ? S1' C1 C2' 90.3(10) 5_656 5_656 ? C2' C2 C1 93.5(12) 5_656 . ? C2' C2 C3 81.3(11) 5_656 . ? C1 C2 C3 113.2(9) . . ? C2' C2 C1' 59.9(8) 5_656 5_656 ? C1 C2 C1' 33.6(10) . 5_656 ? C3 C2 C1' 106.3(10) . 5_656 ? C2' C2 C3' 48.1(7) 5_656 5_656 ? C1 C2 C3' 108.7(9) . 5_656 ? C3 C2 C3' 33.3(7) . 5_656 ? C1' C2 C3' 85.6(8) 5_656 5_656 ? C2' C2 H2A 96.9 5_656 . ? C1 C2 H2A 123.4 . . ? C3 C2 H2A 123.3 . . ? C1' C2 H2A 121.6 5_656 . ? C3' C2 H2A 119.2 5_656 . ? C3' C3 C4 86.6(14) 5_656 . ? C3' C3 C2 99.3(12) 5_656 . ? C4 C3 C2 111.9(9) . . ? C3' C3 C4' 61.1(10) 5_656 5_656 ? C4 C3 C4' 25.5(11) . 5_656 ? C2 C3 C4' 114.5(10) . 5_656 ? C3' C3 C2' 57.0(9) 5_656 5_656 ? C4 C3 C2' 106.8(10) . 5_656 ? C2 C3 C2' 42.3(7) . 5_656 ? C4' C3 C2' 91.9(10) 5_656 5_656 ? C3' C3 H3A 83.7 5_656 . ? C4 C3 H3A 123.0 . . ? C2 C3 H3A 125.0 . . ? C4' C3 H3A 114.5 5_656 . ? C2' C3 H3A 113.7 5_656 . ? C4' C4 C3 91(2) 5_656 . ? C4' C4 C5 79(2) 5_656 . ? C3 C4 C5 128.4(15) . . ? C4' C4 C5' 70(2) 5_656 5_656 ? C3 C4 C5' 127.5(16) . 5_656 ? C5 C4 C5' 9.3(12) . 5_656 ? C4' C4 S1' 85(2) 5_656 5_656 ? C3 C4 S1' 109.5(11) . 5_656 ? C5 C4 S1' 119.5(15) . 5_656 ? C5' C4 S1' 116.3(16) 5_656 5_656 ? C4' C4 C3' 52(2) 5_656 5_656 ? C3 C4 C3' 39.2(8) . 5_656 ? C5 C4 C3' 112.6(13) . 5_656 ? C5' C4 C3' 106.0(14) 5_656 5_656 ? S1' C4 C3' 100.5(11) 5_656 5_656 ? C4' C4 S1 98(3) 5_656 . ? C3 C4 S1 112.0(8) . . ? C5 C4 S1 119.4(14) . . ? C5' C4 S1 118.4(15) 5_656 . ? S1' C4 S1 13.1(13) 5_656 . ? C3' C4 S1 110.9(10) 5_656 . ? C5' C5 O1' 77(10) 5_656 5_656 ? C5' C5 O2 84(10) 5_656 . ? O1' C5 O2 128(2) 5_656 . ? C5' C5 O1 69(10) 5_656 . ? O1' C5 O1 8(3) 5_656 . ? O2 C5 O1 123(3) . . ? C5' C5 O2' 58(10) 5_656 5_656 ? O1' C5 O2' 116(2) 5_656 5_656 ? O2 C5 O2' 25.8(11) . 5_656 ? O1 C5 O2' 109(3) . 5_656 ? C5' C5 C4 125(9) 5_656 . ? O1' C5 C4 115(2) 5_656 . ? O2 C5 C4 115.9(19) . . ? O1 C5 C4 121(3) . . ? O2' C5 C4 127(2) 5_656 . ? C5' C5 C4' 99(9) 5_656 5_656 ? O1' C5 C4' 115(2) 5_656 5_656 ? O2 C5 C4' 115(2) . 5_656 ? O1 C5 C4' 118(3) . 5_656 ? O2' C5 C4' 115(2) 5_656 5_656 ? C4 C5 C4' 26.1(11) . 5_656 ? O1' O1 C5' 68(10) 5_656 5_656 ? O1' O1 C5 55(10) 5_656 . ? C5' O1 C5 13.7(15) 5_656 . ? O1' O1 Co1 124(10) 5_656 . ? C5' O1 Co1 130(2) 5_656 . ? C5 O1 Co1 132(2) . . ? O2' O2 C5 82(3) 5_656 . ? O2' O2 C5' 68(3) 5_656 5_656 ? C5 O2 C5' 14.1(15) . 5_656 ? S1 S1' C4 93(5) 5_656 5_656 ? S1 S1' C1' 111(5) 5_656 . ? C4 S1' C1' 96.0(9) 5_656 . ? S1 S1' C4' 114(5) 5_656 . ? C4 S1' C4' 22.2(9) 5_656 . ? C1' S1' C4' 92.4(7) . . ? S1 S1' C1 83(5) 5_656 5_656 ? C4 S1' C1 93.7(12) 5_656 5_656 ? C1' S1' C1 28.0(8) . 5_656 ? C4' S1' C1 100.7(10) . 5_656 ? C1 C1' C2' 112(2) 5_656 . ? C1 C1' C1 78.3(17) 5_656 . ? C2' C1' C1 131.1(8) . . ? C1 C1' C2 64.6(15) 5_656 5_656 ? C2' C1' C2 47.5(8) . 5_656 ? C1 C1' C2 116.9(9) . 5_656 ? C1 C1' S1' 77(2) 5_656 . ? C2' C1' S1' 110.9(8) . . ? C1 C1' S1' 118.0(8) . . ? C2 C1' S1' 102.0(9) 5_656 . ? C1 C1' C1' 52.1(13) 5_656 5_656 ? C2' C1' C1' 134.3(14) . 5_656 ? C1 C1' C1' 26.2(7) . 5_656 ? C2 C1' C1' 99.8(11) 5_656 5_656 ? S1' C1' C1' 106.3(12) . 5_656 ? C1 C1' S1 66.4(17) 5_656 5_656 ? C2' C1' S1 115.7(10) . 5_656 ? C1 C1' S1 112.1(9) . 5_656 ? C2 C1' S1 97.8(11) 5_656 5_656 ? S1' C1' S1 11.2(12) . 5_656 ? C1' C1' S1 97.1(12) 5_656 5_656 ? C2 C2' C1' 72.6(12) 5_656 . ? C2 C2' C3' 95.0(10) 5_656 . ? C1' C2' C3' 114.1(9) . . ? C2 C2' C3 56.3(8) 5_656 5_656 ? C1' C2' C3 99.4(9) . 5_656 ? C3' C2' C3 38.6(6) . 5_656 ? C2 C2' C1 47.7(8) 5_656 5_656 ? C1' C2' C1 24.9(9) . 5_656 ? C3' C2' C1 109.7(9) . 5_656 ? C3 C2' C1 82.4(8) 5_656 5_656 ? C2 C2' H2'A 101.5 5_656 . ? C1' C2' H2'A 122.2 . . ? C3' C2' H2'A 123.7 . . ? C3 C2' H2'A 125.4 5_656 . ? C1 C2' H2'A 121.2 5_656 . ? C3 C3' C4' 76.2(13) 5_656 . ? C3 C3' C2' 84.3(11) 5_656 . ? C4' C3' C2' 111.5(8) . . ? C3 C3' C4 54.2(10) 5_656 5_656 ? C4' C3' C4 22.0(10) . 5_656 ? C2' C3' C4 104.6(10) . 5_656 ? C3 C3' C2 47.4(8) 5_656 5_656 ? C4' C3' C2 96.7(9) . 5_656 ? C2' C3' C2 36.9(6) . 5_656 ? C4 C3' C2 79.9(8) 5_656 5_656 ? C3 C3' H3'A 108.3 5_656 . ? C4' C3' H3'A 124.6 . . ? C2' C3' H3'A 123.9 . . ? C4 C3' H3'A 127.5 5_656 . ? C2 C3' H3'A 127.7 5_656 . ? C4 C4' C3' 106(2) 5_656 . ? C4 C4' C5 75(2) 5_656 5_656 ? C3' C4' C5 133.0(17) . 5_656 ? C4 C4' C3 64(2) 5_656 5_656 ? C3' C4' C3 42.7(8) . 5_656 ? C5 C4' C3 115.7(16) 5_656 5_656 ? C4 C4' C5' 87(2) 5_656 . ? C3' C4' C5' 131.1(13) . . ? C5 C4' C5' 11.9(12) 5_656 . ? C3 C4' C5' 123.7(12) 5_656 . ? C4 C4' S1' 73(2) 5_656 . ? C3' C4' S1' 111.1(8) . . ? C5 C4' S1' 113.8(16) 5_656 . ? C3 C4' S1' 98.9(10) 5_656 . ? C5' C4' S1' 117.8(13) . . ? C4 C4' S1 62(2) 5_656 5_656 ? C3' C4' S1 115.3(10) . 5_656 ? C5 C4' S1 106.8(16) 5_656 5_656 ? C3 C4' S1 95.6(11) 5_656 5_656 ? C5' C4' S1 112.5(13) . 5_656 ? S1' C4' S1 10.7(12) . 5_656 ? C5 C5' O1' 88(10) 5_656 . ? C5 C5' O2' 109(10) 5_656 . ? O1' C5' O2' 131(3) . . ? C5 C5' O1 97(10) 5_656 5_656 ? O1' C5' O1 10(3) . 5_656 ? O2' C5' O1 125(2) . 5_656 ? C5 C5' O2 82(10) 5_656 5_656 ? O1' C5' O2 130(3) . 5_656 ? O2' C5' O2 27.0(13) . 5_656 ? O1 C5' O2 129(2) 5_656 5_656 ? C5 C5' C4' 69(9) 5_656 . ? O1' C5' C4' 111(3) . . ? O2' C5' C4' 117.9(18) . . ? O1 C5' C4' 117(2) 5_656 . ? O2 C5' C4' 110(2) 5_656 . ? C5 C5' C4 46(8) 5_656 5_656 ? O1' C5' C4 103(3) . 5_656 ? O2' C5' C4 122(2) . 5_656 ? O1 C5' C4 112(2) 5_656 5_656 ? O2 C5' C4 103.3(18) 5_656 5_656 ? C4' C5' C4 23.4(10) . 5_656 ? O1 O1' C5' 102(10) 5_656 . ? O1 O1' C5 117(10) 5_656 5_656 ? C5' O1' C5 15.1(16) . 5_656 ? O1 O1' Co1 52(10) 5_656 5_656 ? C5' O1' Co1 125(3) . 5_656 ? C5 O1' Co1 129(2) 5_656 5_656 ? O2 O2' C5' 85(4) 5_656 . ? O2 O2' C5 72(3) 5_656 5_656 ? C5' O2' C5 12.9(15) . 5_656 ? C7 C6 C6 129.2(5) . 7_456 ? C7 C6 S2 110.1(3) . . ? C6 C6 S2 120.7(4) 7_456 . ? C6 C7 C8 114.1(4) . . ? C6 C7 H7 123.0 . . ? C8 C7 H7 123.0 . . ? C9 C8 C7 112.9(4) . . ? C9 C8 H8 123.5 . . ? C7 C8 H8 123.5 . . ? C8 C9 C10 128.8(4) . . ? C8 C9 S2 110.0(3) . . ? C10 C9 S2 121.2(3) . . ? O4 C10 O3 127.8(4) . . ? O4 C10 C9 117.0(3) . . ? O3 C10 C9 115.2(3) . . ? N1 C11 C12 122.7(4) . . ? N1 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 121.8(4) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 115.3(4) . . ? C12 C13 C16 122.8(4) . . ? C14 C13 C16 121.9(4) . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N1 C15 C14 124.3(4) . . ? N1 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? C13 C16 C17 112.4(3) . . ? C13 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? C13 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C16 112.3(4) 2_656 . ? C16 C17 H17A 109.1 2_656 . ? C16 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 2_656 . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? O1 Co1 O3 176.4(9) . . ? O1 Co1 O4 86.2(9) . 2 ? O3 Co1 O4 96.61(9) . 2 ? O1 Co1 O1' 4.8(15) . 5_656 ? O3 Co1 O1' 172.4(7) . 5_656 ? O4 Co1 O1' 90.9(7) 2 5_656 ? O1 Co1 N1 87.1(9) . . ? O3 Co1 N1 90.92(10) . . ? O4 Co1 N1 86.45(11) 2 . ? O1' Co1 N1 88.3(8) 5_656 . ? O1 Co1 O5 89.9(9) . . ? O3 Co1 O5 92.35(8) . . ? O4 Co1 O5 88.65(8) 2 . ? O1' Co1 O5 89.0(9) 5_656 . ? N1 Co1 O5 174.39(9) . . ? O1 Co1 N2 91.1(10) . 2_556 ? O3 Co1 N2 86.0(5) . 2_556 ? O4 Co1 N2 176.4(5) 2 2_556 ? O1' Co1 N2 86.5(9) 5_656 2_556 ? N1 Co1 N2 90.9(5) . 2_556 ? O5 Co1 N2 93.8(5) . 2_556 ? O1 Co1 N2' 86.4(10) . . ? O3 Co1 N2' 90.8(5) . . ? O4 Co1 N2' 172.4(5) 2 . ? O1' Co1 N2' 81.7(9) 5_656 . ? N1 Co1 N2' 95.1(6) . . ? O5 Co1 N2' 89.4(6) . . ? N2 Co1 N2' 6.5(11) 2_556 . ? C15 N1 C11 116.0(3) . . ? C15 N1 Co1 123.3(3) . . ? C11 N1 Co1 120.6(3) . . ? C10 O3 Co1 134.4(2) . . ? C10 O4 Co1 137.5(2) . 2 ? Co1 O5 Co1 115.86(13) . 2 ? Co1 O5 H5A 108.3 . . ? Co1 O5 H5A 108.3 2 . ? C6 S2 C9 92.95(18) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.036 0.250 0.709 1200 314 ' ' 2 -0.055 0.750 0.180 1200 314 ' ' _platon_squeeze_details ; 8 disordered lattice water molecules have been removed from the asymmetric unit by the SQUEEZE process. ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.353 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 939896' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Co2 N4 O8 S4' _chemical_formula_sum 'C44 H66 Co2 N4 O27 S4' _chemical_formula_weight 1329.14 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' S S 0.1246 0.1234 '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 'C 2' _symmetry_space_group_name_Hall 'C 2y' 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' _cell_length_a 21.584(2) _cell_length_b 16.6520(10) _cell_length_c 18.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.550(13) _cell_angle_gamma 90.00 _cell_volume 6376.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8409 _exptl_absorpt_correction_T_max 0.8685 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12231 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7520 _reflns_number_gt 3749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. simu .02 c21 > c32' dfix 2.43 .04 c22 c25 c21 c30 c22' c25' c21' c30' dfix 2.48 .04 c22' c29' c22' c31' dfix 2.48 .04 c21 c24 c21 c26 c21' c24' c21' c26' c22 c29 c22 c31 sadi .02 c21 c25 c21' c25' c22 c30 c22' c30' c33 c37 c34 c42 sadi .02 c21 c22 c21' c22' c33 c34 flat c22' > c32' flat c22 > c32 flat c21' > c27' flat c21 > c27 simu .02 s3 > o8 simu .02 s1 > o4 sadi .02 c1 c5 c6 c10 c11 c15 c16 c20 c4 c9 c14 c19 sadi .02 c2 c3 c7 c8 c12 c13 c17 c18 sadi .02 c1 c2 c3 c4 c6 c7 c8 c9 c11 c12 c13 c14 c16 c17 c18 c19 isor .01 c29 c31 c31' c39 c3 c13 c10 omit 0 51 ; _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^)+(0.1171P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(4) _refine_ls_number_reflns 7520 _refine_ls_number_parameters 686 _refine_ls_number_restraints 992 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2424 _refine_ls_wR_factor_gt 0.2128 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 0.995 _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 C21 C 0.3845(14) 1.071(2) 0.700(2) 0.078(6) Uani 0.38(3) 1 d PDU . 1 H21A H 0.3653 1.1222 0.6961 0.094 Uiso 0.38(3) 1 calc PR . 1 N1 N 0.2510(16) 0.887(2) 0.7143(19) 0.067(5) Uani 0.38(3) 1 d PDU . 1 C23 C 0.2333(13) 0.964(2) 0.699(2) 0.080(6) Uani 0.38(3) 1 d PDU . 1 H23A H 0.1894 0.9765 0.6902 0.096 Uiso 0.38(3) 1 calc PR . 1 C24 C 0.2746(14) 1.0253(19) 0.695(2) 0.083(6) Uani 0.38(3) 1 d PDU . 1 H24A H 0.2601 1.0789 0.6851 0.100 Uiso 0.38(3) 1 calc PR . 1 C25 C 0.3388(12) 1.0060(18) 0.7050(17) 0.079(5) Uani 0.38(3) 1 d PDU . 1 C26 C 0.3585(15) 0.927(2) 0.721(2) 0.083(6) Uani 0.38(3) 1 d PDU . 1 H26A H 0.4021 0.9130 0.7281 0.100 Uiso 0.38(3) 1 calc PR . 1 C27 C 0.3142(17) 0.8695(19) 0.726(2) 0.075(6) Uani 0.38(3) 1 d PDU . 1 H27A H 0.3279 0.8160 0.7388 0.090 Uiso 0.38(3) 1 calc PR . 1 C22 C 0.4372(13) 1.074(2) 0.700(2) 0.064(5) Uani 0.38(3) 1 d PDU . 1 H22A H 0.4525 1.0200 0.7007 0.076 Uiso 0.38(3) 1 calc PR . 1 N2 N 0.5980(13) 1.2236(18) 0.7020(15) 0.057(5) Uani 0.38(3) 1 d PDU . 1 C28 C 0.6038(12) 1.1444(19) 0.7206(17) 0.057(5) Uani 0.38(3) 1 d PDU . 1 H28A H 0.6451 1.1217 0.7352 0.068 Uiso 0.38(3) 1 calc PR . 1 C29 C 0.5523(13) 1.0967(16) 0.7190(16) 0.055(5) Uani 0.38(3) 1 d PDU . 1 H29A H 0.5583 1.0415 0.7315 0.066 Uiso 0.38(3) 1 calc PR . 1 C30 C 0.4910(11) 1.1275(16) 0.6992(15) 0.062(5) Uani 0.38(3) 1 d PDU . 1 C31 C 0.4836(12) 1.2086(16) 0.6796(18) 0.056(5) Uani 0.38(3) 1 d PDU . 1 H31A H 0.4428 1.2324 0.6644 0.067 Uiso 0.38(3) 1 calc PR . 1 C32 C 0.5379(14) 1.2522(16) 0.6833(18) 0.059(5) Uani 0.38(3) 1 d PDU . 1 H32A H 0.5331 1.3077 0.6717 0.071 Uiso 0.38(3) 1 calc PR . 1 C21' C 0.4052(9) 1.0425(15) 0.7100(14) 0.076(5) Uani 0.62(3) 1 d PDU . 2 H21B H 0.3929 1.0967 0.7148 0.091 Uiso 0.62(3) 1 calc PR . 2 N1' N 0.2488(10) 0.8856(14) 0.7134(11) 0.065(4) Uani 0.62(3) 1 d PDU . 2 C23' C 0.2465(10) 0.9655(14) 0.7239(13) 0.079(5) Uani 0.62(3) 1 d PDU . 2 H23B H 0.2078 0.9863 0.7330 0.095 Uiso 0.62(3) 1 calc PR . 2 C24' C 0.2934(11) 1.0198(13) 0.7230(13) 0.085(5) Uani 0.62(3) 1 d PDU . 2 H24B H 0.2875 1.0756 0.7304 0.102 Uiso 0.62(3) 1 calc PR . 2 C25' C 0.3507(9) 0.9893(12) 0.7106(12) 0.084(5) Uani 0.62(3) 1 d PDU . 2 C26' C 0.3548(10) 0.9058(13) 0.6999(14) 0.077(5) Uani 0.62(3) 1 d PDU . 2 H26B H 0.3932 0.8838 0.6911 0.092 Uiso 0.62(3) 1 calc PR . 2 C27' C 0.3050(11) 0.8557(13) 0.7019(14) 0.076(5) Uani 0.62(3) 1 d PDU . 2 H27B H 0.3095 0.7996 0.6953 0.091 Uiso 0.62(3) 1 calc PR . 2 C22' C 0.4565(9) 1.0405(13) 0.7058(13) 0.065(5) Uani 0.62(3) 1 d PDU . 2 H22B H 0.4723 0.9874 0.7036 0.079 Uiso 0.62(3) 1 calc PR . 2 N2' N 0.5946(8) 1.2242(12) 0.6985(9) 0.056(4) Uani 0.62(3) 1 d PDU . 2 C28' C 0.6089(8) 1.1446(12) 0.6952(11) 0.057(4) Uani 0.62(3) 1 d PDU . 2 H28B H 0.6504 1.1299 0.6907 0.068 Uiso 0.62(3) 1 calc PR . 2 C29' C 0.5659(8) 1.0855(11) 0.6983(11) 0.060(4) Uani 0.62(3) 1 d PDU . 2 H29B H 0.5784 1.0309 0.6972 0.072 Uiso 0.62(3) 1 calc PR . 2 C30' C 0.5049(8) 1.1039(10) 0.7030(10) 0.054(4) Uani 0.62(3) 1 d PDU . 2 C31' C 0.4892(8) 1.1849(11) 0.7070(11) 0.055(4) Uani 0.62(3) 1 d PDU . 2 H31B H 0.4479 1.2005 0.7118 0.066 Uiso 0.62(3) 1 calc PR . 2 C32' C 0.5344(8) 1.2413(11) 0.7037(11) 0.053(4) Uani 0.62(3) 1 d PDU . 2 H32B H 0.5229 1.2962 0.7052 0.063 Uiso 0.62(3) 1 calc PR . 2 S1 S -0.00292(14) 0.9504(2) 0.8639(2) 0.0664(9) Uani 1 1 d DU . . C1 C 0.0432(4) 0.9441(7) 0.8001(7) 0.063(3) Uani 1 1 d DU . . C2 C 0.0235(6) 0.9968(8) 0.7408(7) 0.081(4) Uani 1 1 d DU . . H2B H 0.0438 1.0025 0.6996 0.097 Uiso 1 1 calc R . . C3 C -0.0301(6) 1.0406(8) 0.7485(7) 0.078(4) Uani 1 1 d DU . . H3A H -0.0499 1.0805 0.7139 0.094 Uiso 1 1 calc R . . C4 C -0.0508(5) 1.0192(7) 0.8120(6) 0.067(3) Uani 1 1 d DU . . C5 C 0.0987(5) 0.8897(7) 0.8124(8) 0.061(3) Uani 1 1 d DU . . O1 O 0.1316(4) 0.8885(5) 0.7626(4) 0.060(2) Uani 1 1 d U . . O2 O 0.1032(3) 0.8460(5) 0.8721(5) 0.061(2) Uani 1 1 d U . . S2 S -0.15009(14) 1.1284(2) 0.7840(2) 0.0750(10) Uani 1 1 d DU . . C6 C -0.2059(5) 1.1279(7) 0.8384(6) 0.062(3) Uani 1 1 d DU . . C7 C -0.1894(6) 1.0713(9) 0.8932(8) 0.093(4) Uani 1 1 d DU . . H7A H -0.2158 1.0575 0.9268 0.111 Uiso 1 1 calc R . . C8 C -0.1301(7) 1.0351(10) 0.8962(8) 0.103(5) Uani 1 1 d DU . . H8A H -0.1092 1.0013 0.9360 0.124 Uiso 1 1 calc R . . C9 C -0.1060(6) 1.0544(8) 0.8341(8) 0.081(3) Uani 1 1 d DU . . C10 C -0.2571(4) 1.1865(7) 0.8245(8) 0.057(3) Uani 1 1 d DU . . O3 O -0.2927(3) 1.1884(5) 0.8710(5) 0.068(2) Uani 1 1 d U . . O4 O -0.2635(3) 1.2274(6) 0.7700(6) 0.070(2) Uani 1 1 d U . . S3 S 0.1932(2) 0.7635(3) 0.43770(16) 0.0843(11) Uani 1 1 d DU . . C11 C 0.1505(7) 0.8225(8) 0.4846(5) 0.091(4) Uani 1 1 d DU . . C12 C 0.1149(8) 0.8762(9) 0.4330(7) 0.105(5) Uani 1 1 d DU . . H12A H 0.0878 0.9155 0.4472 0.125 Uiso 1 1 calc R . . C13 C 0.1225(7) 0.8670(9) 0.3580(6) 0.095(4) Uani 1 1 d DU . . H13A H 0.1003 0.8973 0.3162 0.114 Uiso 1 1 calc R . . C14 C 0.1663(6) 0.8086(8) 0.3542(5) 0.076(3) Uani 1 1 d DU . . C15 C 0.1571(9) 0.8133(11) 0.5670(7) 0.092(4) Uani 1 1 d DU . . O5 O 0.1904(5) 0.7621(7) 0.6023(5) 0.084(3) Uani 1 1 d U . . O6 O 0.1235(5) 0.8626(7) 0.5994(6) 0.095(3) Uani 1 1 d U . . S4 S 0.14527(17) 0.8141(3) 0.1980(2) 0.0786(10) Uani 1 1 d DU . . C16 C 0.1936(5) 0.7604(8) 0.1539(6) 0.072(3) Uani 1 1 d DU . . C17 C 0.2394(6) 0.7218(8) 0.2068(7) 0.087(4) Uani 1 1 d DU . . H17A H 0.2703 0.6874 0.1934 0.104 Uiso 1 1 calc R . . C18 C 0.2368(6) 0.7376(8) 0.2826(7) 0.085(4) Uani 1 1 d DU . . H18A H 0.2663 0.7180 0.3254 0.102 Uiso 1 1 calc R . . C19 C 0.1849(6) 0.7859(8) 0.2851(5) 0.082(4) Uani 1 1 d DU . . C20 C 0.1849(6) 0.7611(9) 0.0732(7) 0.066(3) Uani 1 1 d DU . . O7 O 0.1457(4) 0.8094(6) 0.0356(4) 0.073(2) Uani 1 1 d U . . O8 O 0.2131(5) 0.7136(5) 0.0415(5) 0.077(2) Uani 1 1 d U . . C33 C 0.3814(6) 1.0295(8) 0.9123(9) 0.081(4) Uani 1 1 d D . . H33A H 0.3688 1.0841 0.9135 0.097 Uiso 1 1 calc R . . C34 C 0.4335(6) 1.0186(9) 0.9020(8) 0.080(4) Uani 1 1 d D . . H34A H 0.4428 0.9642 0.8927 0.096 Uiso 1 1 calc R . . C35 C 0.2298(6) 0.9334(8) 0.9364(9) 0.076(4) Uani 1 1 d . . . H35A H 0.1888 0.9495 0.9417 0.091 Uiso 1 1 calc R . . C36 C 0.2723(6) 0.9909(9) 0.9305(8) 0.077(4) Uani 1 1 d . . . H36A H 0.2608 1.0459 0.9312 0.092 Uiso 1 1 calc R . . C37 C 0.3339(6) 0.9694(8) 0.9235(9) 0.077(4) Uani 1 1 d D . . C38 C 0.3435(6) 0.8845(9) 0.9235(8) 0.079(4) Uani 1 1 d . . . H38A H 0.3833 0.8647 0.9170 0.095 Uiso 1 1 calc R . . C39 C 0.2997(5) 0.8326(8) 0.9319(7) 0.064(3) Uani 1 1 d U . . H39A H 0.3105 0.7772 0.9359 0.077 Uiso 1 1 calc R . . C40 C 0.5932(5) 1.1039(7) 0.9094(7) 0.064(3) Uani 1 1 d . . . H40A H 0.6348 1.0840 0.9115 0.076 Uiso 1 1 calc R . . C41 C 0.5471(6) 1.0510(8) 0.9014(9) 0.079(4) Uani 1 1 d . . . H41A H 0.5559 0.9957 0.8957 0.095 Uiso 1 1 calc R . . C42 C 0.4857(7) 1.0752(8) 0.9011(7) 0.071(4) Uani 1 1 d D . . C43 C 0.4769(5) 1.1577(8) 0.9030(8) 0.069(4) Uani 1 1 d . . . H43A H 0.4353 1.1786 0.8986 0.082 Uiso 1 1 calc R . . C44 C 0.5254(5) 1.2077(7) 0.9108(8) 0.068(4) Uani 1 1 d . . . H44A H 0.5172 1.2635 0.9138 0.082 Uiso 1 1 calc R . . Co1 Co 0.17295(7) 0.80461(12) 0.70670(11) 0.0682(5) Uani 1 1 d . . . Co2 Co 0.16563(7) 0.76550(11) 0.92982(11) 0.0694(5) Uani 1 1 d . . . N3 N 0.2426(4) 0.8533(6) 0.9350(6) 0.061(3) Uani 1 1 d . . . N4 N 0.5865(4) 1.1838(5) 0.9149(5) 0.047(2) 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 C21 0.069(10) 0.067(11) 0.094(10) 0.009(10) 0.010(10) -0.032(9) N1 0.057(8) 0.063(9) 0.080(9) 0.000(9) 0.014(8) -0.013(8) C23 0.065(10) 0.079(9) 0.090(11) -0.003(10) 0.006(9) -0.013(9) C24 0.071(11) 0.074(10) 0.096(12) -0.003(11) -0.002(11) -0.023(10) C25 0.072(9) 0.067(9) 0.094(9) 0.003(9) 0.012(9) -0.017(9) C26 0.072(9) 0.080(11) 0.097(11) -0.004(10) 0.014(9) -0.013(10) C27 0.065(9) 0.071(10) 0.090(11) -0.001(9) 0.017(9) -0.014(9) C22 0.051(10) 0.069(10) 0.070(9) 0.005(9) 0.010(9) -0.042(9) N2 0.069(8) 0.050(8) 0.052(8) 0.001(8) 0.013(8) -0.014(8) C28 0.059(9) 0.060(8) 0.056(10) 0.001(9) 0.023(8) -0.017(8) C29 0.060(8) 0.060(7) 0.053(8) -0.003(7) 0.028(7) -0.012(7) C30 0.063(8) 0.064(9) 0.059(8) -0.002(8) 0.017(8) -0.017(8) C31 0.048(7) 0.063(8) 0.060(8) 0.015(7) 0.019(7) -0.013(7) C32 0.065(9) 0.058(9) 0.057(10) 0.017(8) 0.019(9) -0.010(8) C21' 0.060(9) 0.074(10) 0.093(9) 0.005(8) 0.015(8) -0.049(8) N1' 0.056(7) 0.059(7) 0.078(8) -0.001(7) 0.010(7) -0.012(7) C23' 0.066(8) 0.081(8) 0.085(10) -0.011(9) 0.005(8) -0.013(8) C24' 0.078(10) 0.080(9) 0.089(10) 0.003(9) -0.004(9) -0.021(9) C25' 0.077(8) 0.075(9) 0.096(9) 0.002(8) 0.013(8) -0.022(8) C26' 0.063(8) 0.080(10) 0.094(11) -0.008(9) 0.031(8) -0.013(8) C27' 0.066(8) 0.068(9) 0.093(10) 0.000(8) 0.014(8) -0.016(8) C22' 0.051(9) 0.066(9) 0.080(8) -0.001(8) 0.014(8) -0.028(8) N2' 0.069(7) 0.047(7) 0.052(7) -0.003(6) 0.012(6) -0.009(6) C28' 0.056(7) 0.065(7) 0.057(9) -0.004(8) 0.028(7) -0.018(7) C29' 0.057(8) 0.067(8) 0.064(9) -0.014(8) 0.030(7) -0.012(7) C30' 0.065(8) 0.054(8) 0.045(7) -0.011(7) 0.017(7) -0.018(7) C31' 0.042(6) 0.063(7) 0.063(7) 0.011(6) 0.020(5) -0.017(6) C32' 0.048(7) 0.069(8) 0.048(8) 0.016(7) 0.025(6) -0.007(7) S1 0.0569(18) 0.0570(18) 0.093(2) 0.0216(17) 0.0322(16) 0.0222(15) C1 0.032(5) 0.052(6) 0.115(8) -0.001(6) 0.034(5) 0.006(5) C2 0.091(8) 0.091(9) 0.070(8) 0.030(7) 0.037(7) 0.022(7) C3 0.083(6) 0.079(6) 0.071(6) 0.019(5) 0.014(5) 0.052(6) C4 0.075(6) 0.065(6) 0.066(6) 0.020(6) 0.029(5) 0.037(6) C5 0.064(6) 0.048(6) 0.074(7) 0.005(6) 0.022(6) -0.003(5) O1 0.072(5) 0.058(5) 0.061(5) -0.001(4) 0.035(4) 0.014(4) O2 0.033(4) 0.065(5) 0.088(6) 0.001(5) 0.018(4) 0.007(4) S2 0.0573(19) 0.064(2) 0.111(3) 0.0240(19) 0.0355(18) 0.0358(17) C6 0.065(6) 0.063(7) 0.068(7) 0.013(6) 0.038(6) 0.023(6) C7 0.086(8) 0.084(9) 0.119(10) 0.025(8) 0.046(8) 0.042(7) C8 0.103(9) 0.104(10) 0.116(10) 0.021(9) 0.052(8) 0.055(8) C9 0.074(7) 0.074(7) 0.101(8) 0.018(7) 0.036(6) 0.020(6) C10 0.023(4) 0.061(5) 0.093(6) 0.010(5) 0.023(4) -0.007(4) O3 0.020(3) 0.042(4) 0.148(8) -0.002(5) 0.027(4) -0.001(3) O4 0.035(4) 0.074(6) 0.103(7) 0.008(5) 0.021(4) 0.015(4) S3 0.138(3) 0.096(2) 0.0242(12) -0.0014(18) 0.0291(16) -0.008(3) C11 0.163(9) 0.097(8) 0.025(5) -0.009(6) 0.044(6) -0.015(8) C12 0.163(11) 0.099(10) 0.053(7) 0.013(7) 0.027(8) -0.003(9) C13 0.135(8) 0.099(7) 0.052(6) 0.024(6) 0.026(6) 0.004(7) C14 0.098(7) 0.091(8) 0.049(6) -0.017(6) 0.037(5) -0.013(7) C15 0.135(10) 0.081(9) 0.064(7) 0.014(7) 0.029(7) -0.015(8) O5 0.141(8) 0.068(6) 0.049(5) 0.004(5) 0.033(5) 0.001(6) O6 0.115(8) 0.102(8) 0.073(6) -0.021(6) 0.029(5) -0.029(7) S4 0.079(2) 0.086(3) 0.072(2) -0.002(2) 0.0200(17) 0.001(2) C16 0.083(8) 0.055(6) 0.080(8) -0.005(7) 0.023(6) -0.011(7) C17 0.083(8) 0.077(8) 0.100(9) 0.000(7) 0.018(7) 0.001(7) C18 0.106(9) 0.087(9) 0.058(7) 0.010(7) 0.009(7) -0.011(8) C19 0.106(8) 0.083(8) 0.063(7) -0.016(6) 0.033(6) -0.012(7) C20 0.065(7) 0.053(6) 0.081(7) -0.001(7) 0.019(6) -0.019(6) O7 0.087(6) 0.088(6) 0.046(5) 0.008(5) 0.020(4) -0.015(6) O8 0.098(6) 0.053(5) 0.083(6) 0.001(5) 0.025(5) 0.004(5) C33 0.064(9) 0.054(8) 0.126(13) -0.002(8) 0.023(8) -0.020(7) C34 0.073(9) 0.089(11) 0.076(9) -0.025(8) 0.012(8) -0.016(8) C35 0.051(7) 0.060(8) 0.125(12) -0.032(8) 0.036(7) -0.031(6) C36 0.072(9) 0.060(8) 0.103(11) -0.008(8) 0.026(8) -0.013(7) C37 0.065(9) 0.066(9) 0.099(11) -0.007(8) 0.019(7) 0.000(7) C38 0.058(8) 0.091(11) 0.091(10) 0.008(8) 0.023(7) 0.005(8) C39 0.034(5) 0.062(6) 0.097(7) -0.006(6) 0.017(5) -0.019(5) C40 0.046(6) 0.058(7) 0.092(9) 0.005(7) 0.027(6) -0.023(6) C41 0.056(8) 0.054(7) 0.136(13) -0.018(8) 0.042(8) -0.008(6) C42 0.096(10) 0.054(7) 0.064(8) -0.004(6) 0.018(7) -0.019(7) C43 0.038(6) 0.075(9) 0.098(10) -0.001(7) 0.026(6) -0.014(6) C44 0.050(7) 0.044(6) 0.114(11) 0.003(7) 0.026(7) 0.003(6) Co1 0.0580(10) 0.0516(9) 0.0989(14) 0.0027(10) 0.0258(9) -0.0030(8) Co2 0.0554(10) 0.0499(9) 0.1083(14) -0.0007(10) 0.0296(9) -0.0032(8) N3 0.036(5) 0.047(6) 0.100(8) -0.004(5) 0.016(5) -0.020(4) N4 0.055(5) 0.041(5) 0.046(5) -0.003(4) 0.011(4) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C21 C22 1.140(18) . ? C21 C25 1.474(15) . ? C21 H21A 0.9500 . ? N1 C23 1.353(15) . ? N1 C27 1.365(15) . ? N1 Co1 2.15(3) . ? C23 C24 1.366(16) . ? C23 H23A 0.9500 . ? C24 C25 1.395(15) . ? C24 H24A 0.9500 . ? C25 C26 1.396(15) . ? C26 C27 1.371(16) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C22 C30 1.470(15) . ? C22 H22A 0.9500 . ? N2 C32 1.352(15) . ? N2 C28 1.361(15) . ? N2 Co1 2.09(2) 3 ? C28 C29 1.360(16) . ? C28 H28A 0.9500 . ? C29 C30 1.392(15) . ? C29 H29A 0.9500 . ? C30 C31 1.398(15) . ? C31 C32 1.369(16) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C21' C22' 1.129(16) . ? C21' C25' 1.474(13) . ? C21' H21B 0.9500 . ? N1' C23' 1.348(14) . ? N1' C27' 1.370(14) . ? N1' Co1 2.103(18) . ? C23' C24' 1.360(15) . ? C23' H23B 0.9500 . ? C24' C25' 1.400(14) . ? C24' H24B 0.9500 . ? C25' C26' 1.410(14) . ? C26' C27' 1.367(15) . ? C26' H26B 0.9500 . ? C27' H27B 0.9500 . ? C22' C30' 1.493(13) . ? C22' H22B 0.9500 . ? N2' C32' 1.354(13) . ? N2' C28' 1.364(14) . ? N2' Co1 2.137(17) 3 ? C28' C29' 1.361(14) . ? C28' H28B 0.9500 . ? C29' C30' 1.374(13) . ? C29' H29B 0.9500 . ? C30' C31' 1.397(14) . ? C31' C32' 1.365(14) . ? C31' H31B 0.9500 . ? C32' H32B 0.9500 . ? S1 C4 1.687(9) . ? S1 C1 1.688(9) . ? C1 C2 1.384(11) . ? C1 C5 1.479(11) . ? C2 C3 1.401(12) . ? C2 H2B 0.9500 . ? C3 C4 1.371(11) . ? C3 H3A 0.9500 . ? C4 C9 1.463(10) . ? C5 O1 1.267(14) . ? C5 O2 1.292(14) . ? O1 Co1 2.042(7) . ? O2 Co2 2.025(8) . ? S2 C9 1.696(10) . ? S2 C6 1.717(9) . ? C6 C7 1.361(12) . ? C6 C10 1.455(11) . ? C7 C8 1.405(12) . ? C7 H7A 0.9500 . ? C8 C9 1.378(12) . ? C8 H8A 0.9500 . ? C10 O4 1.185(14) . ? C10 O3 1.259(13) . ? O3 Co2 2.005(8) 3_455 ? O4 Co1 2.044(9) 3_455 ? S3 C14 1.680(10) . ? S3 C11 1.697(10) . ? C11 C12 1.399(12) . ? C11 C15 1.481(12) . ? C12 C13 1.417(13) . ? C12 H12A 0.9500 . ? C13 C14 1.368(12) . ? C13 H13A 0.9500 . ? C14 C19 1.450(11) . ? C15 O5 1.206(18) . ? C15 O6 1.316(19) . ? C15 Co1 2.492(12) . ? O5 Co1 2.133(9) . ? O6 Co1 2.230(11) . ? S4 C19 1.694(10) . ? S4 C16 1.702(10) . ? C16 C17 1.378(12) . ? C16 C20 1.437(12) . ? C17 C18 1.415(13) . ? C17 H17A 0.9500 . ? C18 C19 1.389(12) . ? C18 H18A 0.9500 . ? C20 O8 1.217(15) . ? C20 O7 1.257(15) . ? O7 Co2 2.185(8) 1_554 ? O8 Co2 2.239(10) 1_554 ? C33 C34 1.193(13) . ? C33 C37 1.478(12) . ? C33 H33A 0.9500 . ? C34 C42 1.471(13) . ? C34 H34A 0.9500 . ? C35 C36 1.345(16) . ? C35 N3 1.365(15) . ? C35 H35A 0.9500 . ? C36 C37 1.410(17) . ? C36 H36A 0.9500 . ? C37 C38 1.429(19) . ? C38 C39 1.315(17) . ? C38 H38A 0.9500 . ? C39 N3 1.293(13) . ? C39 H39A 0.9500 . ? C40 C41 1.312(15) . ? C40 N4 1.345(14) . ? C40 H40A 0.9500 . ? C41 C42 1.384(17) . ? C41 H41A 0.9500 . ? C42 C43 1.389(18) . ? C43 C44 1.319(15) . ? C43 H43A 0.9500 . ? C44 N4 1.364(13) . ? C44 H44A 0.9500 . ? Co1 O4 2.044(9) 3_545 ? Co1 N2 2.09(2) 3_445 ? Co1 N2' 2.137(17) 3_445 ? Co2 O3 2.005(8) 3_545 ? Co2 N4 2.155(9) 3_445 ? Co2 O7 2.185(8) 1_556 ? Co2 N3 2.199(8) . ? Co2 O8 2.239(10) 1_556 ? N4 Co2 2.155(8) 3 ? 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 C22 C21 C25 135(3) . . ? C22 C21 H21A 112.3 . . ? C25 C21 H21A 112.3 . . ? C23 N1 C27 117.5(18) . . ? C23 N1 Co1 114(2) . . ? C27 N1 Co1 128(2) . . ? N1 C23 C24 124.2(19) . . ? N1 C23 H23A 117.9 . . ? C24 C23 H23A 117.9 . . ? C23 C24 C25 117.5(17) . . ? C23 C24 H24A 121.2 . . ? C25 C24 H24A 121.2 . . ? C24 C25 C26 119.6(17) . . ? C24 C25 C21 118.8(19) . . ? C26 C25 C21 122(2) . . ? C27 C26 C25 119.2(18) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? N1 C27 C26 121.9(19) . . ? N1 C27 H27A 119.1 . . ? C26 C27 H27A 119.0 . . ? C21 C22 C30 145(3) . . ? C21 C22 H22A 107.6 . . ? C30 C22 H22A 107.6 . . ? C32 N2 C28 115.8(18) . . ? C32 N2 Co1 118.3(19) . 3 ? C28 N2 Co1 125.8(19) . 3 ? C29 C28 N2 121.9(18) . . ? C29 C28 H28A 119.0 . . ? N2 C28 H28A 119.0 . . ? C28 C29 C30 121.2(17) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C30 C31 118.1(16) . . ? C29 C30 C22 118.8(18) . . ? C31 C30 C22 123.1(18) . . ? C32 C31 C30 116.7(17) . . ? C32 C31 H31A 121.6 . . ? C30 C31 H31A 121.6 . . ? N2 C32 C31 126.2(18) . . ? N2 C32 H32A 116.9 . . ? C31 C32 H32A 116.9 . . ? C22' C21' C25' 141(2) . . ? C22' C21' H21B 109.4 . . ? C25' C21' H21B 109.4 . . ? C23' N1' C27' 116.2(15) . . ? C23' N1' Co1 126.1(16) . . ? C27' N1' Co1 117.6(14) . . ? N1' C23' C24' 127.2(16) . . ? N1' C23' H23B 116.4 . . ? C24' C23' H23B 116.4 . . ? C23' C24' C25' 116.5(15) . . ? C23' C24' H24B 121.7 . . ? C25' C24' H24B 121.7 . . ? C24' C25' C26' 117.7(14) . . ? C24' C25' C21' 121.1(16) . . ? C26' C25' C21' 121.1(16) . . ? C27' C26' C25' 121.6(15) . . ? C27' C26' H26B 119.2 . . ? C25' C26' H26B 119.2 . . ? C26' C27' N1' 120.7(15) . . ? C26' C27' H27B 119.6 . . ? N1' C27' H27B 119.6 . . ? C21' C22' C30' 133(2) . . ? C21' C22' H22B 113.4 . . ? C30' C22' H22B 113.4 . . ? C32' N2' C28' 115.9(14) . . ? C32' N2' Co1 128.3(13) . 3 ? C28' N2' Co1 115.4(12) . 3 ? C29' C28' N2' 122.6(14) . . ? C29' C28' H28B 118.7 . . ? N2' C28' H28B 118.7 . . ? C28' C29' C30' 120.8(14) . . ? C28' C29' H29B 119.6 . . ? C30' C29' H29B 119.6 . . ? C29' C30' C31' 117.7(13) . . ? C29' C30' C22' 122.1(14) . . ? C31' C30' C22' 120.2(13) . . ? C32' C31' C30' 118.5(13) . . ? C32' C31' H31B 120.7 . . ? C30' C31' H31B 120.7 . . ? N2' C32' C31' 124.4(15) . . ? N2' C32' H32B 117.8 . . ? C31' C32' H32B 117.8 . . ? C4 S1 C1 92.2(5) . . ? C2 C1 C5 127.5(10) . . ? C2 C1 S1 111.6(7) . . ? C5 C1 S1 120.9(9) . . ? C1 C2 C3 111.9(9) . . ? C1 C2 H2B 124.0 . . ? C3 C2 H2B 124.0 . . ? C4 C3 C2 112.1(9) . . ? C4 C3 H3A 124.0 . . ? C2 C3 H3A 124.0 . . ? C3 C4 C9 124.1(9) . . ? C3 C4 S1 112.1(7) . . ? C9 C4 S1 123.7(8) . . ? O1 C5 O2 129.8(10) . . ? O1 C5 C1 117.6(10) . . ? O2 C5 C1 112.4(10) . . ? C5 O1 Co1 137.8(8) . . ? C5 O2 Co2 136.7(7) . . ? C9 S2 C6 93.9(5) . . ? C7 C6 C10 131.3(10) . . ? C7 C6 S2 108.6(7) . . ? C10 C6 S2 119.9(8) . . ? C6 C7 C8 114.7(10) . . ? C6 C7 H7A 122.7 . . ? C8 C7 H7A 122.7 . . ? C9 C8 C7 111.7(10) . . ? C9 C8 H8A 124.1 . . ? C7 C8 H8A 124.1 . . ? C8 C9 C4 127.3(10) . . ? C8 C9 S2 110.1(8) . . ? C4 C9 S2 122.6(8) . . ? O4 C10 O3 124.7(10) . . ? O4 C10 C6 118.4(10) . . ? O3 C10 C6 116.8(11) . . ? C10 O3 Co2 141.6(8) . 3_455 ? C10 O4 Co1 140.7(7) . 3_455 ? C14 S3 C11 94.4(6) . . ? C12 C11 C15 131.4(12) . . ? C12 C11 S3 108.2(7) . . ? C15 C11 S3 120.3(11) . . ? C11 C12 C13 114.4(10) . . ? C11 C12 H12A 122.8 . . ? C13 C12 H12A 122.8 . . ? C14 C13 C12 110.6(10) . . ? C14 C13 H13A 124.7 . . ? C12 C13 H13A 124.7 . . ? C13 C14 C19 123.6(10) . . ? C13 C14 S3 112.2(7) . . ? C19 C14 S3 124.1(9) . . ? O5 C15 O6 121.6(12) . . ? O5 C15 C11 121.8(16) . . ? O6 C15 C11 116.6(14) . . ? O5 C15 Co1 58.8(7) . . ? O6 C15 Co1 63.1(7) . . ? C11 C15 Co1 176.5(12) . . ? C15 O5 Co1 92.3(9) . . ? C15 O6 Co1 85.2(9) . . ? C19 S4 C16 93.3(6) . . ? C17 C16 C20 129.1(11) . . ? C17 C16 S4 109.6(8) . . ? C20 C16 S4 121.3(9) . . ? C16 C17 C18 114.8(10) . . ? C16 C17 H17A 122.6 . . ? C18 C17 H17A 122.6 . . ? C19 C18 C17 109.9(9) . . ? C19 C18 H18A 125.0 . . ? C17 C18 H18A 125.0 . . ? C18 C19 C14 123.8(10) . . ? C18 C19 S4 112.2(7) . . ? C14 C19 S4 124.0(9) . . ? O8 C20 O7 120.3(11) . . ? O8 C20 C16 120.7(13) . . ? O7 C20 C16 118.9(12) . . ? C20 O7 Co2 91.5(8) . 1_554 ? C20 O8 Co2 90.1(8) . 1_554 ? C34 C33 C37 128.6(14) . . ? C34 C33 H33A 115.7 . . ? C37 C33 H33A 115.7 . . ? C33 C34 C42 130.8(15) . . ? C33 C34 H34A 114.6 . . ? C42 C34 H34A 114.6 . . ? C36 C35 N3 123.4(12) . . ? C36 C35 H35A 118.3 . . ? N3 C35 H35A 118.3 . . ? C35 C36 C37 120.0(13) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 113.0(12) . . ? C36 C37 C33 122.5(13) . . ? C38 C37 C33 124.4(12) . . ? C39 C38 C37 122.8(12) . . ? C39 C38 H38A 118.6 . . ? C37 C38 H38A 118.6 . . ? N3 C39 C38 123.2(13) . . ? N3 C39 H39A 118.4 . . ? C38 C39 H39A 118.4 . . ? C41 C40 N4 125.5(12) . . ? C41 C40 H40A 117.2 . . ? N4 C40 H40A 117.2 . . ? C40 C41 C42 120.5(12) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? C41 C42 C43 115.0(11) . . ? C41 C42 C34 123.3(12) . . ? C43 C42 C34 121.7(13) . . ? C44 C43 C42 121.2(12) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C43 C44 N4 123.8(11) . . ? C43 C44 H44A 118.1 . . ? N4 C44 H44A 118.1 . . ? O1 Co1 O4 117.6(4) . 3_545 ? O1 Co1 N2 92.5(9) . 3_445 ? O4 Co1 N2 92.1(9) 3_545 3_445 ? O1 Co1 N1' 87.2(7) . . ? O4 Co1 N1' 87.3(7) 3_545 . ? N2 Co1 N1' 179.0(9) 3_445 . ? O1 Co1 O5 148.1(4) . . ? O4 Co1 O5 93.8(4) 3_545 . ? N2 Co1 O5 92.0(8) 3_445 . ? N1' Co1 O5 88.8(7) . . ? O1 Co1 N2' 92.2(6) . 3_445 ? O4 Co1 N2' 94.0(6) 3_545 3_445 ? N2 Co1 N2' 2.0(12) 3_445 3_445 ? N1' Co1 N2' 178.8(8) . 3_445 ? O5 Co1 N2' 91.1(6) . 3_445 ? O1 Co1 N1 87.3(11) . . ? O4 Co1 N1 86.8(11) 3_545 . ? N2 Co1 N1 178.6(12) 3_445 . ? N1' Co1 N1 0.5(15) . . ? O5 Co1 N1 88.9(10) . . ? N2' Co1 N1 179.2(12) 3_445 . ? O1 Co1 O6 87.8(4) . . ? O4 Co1 O6 154.3(4) 3_545 . ? N2 Co1 O6 91.4(8) 3_445 . ? N1' Co1 O6 89.5(6) . . ? O5 Co1 O6 60.6(4) . . ? N2' Co1 O6 89.4(5) 3_445 . ? N1 Co1 O6 90.0(10) . . ? O1 Co1 C15 119.3(5) . . ? O4 Co1 C15 122.5(5) 3_545 . ? N2 Co1 C15 93.6(8) 3_445 . ? N1' Co1 C15 87.4(7) . . ? O5 Co1 C15 28.9(5) . . ? N2' Co1 C15 91.9(6) 3_445 . ? N1 Co1 C15 87.8(10) . . ? O6 Co1 C15 31.8(5) . . ? O3 Co2 O2 118.2(4) 3_545 . ? O3 Co2 N4 88.0(3) 3_545 3_445 ? O2 Co2 N4 86.1(3) . 3_445 ? O3 Co2 O7 151.7(4) 3_545 1_556 ? O2 Co2 O7 89.9(4) . 1_556 ? N4 Co2 O7 91.1(3) 3_445 1_556 ? O3 Co2 N3 91.5(3) 3_545 . ? O2 Co2 N3 89.7(3) . . ? N4 Co2 N3 174.9(4) 3_445 . ? O7 Co2 N3 91.8(4) 1_556 . ? O3 Co2 O8 93.8(4) 3_545 1_556 ? O2 Co2 O8 147.9(4) . 1_556 ? N4 Co2 O8 93.7(3) 3_445 1_556 ? O7 Co2 O8 58.0(3) 1_556 1_556 ? N3 Co2 O8 91.4(4) . 1_556 ? C39 N3 C35 117.4(10) . . ? C39 N3 Co2 122.7(8) . . ? C35 N3 Co2 119.8(7) . . ? C40 N4 C44 113.7(10) . . ? C40 N4 Co2 122.6(8) . 3 ? C44 N4 Co2 123.6(8) . 3 ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.330 -0.051 0.400 2656 756 ' ' _platon_squeeze_details ; 19 disordered lattice water molecules have been removed from the asymmetric unit by the SQUEEZE process. ; _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.153 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.093 #End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 939897'