# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Lili Hou' _publ_contact_author_email houlilibhu@163.com loop_ _publ_author_name 'Xiuli Wang' 'Lili Hou' 'Juwen Zhang' 'Jin-Xia Zhang' 'Guocheng Liu' 'Song Yang' #===END data_hll-4 _database_code_depnum_ccdc_archive 'CCDC 796592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H21 Cd N5 O6' _chemical_formula_sum 'C26 H21 Cd N5 O6' _chemical_formula_weight 611.88 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number No.14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.960(4) _cell_length_b 13.429(6) _cell_length_c 19.779(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.794(17) _cell_angle_gamma 90.00 _cell_volume 2456.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6416 _cell_measurement_theta_min 2.2178 _cell_measurement_theta_max 28.1401 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7502 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3869 _reflns_number_gt 3465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.1272P)^2^+3.2911P] 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 3869 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _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 Cd1 Cd 0.46168(3) 0.58759(3) 0.102532(17) 0.0271(2) Uani 1 1 d . . . N1 N 0.2322(5) 0.5935(3) 0.0175(3) 0.0340(12) Uani 1 1 d . . . C1 C 0.1105(5) 0.6513(4) 0.0105(3) 0.0304(11) Uani 1 1 d . . . O1 O 0.4106(5) 0.7072(3) 0.1888(2) 0.0471(10) Uani 1 1 d . . . N2 N 0.0482(4) 0.5419(4) -0.0801(2) 0.0318(10) Uani 1 1 d . . . C2 C 0.0944(6) 0.7307(5) 0.0533(3) 0.0393(13) Uani 1 1 d . . . H2A H 0.1707 0.7523 0.0944 0.047 Uiso 1 1 calc R . . O2 O 0.3890(4) 0.5440(4) 0.2007(2) 0.0437(10) Uani 1 1 d . . . O3 O 0.5380(4) 0.8560(3) 0.51214(19) 0.0401(10) Uani 1 1 d . . . N3 N -0.0982(4) 0.7851(3) -0.2730(2) 0.0328(10) Uani 1 1 d . . . C3 C -0.0402(7) 0.7751(5) 0.0312(3) 0.0449(14) Uani 1 1 d . . . H3A H -0.0533 0.8292 0.0574 0.054 Uiso 1 1 calc R . . N4 N -0.3071(5) 0.8705(4) -0.3213(2) 0.0324(10) Uani 1 1 d . . . C4 C -0.1582(6) 0.7415(5) -0.0297(3) 0.0458(15) Uani 1 1 d . . . H4A H -0.2476 0.7726 -0.0420 0.055 Uiso 1 1 calc R . . O4 O 0.4794(6) 0.9263(3) 0.4023(3) 0.0501(12) Uani 1 1 d . . . O5 O 0.3286(6) 0.5151(4) 0.5062(3) 0.0636(14) Uani 1 1 d . . . N5 N 0.3281(6) 0.5004(4) 0.4448(3) 0.0466(13) Uani 1 1 d . . . C5 C -0.1427(6) 0.6620(5) -0.0717(3) 0.0399(13) Uani 1 1 d . . . H5A H -0.2198 0.6389 -0.1119 0.048 Uiso 1 1 calc R . . O6 O 0.2921(8) 0.4218(4) 0.4127(4) 0.0717(18) Uani 1 1 d . . . C6 C -0.0060(6) 0.6193(4) -0.0504(3) 0.0301(11) Uani 1 1 d . . . C7 C 0.1899(5) 0.5306(4) -0.0380(3) 0.0309(11) Uani 1 1 d . . . H7A H 0.2503 0.4840 -0.0469 0.037 Uiso 1 1 calc R . . C8 C -0.0243(6) 0.4957(4) -0.1524(3) 0.0399(14) Uani 1 1 d . . . H8A H -0.1130 0.4640 -0.1541 0.048 Uiso 1 1 calc R . . H8B H 0.0379 0.4445 -0.1596 0.048 Uiso 1 1 calc R . . C9 C -0.0602(7) 0.5728(5) -0.2147(3) 0.0382(14) Uani 1 1 d . . . H9A H -0.0882 0.5374 -0.2607 0.046 Uiso 1 1 calc R . . H9B H -0.1426 0.6120 -0.2156 0.046 Uiso 1 1 calc R . . C10 C 0.0618(6) 0.6420(4) -0.2087(3) 0.0359(12) Uani 1 1 d . . . H10A H 0.1438 0.6033 -0.2091 0.043 Uiso 1 1 calc R . . H10B H 0.0912 0.6769 -0.1625 0.043 Uiso 1 1 calc R . . C11 C 0.0210(6) 0.7185(5) -0.2707(3) 0.0427(14) Uani 1 1 d . . . H11A H 0.1054 0.7586 -0.2653 0.051 Uiso 1 1 calc R . . H11B H -0.0065 0.6834 -0.3167 0.051 Uiso 1 1 calc R . . C12 C -0.1015(5) 0.8533(4) -0.2197(3) 0.0312(12) Uani 1 1 d . . . C13 C -0.0033(6) 0.8746(5) -0.1495(3) 0.0431(14) Uani 1 1 d . . . H13A H 0.0844 0.8412 -0.1296 0.052 Uiso 1 1 calc R . . C14 C -0.0422(8) 0.9472(6) -0.1113(3) 0.0551(18) Uani 1 1 d . . . H14A H 0.0202 0.9620 -0.0641 0.066 Uiso 1 1 calc R . . C15 C -0.1720(7) 0.9994(5) -0.1409(3) 0.0520(17) Uani 1 1 d . . . H15A H -0.1943 1.0477 -0.1131 0.062 Uiso 1 1 calc R . . C16 C -0.2692(7) 0.9807(5) -0.2115(3) 0.0425(14) Uani 1 1 d . . . H16A H -0.3551 1.0162 -0.2318 0.051 Uiso 1 1 calc R . . C17 C -0.2313(6) 0.9057(4) -0.2505(3) 0.0341(13) Uani 1 1 d . . . C18 C -0.2246(5) 0.7999(4) -0.3317(3) 0.0335(12) Uani 1 1 d . . . H18A H -0.2497 0.7635 -0.3747 0.040 Uiso 1 1 calc R . . C19 C 0.3990(5) 0.6322(5) 0.2246(3) 0.0363(14) Uani 1 1 d . . . C20 C 0.3994(5) 0.6476(4) 0.3002(3) 0.0322(12) Uani 1 1 d . . . C21 C 0.4335(6) 0.7401(4) 0.3344(3) 0.0324(12) Uani 1 1 d . . . H21A H 0.4514 0.7937 0.3092 0.039 Uiso 1 1 calc R . . C22 C 0.4413(5) 0.7539(4) 0.4065(2) 0.0280(11) Uani 1 1 d . . . C23 C 0.4107(5) 0.6754(4) 0.4433(3) 0.0309(11) Uani 1 1 d . . . H23A H 0.4155 0.6829 0.4909 0.037 Uiso 1 1 calc R . . C24 C 0.3724(6) 0.5846(4) 0.4074(3) 0.0326(13) Uani 1 1 d . . . C25 C 0.3685(6) 0.5691(4) 0.3377(3) 0.0338(12) Uani 1 1 d . . . H25A H 0.3455 0.5067 0.3161 0.041 Uiso 1 1 calc R . . C27 C 0.4904(5) 0.8547(4) 0.4429(3) 0.0295(11) 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 Cd1 0.0284(3) 0.0308(4) 0.0196(3) -0.00069(11) 0.0058(2) 0.00088(12) N1 0.029(2) 0.041(3) 0.026(2) 0.0012(17) 0.0040(19) 0.0065(17) C1 0.030(2) 0.039(3) 0.023(2) 0.003(2) 0.0101(19) 0.002(2) O1 0.059(3) 0.054(3) 0.0269(19) -0.0009(18) 0.0143(18) 0.004(2) N2 0.033(2) 0.034(3) 0.024(2) 0.0018(19) 0.0064(16) -0.0025(18) C2 0.043(3) 0.046(4) 0.027(2) -0.005(2) 0.011(2) 0.005(2) O2 0.047(2) 0.051(3) 0.035(2) -0.018(2) 0.0176(18) -0.0055(19) O3 0.041(2) 0.051(3) 0.0272(18) -0.0139(17) 0.0117(16) -0.0005(18) N3 0.030(2) 0.036(3) 0.028(2) 0.0057(18) 0.0063(17) 0.0039(18) C3 0.054(3) 0.049(4) 0.038(3) -0.001(3) 0.024(3) 0.009(3) N4 0.032(2) 0.035(3) 0.026(2) -0.0001(19) 0.0061(17) 0.0030(19) C4 0.035(3) 0.053(4) 0.051(3) 0.001(3) 0.016(3) 0.009(3) O4 0.071(3) 0.032(3) 0.046(3) -0.0004(18) 0.021(2) -0.008(2) O5 0.080(3) 0.065(3) 0.051(3) 0.010(2) 0.031(2) -0.017(3) N5 0.045(3) 0.042(4) 0.048(3) 0.006(2) 0.013(2) -0.008(2) C5 0.029(2) 0.053(4) 0.036(3) 0.002(3) 0.009(2) 0.001(2) O6 0.106(5) 0.042(4) 0.071(4) -0.004(2) 0.036(4) -0.025(3) C6 0.035(3) 0.027(3) 0.029(2) 0.003(2) 0.012(2) 0.001(2) C7 0.033(2) 0.030(3) 0.027(2) 0.001(2) 0.009(2) 0.003(2) C8 0.044(3) 0.037(4) 0.030(3) -0.004(2) 0.002(2) -0.003(2) C9 0.041(3) 0.042(4) 0.023(3) -0.003(2) 0.002(2) -0.001(2) C10 0.032(3) 0.043(4) 0.033(3) 0.006(2) 0.011(2) 0.008(2) C11 0.036(3) 0.053(4) 0.039(3) 0.010(3) 0.015(2) 0.009(3) C12 0.030(2) 0.034(3) 0.028(2) 0.002(2) 0.009(2) -0.007(2) C13 0.043(3) 0.049(4) 0.029(3) 0.002(3) 0.003(2) -0.005(3) C14 0.061(4) 0.059(4) 0.033(3) -0.007(3) 0.002(3) -0.020(3) C15 0.061(4) 0.054(4) 0.043(3) -0.019(3) 0.023(3) -0.017(3) C16 0.049(3) 0.036(4) 0.044(3) -0.008(3) 0.018(3) -0.001(3) C17 0.033(3) 0.037(4) 0.029(3) 0.002(2) 0.007(2) -0.004(2) C18 0.035(3) 0.034(3) 0.024(2) 0.004(2) 0.003(2) -0.002(2) C19 0.025(2) 0.054(4) 0.028(3) -0.009(3) 0.007(2) 0.006(2) C20 0.025(2) 0.042(3) 0.025(2) -0.008(2) 0.0051(19) 0.006(2) C21 0.034(2) 0.036(3) 0.024(2) 0.002(2) 0.0075(19) -0.004(2) C22 0.027(2) 0.032(3) 0.023(2) -0.0030(19) 0.0063(18) 0.0009(19) C23 0.032(2) 0.038(3) 0.022(2) 0.000(2) 0.0094(19) 0.002(2) C24 0.028(3) 0.034(4) 0.031(3) 0.0042(19) 0.006(2) -0.0042(18) C25 0.031(3) 0.030(3) 0.034(3) -0.007(2) 0.005(2) 0.002(2) C27 0.029(2) 0.028(3) 0.034(3) -0.002(2) 0.013(2) 0.0004(19) _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 Cd1 O4 2.255(4) 2_645 ? Cd1 N1 2.281(5) . ? Cd1 N4 2.305(4) 4_676 ? Cd1 O3 2.315(4) 4_575 ? Cd1 O2 2.383(4) . ? Cd1 O1 2.529(4) . ? N1 C7 1.323(7) . ? N1 C1 1.402(7) . ? C1 C6 1.394(7) . ? C1 C2 1.406(8) . ? O1 C19 1.261(8) . ? N2 C7 1.355(6) . ? N2 C6 1.398(8) . ? N2 C8 1.478(6) . ? C2 C3 1.382(8) . ? C2 H2A 0.9300 . ? O2 C19 1.266(8) . ? O3 C27 1.272(6) . ? O3 Cd1 2.315(4) 4_576 ? N3 C18 1.374(6) . ? N3 C12 1.407(7) . ? N3 C11 1.473(7) . ? C3 C4 1.408(9) . ? C3 H3A 0.9300 . ? N4 C18 1.320(7) . ? N4 C17 1.404(7) . ? N4 Cd1 2.305(4) 4_475 ? C4 C5 1.396(9) . ? C4 H4A 0.9300 . ? O4 C27 1.232(7) . ? O4 Cd1 2.255(4) 2_655 ? O5 N5 1.229(7) . ? N5 O6 1.214(7) . ? N5 C24 1.505(8) . ? C5 C6 1.391(8) . ? C5 H5A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.546(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.499(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.534(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.397(8) . ? C12 C13 1.399(7) . ? C13 C14 1.374(11) . ? C13 H13A 0.9300 . ? C14 C15 1.394(11) . ? C14 H14A 0.9300 . ? C15 C16 1.395(8) . ? C15 H15A 0.9300 . ? C16 C17 1.403(9) . ? C16 H16A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.508(7) . ? C20 C25 1.387(9) . ? C20 C21 1.394(8) . ? C21 C22 1.410(7) . ? C21 H21A 0.9300 . ? C22 C23 1.378(8) . ? C22 C27 1.527(7) . ? C23 C24 1.392(8) . ? C23 H23A 0.9300 . ? C24 C25 1.380(8) . ? C25 H25A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 N1 101.97(17) 2_645 . ? O4 Cd1 N4 92.86(18) 2_645 4_676 ? N1 Cd1 N4 163.25(17) . 4_676 ? O4 Cd1 O3 96.70(17) 2_645 4_575 ? N1 Cd1 O3 86.88(16) . 4_575 ? N4 Cd1 O3 83.66(15) 4_676 4_575 ? O4 Cd1 O2 87.77(17) 2_645 . ? N1 Cd1 O2 94.88(17) . . ? N4 Cd1 O2 93.43(15) 4_676 . ? O3 Cd1 O2 174.77(14) 4_575 . ? O4 Cd1 O1 139.38(16) 2_645 . ? N1 Cd1 O1 94.48(15) . . ? N4 Cd1 O1 78.84(16) 4_676 . ? O3 Cd1 O1 121.29(15) 4_575 . ? O2 Cd1 O1 53.70(15) . . ? C7 N1 C1 105.9(4) . . ? C7 N1 Cd1 120.9(4) . . ? C1 N1 Cd1 133.2(4) . . ? C6 C1 N1 109.0(5) . . ? C6 C1 C2 120.6(5) . . ? N1 C1 C2 130.4(5) . . ? C19 O1 Cd1 87.5(3) . . ? C7 N2 C6 107.5(4) . . ? C7 N2 C8 124.9(5) . . ? C6 N2 C8 126.4(4) . . ? C3 C2 C1 116.8(5) . . ? C3 C2 H2A 121.6 . . ? C1 C2 H2A 121.6 . . ? C19 O2 Cd1 94.0(4) . . ? C27 O3 Cd1 137.5(3) . 4_576 ? C18 N3 C12 105.7(4) . . ? C18 N3 C11 126.1(5) . . ? C12 N3 C11 127.9(4) . . ? C2 C3 C4 122.4(6) . . ? C2 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? C18 N4 C17 105.2(4) . . ? C18 N4 Cd1 127.1(3) . 4_475 ? C17 N4 Cd1 127.3(4) . 4_475 ? C5 C4 C3 120.8(5) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C27 O4 Cd1 144.6(4) . 2_655 ? O6 N5 O5 123.2(6) . . ? O6 N5 C24 118.7(6) . . ? O5 N5 C24 118.1(5) . . ? C6 C5 C4 116.6(5) . . ? C6 C5 H5A 121.7 . . ? C4 C5 H5A 121.7 . . ? C5 C6 C1 122.8(5) . . ? C5 C6 N2 131.8(5) . . ? C1 C6 N2 105.4(4) . . ? N1 C7 N2 112.2(5) . . ? N1 C7 H7A 123.9 . . ? N2 C7 H7A 123.9 . . ? N2 C8 C9 112.0(5) . . ? N2 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 114.3(5) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 112.7(4) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N3 C11 C10 113.7(5) . . ? N3 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? N3 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 121.5(6) . . ? C17 C12 N3 106.0(4) . . ? C13 C12 N3 132.5(5) . . ? C14 C13 C12 117.1(6) . . ? C14 C13 H13A 121.5 . . ? C12 C13 H13A 121.5 . . ? C13 C14 C15 122.1(5) . . ? C13 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C14 C15 C16 121.4(6) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C15 C16 C17 116.8(6) . . ? C15 C16 H16A 121.6 . . ? C17 C16 H16A 121.6 . . ? C12 C17 C16 121.0(5) . . ? C12 C17 N4 109.5(5) . . ? C16 C17 N4 129.4(5) . . ? N4 C18 N3 113.6(5) . . ? N4 C18 H18A 123.2 . . ? N3 C18 H18A 123.2 . . ? O1 C19 O2 123.2(5) . . ? O1 C19 C20 118.7(5) . . ? O2 C19 C20 118.1(6) . . ? C25 C20 C21 118.7(5) . . ? C25 C20 C19 120.4(5) . . ? C21 C20 C19 120.9(5) . . ? C20 C21 C22 121.3(5) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 119.6(5) . . ? C23 C22 C27 121.6(4) . . ? C21 C22 C27 118.8(5) . . ? C22 C23 C24 118.1(5) . . ? C22 C23 H23A 120.9 . . ? C24 C23 H23A 120.9 . . ? C25 C24 C23 122.9(5) . . ? C25 C24 N5 118.2(5) . . ? C23 C24 N5 118.8(5) . . ? C24 C25 C20 119.3(5) . . ? C24 C25 H25A 120.4 . . ? C20 C25 H25A 120.4 . . ? O4 C27 O3 126.9(5) . . ? O4 C27 C22 116.7(5) . . ? O3 C27 C22 116.5(5) . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 2.224 _refine_diff_density_min -1.578 _refine_diff_density_rms 0.198 #===END #===END data_hll-3 _database_code_depnum_ccdc_archive 'CCDC 831732' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H72 Cd3 N12 O20 S2' _chemical_formula_sum 'C70 H72 Cd3 N12 O20 S2' _chemical_formula_weight 1802.76 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall 'P 2c -2n ' _symmetry_Int_Tables_number No.33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.181(5) _cell_length_b 22.175(5) _cell_length_c 18.450(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7438(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5223 _cell_measurement_theta_min 2.4182 _cell_measurement_theta_max 22.9189 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3599 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45788 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12229 _reflns_number_gt 10447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0833P)^2^+3.2633P] 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 -0.02(2) _refine_ls_number_reflns 12229 _refine_ls_number_parameters 964 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.004 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 Cd1 Cd 0.62327(2) 0.500703(19) 0.92682(3) 0.03619(13) Uani 1 1 d . . . S1 S 0.82357(9) 0.51014(7) 0.94519(11) 0.0421(4) Uani 1 1 d . . . O1 O 0.6250(3) 0.6156(2) 0.9343(4) 0.0639(16) Uani 1 1 d . . . N1 N 0.5983(4) 0.5045(3) 1.0438(4) 0.0505(17) Uani 1 1 d . . . C1 C 0.8527(3) 0.4342(2) 0.9403(4) 0.0316(13) Uani 1 1 d . . . O1W O 0.7658(7) 0.6672(4) 0.9580(5) 0.174(5) Uani 1 1 d . . . Cd2 Cd 0.55359(2) 0.824169(18) 0.93487(2) 0.03233(13) Uani 1 1 d . . . S2 S 0.42365(9) 0.49311(7) 0.93315(13) 0.0438(4) Uani 1 1 d . . . O2 O 0.6184(3) 0.3965(2) 0.9142(4) 0.0605(15) Uani 1 1 d . . . N2 N 0.6434(4) 0.5163(3) 0.8093(3) 0.0457(15) Uani 1 1 d . . . C2 C 0.9278(3) 0.4210(3) 0.9358(4) 0.0355(14) Uani 1 1 d . . . H2A H 0.9617 0.4523 0.9324 0.043 Uiso 1 1 calc R . . O2W O 0.6114(8) 1.0015(3) 0.9845(6) 0.188(8) Uani 1 1 d . . . Cd3 Cd 0.67989(2) 0.178108(18) 0.94967(3) 0.03278(13) Uani 1 1 d . . . O3 O 0.7459(3) 0.5066(2) 0.9623(4) 0.0584(16) Uani 1 1 d . . . N3 N 0.5497(3) 0.5425(3) 1.1451(3) 0.0506(16) Uani 1 1 d . . . C3 C 0.9525(3) 0.3609(2) 0.9363(4) 0.0307(13) Uani 1 1 d . . . O4 O 0.8392(5) 0.5372(3) 0.8769(4) 0.094(3) Uani 1 1 d . . . N4 N 0.6330(4) 0.5635(3) 0.7037(3) 0.0461(15) Uani 1 1 d . . . C4 C 0.8989(3) 0.3155(3) 0.9412(4) 0.0333(14) Uani 1 1 d . . . H4A H 0.9137 0.2753 0.9418 0.040 Uiso 1 1 calc R . . O5 O 0.8652(3) 0.5359(3) 1.0039(4) 0.0721(19) Uani 1 1 d . . . N5 N 0.5381(3) 0.8431(3) 1.0562(3) 0.0430(14) Uani 1 1 d . . . C5 C 0.8252(3) 0.3289(3) 0.9449(4) 0.0332(14) Uani 1 1 d . . . O6 O 0.7922(2) 0.22531(19) 0.9532(3) 0.0512(13) Uani 1 1 d . . . N6 N 0.5460(4) 0.8194(3) 0.8100(4) 0.0445(16) Uani 1 1 d . . . C6 C 0.8032(3) 0.3884(3) 0.9447(4) 0.0361(15) Uani 1 1 d . . . H6A H 0.7533 0.3974 0.9476 0.043 Uiso 1 1 calc R . . O7 O 0.7019(2) 0.29155(19) 0.9499(3) 0.0483(13) Uani 1 1 d . . . N7 N 0.5003(3) 0.8854(2) 1.1591(3) 0.0399(14) Uani 1 1 d . . . C7 C 1.0317(3) 0.3463(2) 0.9373(4) 0.0350(14) Uani 1 1 d . . . O8 O 1.0509(2) 0.2937(2) 0.9465(3) 0.0490(13) Uani 1 1 d . . . N8 N 0.5160(4) 0.7877(3) 0.6994(4) 0.0604(19) Uani 1 1 d . . . C8 C 0.7699(3) 0.2788(3) 0.9500(4) 0.0360(14) Uani 1 1 d . . . O9 O 1.0770(2) 0.38826(18) 0.9311(3) 0.0471(12) Uani 1 1 d . . . N9 N 0.3212(3) 0.8104(3) 1.3248(4) 0.0467(16) Uani 1 1 d . . . C9 C 0.6108(4) 0.4634(3) 1.1005(4) 0.0419(16) Uani 1 1 d . . . O10 O 0.4337(2) 0.77829(19) 0.9390(4) 0.0568(15) Uani 1 1 d . . . N10 N 0.6677(4) 1.1578(3) 1.0732(4) 0.0475(16) Uani 1 1 d . . . C10 C 0.6470(5) 0.4104(4) 1.1042(5) 0.062(2) Uani 1 1 d . . . H10A H 0.6679 0.3934 1.0629 0.074 Uiso 1 1 calc R . . O11 O 0.4949(3) 0.9186(2) 0.9116(3) 0.0512(14) Uani 1 1 d . . . N11 N 0.3576(4) 0.7663(3) 1.2229(4) 0.0541(17) Uani 1 1 d . . . C11 C 0.6524(6) 0.3815(5) 1.1711(6) 0.079(3) Uani 1 1 d . . . H11A H 0.6762 0.3444 1.1736 0.095 Uiso 1 1 calc R . . O12 O 0.1588(2) 0.6051(2) 0.9431(3) 0.0545(14) Uani 1 1 d . . . N12 N 0.6366(3) 1.1047(3) 1.1700(3) 0.0428(14) Uani 1 1 d . . . C12 C 0.6243(5) 0.4055(4) 1.2327(5) 0.069(3) Uani 1 1 d . . . H12A H 0.6308 0.3854 1.2765 0.083 Uiso 1 1 calc R . . O13 O 0.1803(2) 0.7008(2) 0.9391(4) 0.0597(16) Uani 1 1 d . . . C13 C 0.5861(5) 0.4593(4) 1.2312(4) 0.065(2) Uani 1 1 d . . . H13A H 0.5653 0.4754 1.2730 0.078 Uiso 1 1 calc R . . O14 O 0.4278(4) 0.4750(3) 1.0090(4) 0.077(2) Uani 1 1 d . . . C14 C 0.5801(4) 0.4884(3) 1.1647(4) 0.0458(18) Uani 1 1 d . . . O15 O 0.3733(3) 0.4570(2) 0.8888(4) 0.0732(19) Uani 1 1 d . . . C15 C 0.5642(5) 0.5514(4) 1.0743(4) 0.058(2) Uani 1 1 d . . . H15A H 0.5518 0.5864 1.0493 0.070 Uiso 1 1 calc R . . O16 O 0.4954(3) 0.4995(2) 0.8995(3) 0.0468(13) Uani 1 1 d . . . C16 C 0.5133(5) 0.5847(4) 1.1943(5) 0.073(3) Uani 1 1 d . . . H16A H 0.5502 0.6052 1.2231 0.088 Uiso 1 1 calc R . . H16B H 0.4818 0.5623 1.2272 0.088 Uiso 1 1 calc R . . O17 O 0.5284(2) 0.71678(19) 0.9423(4) 0.0520(13) Uani 1 1 d . . . C17 C 0.4670(5) 0.6317(4) 1.1542(5) 0.064(2) Uani 1 1 d . . . H17A H 0.4285 0.6117 1.1268 0.077 Uiso 1 1 calc R . . H17B H 0.4977 0.6539 1.1205 0.077 Uiso 1 1 calc R . . C18 C 0.4327(5) 0.6750(4) 1.2088(5) 0.062(2) Uani 1 1 d . . . H18A H 0.4008 0.6528 1.2414 0.074 Uiso 1 1 calc R . . H18B H 0.4713 0.6935 1.2376 0.074 Uiso 1 1 calc R . . O19 O 0.7463(3) 0.0850(2) 0.9531(4) 0.0698(18) Uani 1 1 d . . . C19 C 0.3905(6) 0.7217(4) 1.1728(5) 0.073(3) Uani 1 1 d . . . H19A H 0.3515 0.7028 1.1450 0.087 Uiso 1 1 calc R . . H19B H 0.4224 0.7426 1.1390 0.087 Uiso 1 1 calc R . . C20 C 0.3208(4) 0.8162(3) 1.2013(5) 0.0420(18) Uani 1 1 d . . . C21 C 0.2961(4) 0.8448(3) 1.2658(4) 0.0421(17) Uani 1 1 d . . . C22 C 0.2566(4) 0.8977(4) 1.2622(5) 0.059(2) Uani 1 1 d . . . H22A H 0.2405 0.9170 1.3041 0.071 Uiso 1 1 calc R . . C23 C 0.2419(5) 0.9210(4) 1.1949(6) 0.065(3) Uani 1 1 d . . . H23A H 0.2147 0.9564 1.1912 0.079 Uiso 1 1 calc R . . C24 C 0.2668(5) 0.8928(4) 1.1321(5) 0.068(3) Uani 1 1 d . . . H24A H 0.2556 0.9098 1.0873 0.082 Uiso 1 1 calc R . . C25 C 0.3064(5) 0.8419(4) 1.1342(5) 0.060(2) Uani 1 1 d . . . H25A H 0.3238 0.8242 1.0918 0.072 Uiso 1 1 calc R . . C26 C 0.3569(4) 0.7642(3) 1.2959(4) 0.0512(19) Uani 1 1 d . . . H26A H 0.3790 0.7337 1.3230 0.061 Uiso 1 1 calc R . . C27 C 0.5462(4) 0.8389(4) 1.1775(4) 0.0435(19) Uani 1 1 d . . . C28 C 0.5681(6) 0.8171(4) 1.2460(5) 0.064(3) Uani 1 1 d . . . H28A H 0.5526 0.8355 1.2886 0.077 Uiso 1 1 calc R . . C29 C 0.6137(6) 0.7671(4) 1.2470(6) 0.077(3) Uani 1 1 d . . . H29A H 0.6292 0.7510 1.2910 0.093 Uiso 1 1 calc R . . C30 C 0.6375(5) 0.7397(4) 1.1795(5) 0.070(3) Uani 1 1 d . . . H30A H 0.6684 0.7063 1.1814 0.084 Uiso 1 1 calc R . . C31 C 0.6167(4) 0.7605(3) 1.1150(5) 0.0521(19) Uani 1 1 d . . . H31A H 0.6318 0.7419 1.0723 0.063 Uiso 1 1 calc R . . C32 C 0.5704(4) 0.8127(3) 1.1139(4) 0.0443(18) Uani 1 1 d . . . C33 C 0.4981(4) 0.8848(3) 1.0850(4) 0.0445(17) Uani 1 1 d . . . H33A H 0.4704 0.9119 1.0580 0.053 Uiso 1 1 calc R . . C34 C 0.4670(5) 0.9287(3) 1.2089(5) 0.054(2) Uani 1 1 d . . . H34A H 0.4436 0.9069 1.2482 0.064 Uiso 1 1 calc R . . H34B H 0.4290 0.9509 1.1833 0.064 Uiso 1 1 calc R . . C35 C 0.5191(5) 0.9711(3) 1.2390(4) 0.053(2) Uani 1 1 d . . . H35A H 0.5585 0.9488 1.2621 0.063 Uiso 1 1 calc R . . H35B H 0.4947 0.9948 1.2760 0.063 Uiso 1 1 calc R . . C36 C 0.5532(4) 1.0149(3) 1.1814(4) 0.0449(18) Uani 1 1 d . . . H36A H 0.5811 0.9921 1.1461 0.054 Uiso 1 1 calc R . . H36B H 0.5142 1.0361 1.1561 0.054 Uiso 1 1 calc R . . C37 C 0.6033(5) 1.0601(4) 1.2193(4) 0.059(2) Uani 1 1 d . . . H37A H 0.5752 1.0813 1.2559 0.071 Uiso 1 1 calc R . . H37B H 0.6423 1.0383 1.2437 0.071 Uiso 1 1 calc R . . C38 C 0.6820(4) 1.1506(3) 1.1944(4) 0.0423(18) Uani 1 1 d . . . C39 C 0.7002(4) 1.1831(3) 1.1333(4) 0.0428(18) Uani 1 1 d . . . C40 C 0.7453(4) 1.2344(3) 1.1402(5) 0.053(2) Uani 1 1 d . . . H40A H 0.7590 1.2572 1.1001 0.063 Uiso 1 1 calc R . . C41 C 0.7684(5) 1.2495(4) 1.2091(5) 0.060(2) Uani 1 1 d . . . H41A H 0.7973 1.2837 1.2153 0.072 Uiso 1 1 calc R . . C42 C 0.7499(6) 1.2151(4) 1.2697(5) 0.070(3) Uani 1 1 d . . . H42A H 0.7680 1.2258 1.3151 0.084 Uiso 1 1 calc R . . C43 C 0.7053(5) 1.1659(4) 1.2630(5) 0.061(2) Uani 1 1 d . . . H43A H 0.6911 1.1435 1.3032 0.074 Uiso 1 1 calc R . . C44 C 0.6314(4) 1.1109(3) 1.0986(4) 0.0428(17) Uani 1 1 d . . . H44A H 0.6048 1.0847 1.0693 0.051 Uiso 1 1 calc R . . C45 C 0.6842(4) 0.4845(3) 0.7570(4) 0.0439(17) Uani 1 1 d . . . C46 C 0.7269(4) 0.4336(4) 0.7625(5) 0.055(2) Uani 1 1 d . . . H46A H 0.7329 0.4138 0.8065 0.066 Uiso 1 1 calc R . . C47 C 0.7601(5) 0.4134(4) 0.7011(5) 0.064(2) Uani 1 1 d . . . H47A H 0.7876 0.3780 0.7030 0.076 Uiso 1 1 calc R . . C48 C 0.7542(5) 0.4441(5) 0.6354(5) 0.072(3) Uani 1 1 d . . . H48A H 0.7796 0.4296 0.5952 0.086 Uiso 1 1 calc R . . C49 C 0.7128(5) 0.4940(4) 0.6282(4) 0.058(2) Uani 1 1 d . . . H49A H 0.7079 0.5137 0.5840 0.070 Uiso 1 1 calc R . . C50 C 0.6777(4) 0.5146(3) 0.6909(4) 0.0460(18) Uani 1 1 d . . . C51 C 0.6153(4) 0.5625(3) 0.7741(4) 0.0481(18) Uani 1 1 d . . . H51A H 0.5860 0.5916 0.7960 0.058 Uiso 1 1 calc R . . C52 C 0.6113(5) 0.6077(3) 0.6485(4) 0.057(2) Uani 1 1 d . . . H52A H 0.5868 0.5868 0.6091 0.068 Uiso 1 1 calc R . . H52B H 0.6553 0.6265 0.6290 0.068 Uiso 1 1 calc R . . C53 C 0.5601(5) 0.6570(4) 0.6775(4) 0.061(2) Uani 1 1 d . . . H53A H 0.5847 0.6793 0.7157 0.073 Uiso 1 1 calc R . . H53B H 0.5162 0.6388 0.6977 0.073 Uiso 1 1 calc R . . C54 C 0.5391(6) 0.7001(4) 0.6157(4) 0.071(3) Uani 1 1 d . . . H54A H 0.5174 0.6771 0.5764 0.085 Uiso 1 1 calc R . . H54B H 0.5830 0.7196 0.5974 0.085 Uiso 1 1 calc R . . C55 C 0.4839(6) 0.7486(4) 0.6415(5) 0.081(3) Uani 1 1 d . . . H55A H 0.4696 0.7734 0.6006 0.098 Uiso 1 1 calc R . . H55B H 0.4400 0.7290 0.6599 0.098 Uiso 1 1 calc R . . C56 C 0.5624(6) 0.8358(4) 0.6903(5) 0.054(2) Uani 1 1 d . . . C57 C 0.5801(4) 0.8541(3) 0.7594(4) 0.0421(17) Uani 1 1 d . . . C58 C 0.6278(5) 0.9031(3) 0.7678(5) 0.061(2) Uani 1 1 d . . . H58A H 0.6410 0.9169 0.8136 0.073 Uiso 1 1 calc R . . C59 C 0.6547(6) 0.9301(4) 0.7058(6) 0.079(3) Uani 1 1 d . . . H59A H 0.6862 0.9628 0.7111 0.095 Uiso 1 1 calc R . . C60 C 0.6382(7) 0.9119(5) 0.6383(6) 0.091(4) Uani 1 1 d . . . H60A H 0.6576 0.9324 0.5987 0.110 Uiso 1 1 calc R . . C61 C 0.5941(7) 0.8646(5) 0.6279(5) 0.088(4) Uani 1 1 d . . . H61A H 0.5841 0.8506 0.5814 0.106 Uiso 1 1 calc R . . C62 C 0.5068(5) 0.7787(4) 0.7718(5) 0.061(2) Uani 1 1 d . . . H62A H 0.4776 0.7487 0.7921 0.073 Uiso 1 1 calc R . . C63 C 0.3865(3) 0.5672(3) 0.9348(4) 0.0379(15) Uani 1 1 d . . . C64 C 0.3113(3) 0.5777(3) 0.9387(4) 0.0385(16) Uani 1 1 d . . . H64A H 0.2789 0.5453 0.9394 0.046 Uiso 1 1 calc R . . C65 C 0.2846(3) 0.6352(3) 0.9417(4) 0.0371(15) Uani 1 1 d . . . C66 C 0.3326(3) 0.6842(3) 0.9432(5) 0.0415(17) Uani 1 1 d . . . H66A H 0.3142 0.7232 0.9460 0.050 Uiso 1 1 calc R . . C67 C 0.4092(3) 0.6745(3) 0.9407(4) 0.0396(15) Uani 1 1 d . . . C68 C 0.4349(3) 0.6144(2) 0.9356(4) 0.0387(15) Uani 1 1 d . . . H68A H 0.4851 0.6070 0.9327 0.046 Uiso 1 1 calc R . . C69 C 0.4606(4) 0.7262(3) 0.9404(5) 0.0437(16) Uani 1 1 d . . . C70 C 0.2015(3) 0.6485(3) 0.9424(5) 0.0460(18) 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 Cd1 0.0271(2) 0.0467(2) 0.0348(3) -0.0013(2) 0.0023(2) 0.00605(19) S1 0.0301(8) 0.0380(8) 0.0582(13) 0.0001(8) 0.0065(8) -0.0010(6) O1 0.055(3) 0.058(3) 0.078(5) 0.007(3) 0.015(3) 0.010(2) N1 0.049(4) 0.065(4) 0.037(4) -0.004(3) 0.004(3) 0.017(3) C1 0.023(3) 0.037(3) 0.035(4) 0.001(3) 0.001(3) -0.003(2) O1W 0.293(14) 0.133(7) 0.096(8) 0.034(6) -0.048(9) -0.121(9) Cd2 0.0274(2) 0.0332(2) 0.0363(3) -0.0018(2) 0.0024(2) -0.00476(16) S2 0.0298(8) 0.0399(8) 0.0617(13) 0.0109(9) 0.0085(10) 0.0016(6) O2 0.049(3) 0.052(3) 0.080(4) -0.007(3) -0.006(3) 0.005(2) N2 0.046(4) 0.057(4) 0.034(4) 0.000(3) 0.006(3) 0.009(3) C2 0.027(3) 0.041(3) 0.039(4) -0.003(3) 0.000(3) -0.004(2) O2W 0.41(2) 0.063(5) 0.088(7) -0.014(4) -0.007(9) 0.064(9) Cd3 0.0255(2) 0.0323(2) 0.0406(3) 0.0049(2) -0.0005(2) -0.00287(17) O3 0.024(2) 0.052(3) 0.099(5) -0.007(3) -0.006(3) 0.004(2) N3 0.050(4) 0.070(4) 0.032(4) -0.013(3) 0.005(3) 0.010(3) C3 0.024(3) 0.037(3) 0.032(3) 0.000(3) 0.000(3) -0.004(2) O4 0.133(7) 0.065(4) 0.085(5) 0.037(4) 0.053(5) 0.038(4) N4 0.054(4) 0.045(3) 0.040(4) 0.004(3) 0.001(3) 0.005(3) C4 0.036(3) 0.039(3) 0.026(4) 0.004(3) -0.003(3) 0.003(2) O5 0.043(3) 0.062(4) 0.111(5) -0.038(4) -0.013(3) 0.002(3) N5 0.046(4) 0.046(3) 0.038(4) -0.004(3) -0.003(3) 0.002(3) C5 0.024(3) 0.043(3) 0.032(4) -0.001(3) 0.005(3) -0.006(2) O6 0.040(3) 0.042(2) 0.072(4) 0.009(3) -0.006(3) -0.007(2) N6 0.056(4) 0.040(3) 0.038(4) -0.001(3) -0.001(3) -0.002(3) C6 0.031(3) 0.044(3) 0.034(4) -0.007(3) -0.003(3) -0.008(3) O7 0.029(2) 0.046(2) 0.070(4) 0.004(3) 0.002(3) -0.0088(19) N7 0.042(3) 0.040(3) 0.038(4) -0.003(3) 0.009(3) -0.003(3) C7 0.039(3) 0.034(3) 0.033(4) -0.002(3) 0.003(4) 0.002(3) O8 0.042(3) 0.042(3) 0.064(4) 0.001(3) 0.002(3) 0.0024(19) N8 0.086(5) 0.052(4) 0.043(4) -0.006(3) -0.017(4) 0.017(4) C8 0.038(4) 0.036(3) 0.034(4) 0.004(3) 0.003(3) -0.004(3) O9 0.023(2) 0.044(2) 0.074(4) -0.003(3) 0.001(3) -0.0041(18) N9 0.054(4) 0.044(3) 0.042(4) -0.006(3) 0.000(3) 0.005(3) C9 0.033(4) 0.051(4) 0.042(4) -0.005(3) 0.004(3) 0.000(3) O10 0.040(3) 0.042(2) 0.088(5) 0.001(3) -0.006(3) -0.011(2) N10 0.056(4) 0.048(4) 0.039(4) 0.001(3) -0.005(3) -0.009(3) C10 0.054(5) 0.073(6) 0.057(6) -0.009(4) 0.007(4) 0.011(4) O11 0.049(3) 0.048(3) 0.057(4) 0.006(2) 0.002(3) 0.011(2) N11 0.059(4) 0.056(4) 0.047(4) -0.014(3) 0.009(3) 0.001(3) C11 0.087(7) 0.074(6) 0.076(7) 0.011(5) -0.009(6) 0.032(6) O12 0.025(2) 0.060(3) 0.078(4) -0.006(3) 0.004(3) -0.006(2) N12 0.053(4) 0.038(3) 0.037(3) 0.003(2) -0.002(3) -0.008(3) C12 0.080(7) 0.082(7) 0.046(5) 0.016(5) 0.006(5) 0.004(5) O13 0.028(2) 0.061(3) 0.090(5) 0.012(4) 0.007(3) 0.013(2) C13 0.079(6) 0.085(6) 0.030(4) -0.003(4) 0.007(4) -0.018(5) O14 0.079(4) 0.074(4) 0.079(5) 0.035(3) 0.035(4) 0.024(3) C14 0.043(4) 0.051(4) 0.043(5) -0.007(3) -0.003(4) 0.000(4) O15 0.037(3) 0.051(3) 0.132(6) -0.014(3) 0.001(3) -0.010(3) C15 0.056(5) 0.074(5) 0.044(5) -0.006(4) 0.006(4) 0.015(4) O16 0.025(2) 0.062(3) 0.053(3) 0.004(2) 0.001(2) 0.002(2) C16 0.080(7) 0.072(6) 0.067(7) -0.028(5) 0.023(5) 0.013(5) O17 0.036(2) 0.041(2) 0.079(4) 0.004(3) 0.000(3) -0.0119(19) C17 0.067(6) 0.068(5) 0.058(6) -0.023(4) 0.012(4) 0.003(5) C18 0.063(6) 0.058(5) 0.065(6) -0.012(4) 0.011(5) 0.014(4) O19 0.063(3) 0.049(3) 0.097(5) 0.018(3) 0.023(4) 0.023(3) C19 0.094(7) 0.076(6) 0.047(5) -0.019(4) 0.012(5) 0.005(5) C20 0.041(4) 0.043(4) 0.042(5) -0.003(3) -0.007(3) 0.001(3) C21 0.037(4) 0.040(4) 0.049(5) 0.000(3) 0.000(3) -0.006(3) C22 0.047(5) 0.058(5) 0.072(6) 0.002(4) 0.011(4) 0.008(4) C23 0.056(5) 0.058(5) 0.083(8) 0.019(5) -0.006(5) 0.007(4) C24 0.071(6) 0.067(6) 0.067(6) 0.032(5) -0.003(5) 0.006(5) C25 0.065(6) 0.071(6) 0.043(5) 0.006(4) 0.005(4) -0.011(5) C26 0.060(5) 0.042(4) 0.052(5) -0.010(3) 0.004(4) 0.005(4) C27 0.043(5) 0.054(5) 0.033(4) 0.000(3) 0.000(3) -0.006(4) C28 0.084(7) 0.064(6) 0.044(5) -0.002(4) 0.003(5) -0.006(5) C29 0.083(7) 0.084(7) 0.064(7) 0.021(5) -0.015(5) 0.018(6) C30 0.082(7) 0.062(5) 0.065(6) 0.014(4) -0.004(5) 0.023(5) C31 0.050(5) 0.051(4) 0.056(5) 0.001(4) 0.002(4) 0.010(4) C32 0.036(4) 0.057(5) 0.040(4) -0.001(3) -0.005(3) 0.004(3) C33 0.039(4) 0.039(4) 0.056(5) 0.004(3) -0.001(4) 0.003(3) C34 0.057(5) 0.040(4) 0.064(5) -0.008(4) 0.027(4) -0.010(4) C35 0.074(6) 0.046(4) 0.038(4) -0.007(3) 0.017(4) -0.010(4) C36 0.055(5) 0.042(4) 0.037(4) 0.001(3) 0.012(4) -0.005(3) C37 0.084(6) 0.062(5) 0.032(4) 0.012(4) -0.006(4) -0.030(4) C38 0.041(4) 0.044(4) 0.042(5) 0.000(3) -0.002(3) -0.002(3) C39 0.044(4) 0.038(4) 0.046(5) -0.011(3) -0.005(4) 0.003(3) C40 0.053(5) 0.045(4) 0.060(5) 0.007(4) -0.003(4) -0.016(4) C41 0.062(5) 0.050(5) 0.068(6) -0.004(4) -0.014(5) -0.015(4) C42 0.091(7) 0.075(6) 0.044(5) -0.010(4) -0.010(5) -0.017(5) C43 0.071(6) 0.070(6) 0.043(5) 0.006(4) -0.009(4) -0.023(5) C44 0.047(4) 0.046(4) 0.036(4) 0.003(3) -0.004(3) -0.005(3) C45 0.035(4) 0.053(4) 0.043(4) -0.005(3) 0.000(3) 0.004(3) C46 0.045(5) 0.067(5) 0.052(5) 0.006(4) -0.002(4) 0.023(4) C47 0.059(6) 0.077(6) 0.055(6) -0.001(5) -0.004(4) 0.025(4) C48 0.067(6) 0.107(8) 0.042(5) -0.016(5) 0.012(5) 0.027(6) C49 0.073(6) 0.069(5) 0.033(4) -0.010(4) 0.007(4) 0.007(4) C50 0.042(4) 0.051(4) 0.045(5) 0.003(3) 0.001(4) -0.001(3) C51 0.045(4) 0.065(5) 0.034(4) -0.007(3) -0.004(3) 0.015(4) C52 0.082(6) 0.055(5) 0.034(4) -0.005(3) -0.004(4) 0.007(4) C53 0.089(6) 0.044(4) 0.050(5) -0.007(3) -0.029(5) 0.007(4) C54 0.131(9) 0.048(5) 0.035(5) -0.009(4) -0.023(5) 0.021(5) C55 0.116(9) 0.067(6) 0.061(6) -0.024(5) -0.041(6) 0.031(6) C56 0.072(6) 0.043(5) 0.048(5) 0.004(4) 0.007(4) 0.017(4) C57 0.062(5) 0.037(4) 0.028(4) 0.002(3) 0.007(3) 0.005(3) C58 0.091(7) 0.047(5) 0.046(5) 0.001(3) 0.018(5) 0.007(4) C59 0.089(8) 0.064(6) 0.083(8) 0.019(5) 0.038(6) -0.008(5) C60 0.140(11) 0.075(7) 0.059(7) 0.010(5) 0.027(7) -0.007(7) C61 0.151(11) 0.085(7) 0.028(5) 0.007(4) 0.013(6) 0.060(8) C62 0.075(6) 0.062(5) 0.046(5) -0.004(4) -0.007(4) 0.009(4) C63 0.029(3) 0.040(3) 0.044(4) 0.003(3) -0.001(4) -0.004(2) C64 0.025(3) 0.043(3) 0.048(5) 0.005(3) 0.003(3) -0.008(2) C65 0.029(3) 0.037(3) 0.045(4) 0.000(3) -0.003(3) -0.002(2) C66 0.027(3) 0.042(3) 0.056(5) -0.005(3) 0.006(4) 0.001(3) C67 0.024(3) 0.053(3) 0.042(4) 0.002(3) -0.004(3) -0.009(3) C68 0.021(3) 0.036(3) 0.059(5) 0.011(4) -0.003(3) -0.005(2) C69 0.041(4) 0.043(4) 0.047(5) -0.002(3) 0.005(4) -0.010(3) C70 0.026(3) 0.055(4) 0.057(5) 0.004(4) 0.000(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.226(6) . ? Cd1 N1 2.207(7) . ? Cd1 O3 2.328(5) . ? Cd1 O2 2.325(5) . ? Cd1 O16 2.379(5) . ? Cd1 O1 2.552(5) . ? S1 O4 1.425(6) . ? S1 O5 1.439(6) . ? S1 O3 1.449(5) . ? S1 C1 1.768(6) . ? N1 C15 1.335(10) . ? N1 C9 1.406(9) . ? C1 C6 1.359(8) . ? C1 C2 1.399(8) . ? Cd2 N6 2.311(7) . ? Cd2 N5 2.295(6) . ? Cd2 O13 2.370(4) 4_565 ? Cd2 O11 2.390(5) . ? Cd2 O10 2.407(4) . ? Cd2 O17 2.429(4) . ? Cd2 O12 2.479(5) 4_565 ? Cd2 C69 2.755(6) . ? Cd2 C70 2.760(6) 4_565 ? S2 O16 1.452(5) . ? S2 O14 1.458(7) . ? S2 O15 1.466(6) . ? S2 C63 1.778(6) . ? N2 C51 1.317(9) . ? N2 C45 1.406(9) . ? C2 C3 1.406(8) . ? C2 H2A 0.9300 . ? Cd3 O6 2.295(4) . ? Cd3 N9 2.319(7) 2_664 ? Cd3 N10 2.334(7) 1_545 ? Cd3 O19 2.393(5) . ? Cd3 O9 2.405(4) 4_455 ? Cd3 O8 2.428(4) 4_455 ? Cd3 O7 2.547(4) . ? Cd3 C7 2.757(6) 4_455 ? Cd3 C8 2.768(6) . ? N3 C15 1.348(10) . ? N3 C14 1.370(10) . ? N3 C16 1.462(9) . ? C3 C4 1.404(8) . ? C3 C7 1.476(8) . ? N4 C51 1.338(9) . ? N4 C50 1.374(9) . ? N4 C52 1.468(9) . ? C4 C5 1.375(8) . ? C4 H4A 0.9300 . ? N5 C33 1.291(9) . ? N5 C32 1.390(10) . ? C5 C6 1.378(8) . ? C5 C8 1.501(8) . ? O6 C8 1.255(7) . ? N6 C62 1.350(11) . ? N6 C57 1.359(9) . ? C6 H6A 0.9300 . ? O7 C8 1.268(7) . ? N7 C33 1.367(9) . ? N7 C27 1.368(10) . ? N7 C34 1.461(9) . ? C7 O8 1.229(7) . ? C7 O9 1.249(7) . ? C7 Cd3 2.757(6) 4 ? O8 Cd3 2.428(4) 4 ? N8 C62 1.361(11) . ? N8 C56 1.370(12) . ? N8 C55 1.495(11) . ? O9 Cd3 2.405(4) 4 ? N9 C26 1.326(9) . ? N9 C21 1.404(10) . ? N9 Cd3 2.319(7) 2_665 ? C9 C10 1.349(10) . ? C9 C14 1.423(10) . ? O10 C69 1.256(8) . ? N10 C44 1.316(9) . ? N10 C39 1.377(10) . ? N10 Cd3 2.334(7) 1_565 ? C10 C11 1.395(13) . ? C10 H10A 0.9300 . ? N11 C20 1.353(10) . ? N11 C26 1.348(10) . ? N11 C19 1.481(10) . ? C11 C12 1.354(13) . ? C11 H11A 0.9300 . ? O12 C70 1.238(8) . ? O12 Cd2 2.479(4) 4_465 ? N12 C44 1.327(9) . ? N12 C38 1.385(9) . ? N12 C37 1.474(9) . ? C12 C13 1.381(13) . ? C12 H12A 0.9300 . ? O13 C70 1.223(8) . ? O13 Cd2 2.370(4) 4_465 ? C13 C14 1.390(11) . ? C13 H13A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.530(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? O17 C69 1.250(8) . ? C17 C18 1.526(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.448(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.388(12) . ? C20 C21 1.421(11) . ? C21 C22 1.377(11) . ? C22 C23 1.372(13) . ? C22 H22A 0.9300 . ? C23 C24 1.393(13) . ? C23 H23A 0.9300 . ? C24 C25 1.340(12) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C32 1.381(11) . ? C27 C28 1.411(12) . ? C28 C29 1.386(13) . ? C28 H28A 0.9300 . ? C29 C30 1.450(13) . ? C29 H29A 0.9300 . ? C30 C31 1.332(11) . ? C30 H30A 0.9300 . ? C31 C32 1.431(10) . ? C31 H31A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.445(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.567(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.525(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C43 1.376(11) . ? C38 C39 1.377(11) . ? C39 C40 1.408(10) . ? C40 C41 1.378(12) . ? C40 H40A 0.9300 . ? C41 C42 1.396(12) . ? C41 H41A 0.9300 . ? C42 C43 1.366(12) . ? C42 H42A 0.9300 . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C46 1.374(10) . ? C45 C50 1.395(11) . ? C46 C47 1.360(12) . ? C46 H46A 0.9300 . ? C47 C48 1.396(13) . ? C47 H47A 0.9300 . ? C48 C49 1.344(12) . ? C48 H48A 0.9300 . ? C49 C50 1.399(11) . ? C49 H49A 0.9300 . ? C51 H51A 0.9300 . ? C52 C53 1.532(11) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.535(11) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.546(12) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.376(12) . ? C56 C61 1.438(14) . ? C57 C58 1.398(11) . ? C58 C59 1.381(12) . ? C58 H58A 0.9300 . ? C59 C60 1.342(15) . ? C59 H59A 0.9300 . ? C60 C61 1.336(16) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 H62A 0.9300 . ? C63 C68 1.367(8) . ? C63 C64 1.388(8) . ? C64 C65 1.366(8) . ? C64 H64A 0.9300 . ? C65 C66 1.395(8) . ? C65 C70 1.540(8) . ? C66 C67 1.410(8) . ? C66 H66A 0.9300 . ? C67 C68 1.415(8) . ? C67 C69 1.477(8) . ? C68 H68A 0.9300 . ? C70 Cd2 2.760(6) 4_465 ? 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 Cd1 N1 168.7(2) . . ? N2 Cd1 O3 96.2(2) . . ? N1 Cd1 O3 85.4(3) . . ? N2 Cd1 O2 93.6(2) . . ? N1 Cd1 O2 97.3(2) . . ? O3 Cd1 O2 96.95(17) . . ? N2 Cd1 O16 87.5(2) . . ? N1 Cd1 O16 90.4(2) . . ? O3 Cd1 O16 175.1(2) . . ? O2 Cd1 O16 86.01(18) . . ? N2 Cd1 O1 84.0(2) . . ? N1 Cd1 O1 84.9(2) . . ? O3 Cd1 O1 85.21(17) . . ? O2 Cd1 O1 177.0(2) . . ? O16 Cd1 O1 91.97(17) . . ? O4 S1 O5 113.2(5) . . ? O4 S1 O3 114.2(4) . . ? O5 S1 O3 111.7(4) . . ? O4 S1 C1 107.2(4) . . ? O5 S1 C1 105.1(3) . . ? O3 S1 C1 104.6(3) . . ? C15 N1 C9 105.4(6) . . ? C15 N1 Cd1 122.5(6) . . ? C9 N1 Cd1 132.1(5) . . ? C6 C1 C2 119.6(5) . . ? C6 C1 S1 120.7(5) . . ? C2 C1 S1 119.6(4) . . ? N6 Cd2 N5 166.8(2) . . ? N6 Cd2 O13 94.6(2) . 4_565 ? N5 Cd2 O13 97.5(2) . 4_565 ? N6 Cd2 O11 80.4(2) . . ? N5 Cd2 O11 87.7(2) . . ? O13 Cd2 O11 130.13(17) 4_565 . ? N6 Cd2 O10 87.6(2) . . ? N5 Cd2 O10 86.3(2) . . ? O13 Cd2 O10 141.31(16) 4_565 . ? O11 Cd2 O10 88.38(17) . . ? N6 Cd2 O17 90.0(2) . . ? N5 Cd2 O17 95.8(2) . . ? O13 Cd2 O17 87.28(16) 4_565 . ? O11 Cd2 O17 141.75(17) . . ? O10 Cd2 O17 54.06(15) . . ? N6 Cd2 O12 97.8(2) . 4_565 ? N5 Cd2 O12 85.4(2) . 4_565 ? O13 Cd2 O12 52.84(15) 4_565 4_565 ? O11 Cd2 O12 78.50(16) . 4_565 ? O10 Cd2 O12 164.70(16) . 4_565 ? O17 Cd2 O12 139.71(15) . 4_565 ? N6 Cd2 C69 88.0(2) . . ? N5 Cd2 C69 91.9(2) . . ? O13 Cd2 C69 114.26(19) 4_565 . ? O11 Cd2 C69 115.09(19) . . ? O10 Cd2 C69 27.10(17) . . ? O17 Cd2 C69 26.98(17) . . ? O12 Cd2 C69 166.07(19) 4_565 . ? N6 Cd2 C70 96.8(2) . 4_565 ? N5 Cd2 C70 91.8(2) . 4_565 ? O13 Cd2 C70 26.20(18) 4_565 4_565 ? O11 Cd2 C70 104.58(19) . 4_565 ? O10 Cd2 C70 166.82(19) . 4_565 ? O17 Cd2 C70 113.33(18) . 4_565 ? O12 Cd2 C70 26.64(17) 4_565 4_565 ? C69 Cd2 C70 140.3(2) . 4_565 ? O16 S2 O14 113.0(4) . . ? O16 S2 O15 112.1(4) . . ? O14 S2 O15 114.7(4) . . ? O16 S2 C63 105.0(3) . . ? O14 S2 C63 104.9(4) . . ? O15 S2 C63 106.1(3) . . ? C51 N2 C45 104.8(6) . . ? C51 N2 Cd1 122.5(5) . . ? C45 N2 Cd1 132.7(5) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? O6 Cd3 N9 89.2(2) . 2_664 ? O6 Cd3 N10 98.3(2) . 1_545 ? N9 Cd3 N10 172.3(2) 2_664 1_545 ? O6 Cd3 O19 86.79(18) . . ? N9 Cd3 O19 97.2(2) 2_664 . ? N10 Cd3 O19 81.7(2) 1_545 . ? O6 Cd3 O9 167.19(17) . 4_455 ? N9 Cd3 O9 85.3(2) 2_664 4_455 ? N10 Cd3 O9 87.0(2) 1_545 4_455 ? O19 Cd3 O9 82.42(17) . 4_455 ? O6 Cd3 O8 137.92(15) . 4_455 ? N9 Cd3 O8 86.5(2) 2_664 4_455 ? N10 Cd3 O8 89.0(2) 1_545 4_455 ? O19 Cd3 O8 135.28(17) . 4_455 ? O9 Cd3 O8 53.35(14) 4_455 4_455 ? O6 Cd3 O7 53.84(15) . . ? N9 Cd3 O7 84.0(2) 2_664 . ? N10 Cd3 O7 101.8(2) 1_545 . ? O19 Cd3 O7 140.63(17) . . ? O9 Cd3 O7 136.62(14) 4_455 . ? O8 Cd3 O7 84.09(14) 4_455 . ? O6 Cd3 C7 163.91(16) . 4_455 ? N9 Cd3 C7 86.0(2) 2_664 4_455 ? N10 Cd3 C7 87.1(2) 1_545 4_455 ? O19 Cd3 C7 109.04(18) . 4_455 ? O9 Cd3 C7 26.90(15) 4_455 4_455 ? O8 Cd3 C7 26.46(16) 4_455 4_455 ? O7 Cd3 C7 110.30(15) . 4_455 ? O6 Cd3 C8 26.67(17) . . ? N9 Cd3 C8 85.3(2) 2_664 . ? N10 Cd3 C8 102.1(2) 1_545 . ? O19 Cd3 C8 113.45(19) . . ? O9 Cd3 C8 162.51(17) 4_455 . ? O8 Cd3 C8 111.27(17) 4_455 . ? O7 Cd3 C8 27.20(16) . . ? C7 Cd3 C8 137.36(17) 4_455 . ? S1 O3 Cd1 151.0(4) . . ? C15 N3 C14 107.8(6) . . ? C15 N3 C16 126.7(8) . . ? C14 N3 C16 125.4(7) . . ? C4 C3 C2 117.3(5) . . ? C4 C3 C7 121.2(5) . . ? C2 C3 C7 121.4(5) . . ? C51 N4 C50 107.2(6) . . ? C51 N4 C52 128.3(6) . . ? C50 N4 C52 124.5(6) . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C33 N5 C32 105.6(6) . . ? C33 N5 Cd2 127.0(5) . . ? C32 N5 Cd2 127.3(5) . . ? C6 C5 C4 119.3(5) . . ? C6 C5 C8 120.9(5) . . ? C4 C5 C8 119.8(5) . . ? C8 O6 Cd3 98.2(4) . . ? C62 N6 C57 105.2(7) . . ? C62 N6 Cd2 125.6(6) . . ? C57 N6 Cd2 129.2(5) . . ? C1 C6 C5 121.5(6) . . ? C1 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C8 O7 Cd3 86.1(3) . . ? C33 N7 C27 105.0(6) . . ? C33 N7 C34 128.5(7) . . ? C27 N7 C34 126.3(7) . . ? O8 C7 O9 122.2(6) . . ? O8 C7 C3 119.2(5) . . ? O9 C7 C3 118.5(5) . . ? O8 C7 Cd3 61.6(3) . 4 ? O9 C7 Cd3 60.6(3) . 4 ? C3 C7 Cd3 175.7(5) . 4 ? C7 O8 Cd3 91.9(4) . 4 ? C62 N8 C56 108.1(7) . . ? C62 N8 C55 124.6(9) . . ? C56 N8 C55 127.2(8) . . ? O6 C8 O7 121.7(5) . . ? O6 C8 C5 119.1(5) . . ? O7 C8 C5 119.2(5) . . ? O6 C8 Cd3 55.1(3) . . ? O7 C8 Cd3 66.7(3) . . ? C5 C8 Cd3 173.0(4) . . ? C7 O9 Cd3 92.5(3) . 4 ? C26 N9 C21 105.5(7) . . ? C26 N9 Cd3 119.2(6) . 2_665 ? C21 N9 Cd3 135.1(5) . 2_665 ? C10 C9 N1 132.9(7) . . ? C10 C9 C14 119.3(7) . . ? N1 C9 C14 107.7(6) . . ? C69 O10 Cd2 92.1(4) . . ? C44 N10 C39 104.5(6) . . ? C44 N10 Cd3 123.2(5) . 1_565 ? C39 N10 Cd3 131.8(5) . 1_565 ? C9 C10 C11 118.7(8) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C20 N11 C26 108.6(7) . . ? C20 N11 C19 124.3(7) . . ? C26 N11 C19 127.1(7) . . ? C12 C11 C10 122.4(9) . . ? C12 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? C70 O12 Cd2 89.5(4) . 4_465 ? C44 N12 C38 106.8(6) . . ? C44 N12 C37 130.7(6) . . ? C38 N12 C37 122.5(6) . . ? C13 C12 C11 120.8(9) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C70 O13 Cd2 95.0(4) . 4_465 ? C12 C13 C14 117.3(8) . . ? C12 C13 H13A 121.4 . . ? C14 C13 H13A 121.4 . . ? N3 C14 C13 132.2(7) . . ? N3 C14 C9 106.2(6) . . ? C13 C14 C9 121.5(7) . . ? N1 C15 N3 112.7(8) . . ? N1 C15 H15A 123.6 . . ? N3 C15 H15A 123.7 . . ? S2 O16 Cd1 142.0(3) . . ? N3 C16 C17 112.6(7) . . ? N3 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N3 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C69 O17 Cd2 91.2(4) . . ? C16 C17 C18 109.5(7) . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 111.2(8) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 N11 113.9(8) . . ? C18 C19 H19A 108.8 . . ? N11 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? N11 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N11 C20 C25 133.7(8) . . ? N11 C20 C21 105.9(7) . . ? C25 C20 C21 120.3(8) . . ? N9 C21 C22 132.0(8) . . ? N9 C21 C20 107.7(6) . . ? C22 C21 C20 120.3(8) . . ? C23 C22 C21 117.8(9) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C22 C23 C24 121.3(8) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C25 C24 C23 122.0(8) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C24 C25 C20 118.2(9) . . ? C24 C25 H25A 120.9 . . ? C20 C25 H25A 120.9 . . ? N9 C26 N11 112.2(7) . . ? N9 C26 H26A 123.9 . . ? N11 C26 H26A 123.9 . . ? N7 C27 C32 107.5(7) . . ? N7 C27 C28 130.7(8) . . ? C32 C27 C28 121.8(8) . . ? C29 C28 C27 117.0(9) . . ? C29 C28 H28A 121.5 . . ? C27 C28 H28A 121.5 . . ? C28 C29 C30 120.1(8) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C31 C30 C29 122.5(8) . . ? C31 C30 H30A 118.7 . . ? C29 C30 H30A 118.7 . . ? C30 C31 C32 117.4(8) . . ? C30 C31 H31A 121.3 . . ? C32 C31 H31A 121.3 . . ? C27 C32 N5 108.2(7) . . ? C27 C32 C31 121.1(7) . . ? N5 C32 C31 130.6(7) . . ? N5 C33 N7 113.7(6) . . ? N5 C33 H33A 123.2 . . ? N7 C33 H33A 123.2 . . ? N7 C34 C35 113.4(7) . . ? N7 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? N7 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C36 113.7(7) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 109.5(6) . . ? C37 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? C37 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.2 . . ? N12 C37 C36 113.8(6) . . ? N12 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? N12 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C43 C38 C39 123.3(7) . . ? C43 C38 N12 131.5(7) . . ? C39 C38 N12 105.2(7) . . ? C38 C39 N10 110.0(7) . . ? C38 C39 C40 119.3(7) . . ? N10 C39 C40 130.7(8) . . ? C41 C40 C39 117.1(7) . . ? C41 C40 H40A 121.5 . . ? C39 C40 H40A 121.5 . . ? C40 C41 C42 122.3(7) . . ? C40 C41 H41A 118.9 . . ? C42 C41 H41A 118.9 . . ? C43 C42 C41 120.4(8) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C42 C43 C38 117.6(8) . . ? C42 C43 H43A 121.2 . . ? C38 C43 H43A 121.2 . . ? N10 C44 N12 113.5(6) . . ? N10 C44 H44A 123.2 . . ? N12 C44 H44A 123.2 . . ? C46 C45 C50 120.4(7) . . ? C46 C45 N2 131.2(7) . . ? C50 C45 N2 108.4(6) . . ? C47 C46 C45 117.5(8) . . ? C47 C46 H46A 121.3 . . ? C45 C46 H46A 121.3 . . ? C46 C47 C48 121.8(8) . . ? C46 C47 H47A 119.1 . . ? C48 C47 H47A 119.1 . . ? C49 C48 C47 122.1(8) . . ? C49 C48 H48A 119.0 . . ? C47 C48 H48A 119.0 . . ? C48 C49 C50 116.4(8) . . ? C48 C49 H49A 121.8 . . ? C50 C49 H49A 121.8 . . ? N4 C50 C45 106.1(7) . . ? N4 C50 C49 132.1(8) . . ? C45 C50 C49 121.8(7) . . ? N2 C51 N4 113.4(7) . . ? N2 C51 H51A 123.3 . . ? N4 C51 H51A 123.3 . . ? N4 C52 C53 113.5(7) . . ? N4 C52 H52A 108.9 . . ? C53 C52 H52A 108.9 . . ? N4 C52 H52B 108.9 . . ? C53 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 C54 109.7(7) . . ? C52 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? C52 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C53 C54 C55 111.5(8) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? N8 C55 C54 111.7(8) . . ? N8 C55 H55A 109.3 . . ? C54 C55 H55A 109.3 . . ? N8 C55 H55B 109.3 . . ? C54 C55 H55B 109.3 . . ? H55A C55 H55B 107.9 . . ? C57 C56 N8 105.1(8) . . ? C57 C56 C61 121.2(10) . . ? N8 C56 C61 133.7(10) . . ? N6 C57 C56 111.2(7) . . ? N6 C57 C58 130.2(7) . . ? C56 C57 C58 118.5(7) . . ? C59 C58 C57 117.7(9) . . ? C59 C58 H58A 121.2 . . ? C57 C58 H58A 121.2 . . ? C60 C59 C58 124.0(10) . . ? C60 C59 H59A 118.0 . . ? C58 C59 H59A 118.0 . . ? C61 C60 C59 120.3(10) . . ? C61 C60 H60A 119.9 . . ? C59 C60 H60A 119.9 . . ? C60 C61 C56 118.3(10) . . ? C60 C61 H61A 120.9 . . ? C56 C61 H61A 120.9 . . ? N6 C62 N8 110.4(8) . . ? N6 C62 H62A 124.8 . . ? N8 C62 H62A 124.8 . . ? C68 C63 C64 120.3(6) . . ? C68 C63 S2 117.6(4) . . ? C64 C63 S2 122.0(4) . . ? C63 C64 C65 120.6(5) . . ? C63 C64 H64A 119.7 . . ? C65 C64 H64A 119.7 . . ? C64 C65 C66 120.4(5) . . ? C64 C65 C70 121.9(5) . . ? C66 C65 C70 117.7(5) . . ? C67 C66 C65 120.0(5) . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 118.1(5) . . ? C66 C67 C69 120.4(6) . . ? C68 C67 C69 121.4(5) . . ? C63 C68 C67 120.6(5) . . ? C63 C68 H68A 119.7 . . ? C67 C68 H68A 119.7 . . ? O17 C69 O10 122.5(6) . . ? O17 C69 C67 119.6(6) . . ? O10 C69 C67 117.8(6) . . ? O17 C69 Cd2 61.8(3) . . ? O10 C69 Cd2 60.8(3) . . ? C67 C69 Cd2 177.7(6) . . ? O13 C70 O12 122.7(6) . . ? O13 C70 C65 119.4(6) . . ? O12 C70 C65 117.8(6) . . ? O13 C70 Cd2 58.8(3) . 4_465 ? O12 C70 Cd2 63.9(3) . 4_465 ? C65 C70 Cd2 176.3(5) . 4_465 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.002 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.093 #===END data_hll-2 _database_code_depnum_ccdc_archive 'CCDC 831733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 Co3 N16 O18 S2' _chemical_formula_sum 'C88 H88 Co3 N16 O18 S2' _chemical_formula_weight 1898.65 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/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number No.15 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 45.497(2) _cell_length_b 10.5235(5) _cell_length_c 19.0900(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.9690(10) _cell_angle_gamma 90.00 _cell_volume 9002.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6034 _cell_measurement_theta_min 2.3675 _cell_measurement_theta_max 24.5043 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3916 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28951 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7927 _reflns_number_gt 5990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0531P)^2^+2.7348P] 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 7927 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _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 O2W O 0.0284(2) 0.5464(12) 0.7897(7) 0.308(11) Uani 0.50 1 d P . . O1W O 0.00693(19) 0.3231(8) 0.6852(5) 0.160(4) Uani 0.50 1 d P . . C44 C 0.24143(7) 0.3055(3) 0.98081(17) 0.0455(8) Uani 1 1 d . . . H44A H 0.2511 0.3325 0.9419 0.055 Uiso 1 1 calc R . . H44B H 0.2214 0.2781 0.9608 0.055 Uiso 1 1 calc R . . N4 N 0.13721(5) 1.2720(2) 0.53525(12) 0.0319(5) Uani 1 1 d . . . C15 C 0.15502(6) 1.1904(3) 0.57392(15) 0.0349(7) Uani 1 1 d . . . H15 H 0.1693 1.1429 0.5560 0.042 Uiso 1 1 calc R . . N3 N 0.15066(5) 1.1821(2) 0.64193(12) 0.0381(6) Uani 1 1 d . . . C16 C 0.16446(7) 1.0898(3) 0.69488(17) 0.0500(9) Uani 1 1 d . . . H16A H 0.1693 1.1310 0.7409 0.060 Uiso 1 1 calc R . . H16B H 0.1829 1.0594 0.6820 0.060 Uiso 1 1 calc R . . C45 C 0.14400(8) 0.9783(3) 0.70014(18) 0.0545(9) Uani 1 1 d . . . H45A H 0.1256 1.0099 0.7131 0.065 Uiso 1 1 calc R . . H45B H 0.1534 0.9231 0.7382 0.065 Uiso 1 1 calc R . . Co1 Co 0.0000 -0.01766(5) 0.7500 0.02824(14) Uani 1 2 d S . . O1 O 0.12735(4) 0.50689(17) 0.93712(10) 0.0325(5) Uani 1 1 d . . . N1 N 0.13590(5) 0.6633(2) 0.81588(12) 0.0337(6) Uani 1 1 d . . . C1 C 0.14851(7) 0.6239(3) 0.70764(16) 0.0381(7) Uani 1 1 d . . . Co2 Co 0.139131(7) 0.69745(3) 0.927334(18) 0.02591(11) Uani 1 1 d . . . N2 N 0.12575(5) 0.7125(2) 0.70060(12) 0.0391(6) Uani 1 1 d . . . O2 O 0.07952(4) 0.50883(19) 0.88646(13) 0.0513(6) Uani 1 1 d . . . C2 C 0.15418(6) 0.5907(3) 0.77960(15) 0.0345(7) Uani 1 1 d . . . S3 S 0.166401(15) 0.02849(7) 0.92588(4) 0.03281(18) Uani 1 1 d . . . O3 O 0.05670(4) -0.0720(2) 0.80440(10) 0.0408(5) Uani 1 1 d . . . C3 C 0.17487(7) 0.4963(3) 0.80326(17) 0.0448(8) Uani 1 1 d . . . H3 H 0.1783 0.4699 0.8505 0.054 Uiso 1 1 calc R . . O4 O 0.03170(4) 0.10810(18) 0.78511(10) 0.0377(5) Uani 1 1 d . . . C4 C 0.19023(8) 0.4430(4) 0.75414(19) 0.0564(9) Uani 1 1 d . . . H4 H 0.2042 0.3798 0.7687 0.068 Uiso 1 1 calc R . . N5 N 0.18482(4) 0.6483(2) 0.94976(12) 0.0288(5) Uani 1 1 d . . . C5 C 0.18517(8) 0.4819(4) 0.6835(2) 0.0610(10) Uani 1 1 d . . . H5 H 0.1965 0.4462 0.6524 0.073 Uiso 1 1 calc R . . O5 O 0.15627(4) -0.10350(18) 0.91921(11) 0.0416(5) Uani 1 1 d . . . N6 N 0.22340(5) 0.5239(2) 0.99338(13) 0.0346(6) Uani 1 1 d . . . C6 C 0.16407(8) 0.5710(3) 0.65829(18) 0.0532(9) Uani 1 1 d . . . H6 H 0.1604 0.5949 0.6107 0.064 Uiso 1 1 calc R . . O6 O 0.18466(4) 0.0631(2) 0.87459(12) 0.0493(6) Uani 1 1 d . . . N7 N 0.00752(5) -0.1049(2) 0.66121(13) 0.0371(6) Uani 1 1 d . . . C7 C 0.11961(6) 0.7314(3) 0.76641(15) 0.0374(7) Uani 1 1 d . . . H7 H 0.1051 0.7878 0.7758 0.045 Uiso 1 1 calc R . . O7 O 0.17894(4) 0.0625(2) 0.99802(11) 0.0498(6) Uani 1 1 d . . . N8 N -0.00023(6) -0.2278(3) 0.56499(14) 0.0469(7) Uani 1 1 d . . . C8 C 0.11512(8) 0.7925(3) 0.63843(16) 0.0504(9) Uani 1 1 d . . . H8A H 0.0957 0.8269 0.6422 0.060 Uiso 1 1 calc R . . H8B H 0.1129 0.7410 0.5957 0.060 Uiso 1 1 calc R . . O8 O 0.09155(4) 0.75199(19) 0.90513(10) 0.0377(5) Uani 1 1 d . . . H8C H 0.0808 0.6859 0.8959 0.057 Uiso 1 1 d R . . H8D H 0.0871 0.7890 0.9416 0.057 Uiso 1 1 d R . . C9 C 0.12780(6) 1.2651(3) 0.64872(15) 0.0371(7) Uani 1 1 d . . . C10 C 0.11942(6) 1.3215(3) 0.58180(14) 0.0329(7) Uani 1 1 d . . . C11 C 0.09654(6) 1.4105(3) 0.57127(16) 0.0415(8) Uani 1 1 d . . . H11 H 0.0903 1.4479 0.5270 0.050 Uiso 1 1 calc R . . C12 C 0.08338(7) 1.4414(4) 0.62878(18) 0.0551(9) Uani 1 1 d . . . H12 H 0.0681 1.5011 0.6231 0.066 Uiso 1 1 calc R . . C13 C 0.09239(8) 1.3855(4) 0.69517(18) 0.0600(10) Uani 1 1 d . . . H13 H 0.0831 1.4098 0.7328 0.072 Uiso 1 1 calc R . . C14 C 0.11444(7) 1.2961(3) 0.70645(17) 0.0509(9) Uani 1 1 d . . . H14 H 0.1202 1.2579 0.7506 0.061 Uiso 1 1 calc R . . C18 C 0.23365(6) 0.6073(3) 0.94689(16) 0.0352(7) Uani 1 1 d . . . C19 C 0.20946(6) 0.6851(3) 0.91962(15) 0.0297(6) Uani 1 1 d . . . C20 C 0.21248(6) 0.7764(3) 0.86963(16) 0.0391(7) Uani 1 1 d . . . H20 H 0.1965 0.8281 0.8505 0.047 Uiso 1 1 calc R . . C21 C 0.23978(7) 0.7887(3) 0.84902(19) 0.0530(9) Uani 1 1 d . . . H21 H 0.2423 0.8498 0.8154 0.064 Uiso 1 1 calc R . . C22 C 0.26379(7) 0.7114(3) 0.8776(2) 0.0584(10) Uani 1 1 d . . . H22 H 0.2820 0.7233 0.8628 0.070 Uiso 1 1 calc R . . C23 C 0.26145(6) 0.6191(3) 0.92640(19) 0.0504(9) Uani 1 1 d . . . H23 H 0.2775 0.5671 0.9449 0.061 Uiso 1 1 calc R . . C24 C 0.19451(6) 0.5533(3) 0.99162(15) 0.0330(7) Uani 1 1 d . . . H24 H 0.1824 0.5096 1.0180 0.040 Uiso 1 1 calc R . . C25 C 0.23982(6) 0.4165(3) 1.03043(16) 0.0421(8) Uani 1 1 d . . . H25A H 0.2300 0.3895 1.0692 0.051 Uiso 1 1 calc R . . H25B H 0.2599 0.4436 1.0506 0.051 Uiso 1 1 calc R . . C26 C 0.13173(6) 0.2460(3) 0.91678(14) 0.0297(6) Uani 1 1 d . . . H26 H 0.1485 0.2881 0.9406 0.036 Uiso 1 1 calc R . . C27 C 0.10507(6) 0.3128(3) 0.89491(14) 0.0273(6) Uani 1 1 d . . . C28 C 0.08017(5) 0.2475(3) 0.86039(13) 0.0276(6) Uani 1 1 d . . . H28 H 0.0623 0.2908 0.8468 0.033 Uiso 1 1 calc R . . C29 C 0.08157(5) 0.1191(3) 0.84591(13) 0.0271(6) Uani 1 1 d . . . C30 C 0.10823(6) 0.0547(3) 0.86745(14) 0.0288(6) Uani 1 1 d . . . H30 H 0.1093 -0.0316 0.8578 0.035 Uiso 1 1 calc R . . C31 C 0.13303(5) 0.1169(3) 0.90283(14) 0.0275(6) Uani 1 1 d . . . C32 C 0.10372(6) 0.4540(3) 0.90714(14) 0.0310(6) Uani 1 1 d . . . C33 C 0.05530(6) 0.0452(3) 0.80960(14) 0.0303(6) Uani 1 1 d . . . C36 C 0.02087(7) -0.1393(3) 0.55287(16) 0.0439(8) Uani 1 1 d . . . C37 C 0.02555(6) -0.0622(3) 0.61373(15) 0.0361(7) Uani 1 1 d . . . C38 C 0.04503(7) 0.0398(3) 0.61835(17) 0.0460(8) Uani 1 1 d . . . H38 H 0.0482 0.0921 0.6582 0.055 Uiso 1 1 calc R . . C39 C 0.05946(8) 0.0607(4) 0.56192(19) 0.0594(10) Uani 1 1 d . . . H39 H 0.0728 0.1282 0.5638 0.071 Uiso 1 1 calc R . . C40 C 0.05464(9) -0.0167(4) 0.5019(2) 0.0693(11) Uani 1 1 d . . . H40 H 0.0648 0.0003 0.4648 0.083 Uiso 1 1 calc R . . C41 C 0.03534(8) -0.1170(4) 0.49623(19) 0.0632(11) Uani 1 1 d . . . H41 H 0.0321 -0.1681 0.4559 0.076 Uiso 1 1 calc R . . C42 C -0.00716(6) -0.2028(3) 0.62907(17) 0.0421(8) Uani 1 1 d . . . H42 H -0.0210 -0.2499 0.6489 0.050 Uiso 1 1 calc R . . C43 C -0.01300(8) -0.3310(3) 0.5178(2) 0.0594(10) Uani 1 1 d . . . H43A H -0.0165 -0.3008 0.4691 0.071 Uiso 1 1 calc R . . H43B H -0.0321 -0.3555 0.5298 0.071 Uiso 1 1 calc R . . C46 C 0.00716(8) -0.4454(4) 0.5236(2) 0.0629(11) Uani 1 1 d . . . H46A H 0.0114 -0.4736 0.5727 0.075 Uiso 1 1 calc R . . H46B H 0.0259 -0.4220 0.5095 0.075 Uiso 1 1 calc R . . C47 C 0.13624(8) 0.8998(3) 0.63242(17) 0.0557(9) Uani 1 1 d . . . H47A H 0.1274 0.9551 0.5939 0.067 Uiso 1 1 calc R . . H47B H 0.1545 0.8653 0.6203 0.067 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 O2W 0.187(9) 0.266(13) 0.378(16) -0.247(13) -0.216(11) 0.185(10) O1W 0.147(7) 0.084(6) 0.250(11) 0.057(6) 0.036(7) -0.010(5) C44 0.0450(18) 0.034(2) 0.055(2) 0.0068(16) 0.0023(15) 0.0098(14) N4 0.0293(12) 0.0320(15) 0.0344(13) 0.0056(11) 0.0059(10) 0.0021(10) C15 0.0337(15) 0.0339(19) 0.0380(16) 0.0038(14) 0.0082(13) -0.0026(13) N3 0.0443(14) 0.0355(16) 0.0341(14) 0.0094(11) 0.0056(11) 0.0000(12) C16 0.055(2) 0.046(2) 0.0457(19) 0.0183(16) -0.0005(15) -0.0012(16) C45 0.074(2) 0.043(2) 0.0445(19) 0.0131(17) 0.0044(17) -0.0013(18) Co1 0.0284(3) 0.0239(3) 0.0315(3) 0.000 0.0029(2) 0.000 O1 0.0339(11) 0.0214(11) 0.0406(11) -0.0019(9) 0.0024(9) -0.0035(8) N1 0.0391(13) 0.0282(14) 0.0341(13) 0.0000(11) 0.0067(11) 0.0035(11) C1 0.0477(18) 0.0293(18) 0.0384(17) -0.0035(14) 0.0107(14) -0.0035(14) Co2 0.0255(2) 0.0217(2) 0.0306(2) -0.00160(16) 0.00530(15) 0.00171(15) N2 0.0512(15) 0.0314(16) 0.0351(14) 0.0029(11) 0.0082(11) 0.0036(12) O2 0.0346(12) 0.0275(13) 0.0858(17) -0.0080(11) -0.0068(11) 0.0054(9) C2 0.0402(16) 0.0258(17) 0.0378(16) -0.0053(13) 0.0074(13) -0.0007(13) S3 0.0266(4) 0.0255(4) 0.0450(4) 0.0035(3) 0.0027(3) 0.0038(3) O3 0.0404(12) 0.0259(12) 0.0527(13) -0.0048(10) -0.0015(10) -0.0053(9) C3 0.053(2) 0.037(2) 0.0430(18) -0.0062(15) 0.0054(15) 0.0044(15) O4 0.0294(10) 0.0334(13) 0.0455(12) 0.0015(9) -0.0071(9) -0.0015(9) C4 0.058(2) 0.048(2) 0.062(2) -0.0121(19) 0.0073(18) 0.0159(17) N5 0.0270(12) 0.0248(13) 0.0344(13) 0.0025(11) 0.0053(10) 0.0034(10) C5 0.069(3) 0.062(3) 0.056(2) -0.016(2) 0.0242(19) 0.009(2) O5 0.0383(11) 0.0200(12) 0.0657(14) 0.0043(10) 0.0069(10) 0.0040(9) N6 0.0313(13) 0.0267(14) 0.0454(15) 0.0048(11) 0.0050(11) 0.0056(10) C6 0.073(2) 0.047(2) 0.0439(19) -0.0059(17) 0.0228(17) 0.0033(19) O6 0.0380(12) 0.0458(14) 0.0680(15) 0.0119(12) 0.0200(11) 0.0045(10) N7 0.0377(14) 0.0307(16) 0.0431(14) -0.0071(12) 0.0074(11) -0.0061(11) C7 0.0440(17) 0.0327(19) 0.0366(17) -0.0025(14) 0.0098(14) 0.0015(14) O7 0.0443(12) 0.0490(15) 0.0493(13) -0.0035(11) -0.0110(10) 0.0090(11) N8 0.0493(16) 0.0408(18) 0.0492(16) -0.0208(13) 0.0046(13) -0.0008(13) C8 0.070(2) 0.042(2) 0.0364(17) 0.0042(15) 0.0029(16) 0.0008(17) O8 0.0340(11) 0.0309(12) 0.0484(12) -0.0067(10) 0.0074(9) -0.0020(9) C9 0.0384(16) 0.0385(19) 0.0347(16) 0.0045(14) 0.0074(13) -0.0040(14) C10 0.0318(15) 0.0328(18) 0.0348(16) 0.0011(13) 0.0078(12) -0.0050(12) C11 0.0370(17) 0.048(2) 0.0401(17) 0.0040(15) 0.0094(13) 0.0046(14) C12 0.046(2) 0.068(3) 0.053(2) 0.0006(19) 0.0131(16) 0.0145(17) C13 0.060(2) 0.080(3) 0.045(2) 0.0017(19) 0.0244(17) 0.005(2) C14 0.057(2) 0.062(3) 0.0367(18) 0.0088(16) 0.0152(15) -0.0013(18) C18 0.0291(15) 0.0285(18) 0.0480(18) 0.0023(14) 0.0067(13) 0.0025(12) C19 0.0278(14) 0.0226(16) 0.0391(16) -0.0004(13) 0.0074(12) 0.0014(11) C20 0.0361(16) 0.0320(19) 0.0506(19) 0.0075(15) 0.0110(14) 0.0063(13) C21 0.051(2) 0.040(2) 0.074(2) 0.0186(18) 0.0262(18) 0.0029(16) C22 0.0380(18) 0.049(2) 0.095(3) 0.014(2) 0.0314(18) 0.0002(16) C23 0.0283(16) 0.040(2) 0.084(3) 0.0103(19) 0.0127(16) 0.0064(14) C24 0.0309(15) 0.0314(18) 0.0381(16) 0.0001(14) 0.0098(12) 0.0015(13) C25 0.0368(16) 0.0353(19) 0.0510(19) 0.0117(15) -0.0015(14) 0.0104(14) C26 0.0269(14) 0.0261(16) 0.0347(15) 0.0004(13) 0.0016(11) -0.0026(11) C27 0.0303(14) 0.0207(16) 0.0315(14) -0.0002(12) 0.0069(11) 0.0003(11) C28 0.0243(14) 0.0264(16) 0.0318(15) 0.0022(12) 0.0041(11) 0.0019(11) C29 0.0270(14) 0.0234(16) 0.0303(14) -0.0005(12) 0.0030(11) -0.0018(11) C30 0.0330(15) 0.0183(15) 0.0351(15) -0.0012(12) 0.0061(12) -0.0004(11) C31 0.0273(14) 0.0230(16) 0.0309(14) 0.0000(12) 0.0016(11) 0.0022(11) C32 0.0342(16) 0.0226(16) 0.0363(16) -0.0009(13) 0.0065(12) -0.0011(12) C33 0.0301(15) 0.0309(18) 0.0289(15) 0.0006(13) 0.0021(12) -0.0046(12) C36 0.0471(18) 0.040(2) 0.0436(18) -0.0092(15) 0.0061(15) 0.0039(15) C37 0.0369(16) 0.0364(19) 0.0351(16) -0.0044(14) 0.0065(13) 0.0013(14) C38 0.0501(19) 0.046(2) 0.0422(18) -0.0053(16) 0.0100(15) -0.0064(16) C39 0.064(2) 0.057(3) 0.062(2) 0.002(2) 0.0237(19) -0.0122(19) C40 0.077(3) 0.081(3) 0.057(2) 0.002(2) 0.035(2) -0.002(2) C41 0.073(3) 0.076(3) 0.045(2) -0.017(2) 0.0209(19) 0.003(2) C42 0.0377(17) 0.0349(19) 0.054(2) -0.0060(16) 0.0094(14) -0.0033(14) C43 0.059(2) 0.046(2) 0.067(2) -0.0286(19) -0.0067(18) 0.0031(17) C46 0.062(2) 0.054(3) 0.066(2) -0.027(2) -0.0079(18) 0.0094(19) C47 0.077(3) 0.047(2) 0.0428(19) 0.0146(17) 0.0103(17) 0.0005(18) _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 C44 C25 1.514(4) . ? C44 C44 1.520(6) 7_557 ? N4 C15 1.316(3) . ? N4 C10 1.402(3) . ? N4 Co2 2.102(2) 6_575 ? C15 N3 1.350(4) . ? N3 C9 1.381(4) . ? N3 C16 1.463(4) . ? C16 C45 1.512(5) . ? C45 C47 1.523(5) . ? Co1 O4 1.9865(18) . ? Co1 O4 1.9865(18) 2_556 ? Co1 N7 2.008(2) . ? Co1 N7 2.008(2) 2_556 ? O1 C32 1.257(3) . ? O1 Co2 2.0925(18) . ? N1 C7 1.309(4) . ? N1 C2 1.398(4) . ? N1 Co2 2.138(2) . ? C1 N2 1.383(4) . ? C1 C6 1.389(4) . ? C1 C2 1.398(4) . ? Co2 N4 2.102(2) 6_576 ? Co2 N5 2.113(2) . ? Co2 O8 2.2085(18) . ? Co2 O5 2.2498(19) 1_565 ? N2 C7 1.348(4) . ? N2 C8 1.467(4) . ? O2 C32 1.245(3) . ? C2 C3 1.389(4) . ? S3 O6 1.436(2) . ? S3 O7 1.441(2) . ? S3 O5 1.462(2) . ? S3 C31 1.770(3) . ? O3 C33 1.240(3) . ? C3 C4 1.382(4) . ? O4 C33 1.279(3) . ? C4 C5 1.389(5) . ? N5 C24 1.308(3) . ? N5 C19 1.400(3) . ? C5 C6 1.369(5) . ? O5 Co2 2.2498(19) 1_545 ? N6 C24 1.345(3) . ? N6 C18 1.386(4) . ? N6 C25 1.467(3) . ? N7 C42 1.320(4) . ? N7 C37 1.398(4) . ? N8 C42 1.341(4) . ? N8 C36 1.385(4) . ? N8 C43 1.465(4) . ? C8 C47 1.499(5) . ? C9 C14 1.387(4) . ? C9 C10 1.400(4) . ? C10 C11 1.389(4) . ? C11 C12 1.377(4) . ? C12 C13 1.393(5) . ? C13 C14 1.365(5) . ? C18 C23 1.393(4) . ? C18 C19 1.398(4) . ? C19 C20 1.378(4) . ? C20 C21 1.372(4) . ? C21 C22 1.395(4) . ? C22 C23 1.363(5) . ? C26 C31 1.388(4) . ? C26 C27 1.401(4) . ? C27 C28 1.390(4) . ? C27 C32 1.507(4) . ? C28 C29 1.383(4) . ? C29 C30 1.388(4) . ? C29 C33 1.492(3) . ? C30 C31 1.376(3) . ? C36 C41 1.380(5) . ? C36 C37 1.403(4) . ? C37 C38 1.385(4) . ? C38 C39 1.373(4) . ? C39 C40 1.392(5) . ? C40 C41 1.365(5) . ? C43 C46 1.506(5) . ? C46 C46 1.535(6) 5_546 ? 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 C25 C44 C44 111.6(3) . 7_557 ? C15 N4 C10 104.7(2) . . ? C15 N4 Co2 121.57(19) . 6_575 ? C10 N4 Co2 133.71(18) . 6_575 ? N4 C15 N3 113.8(3) . . ? C15 N3 C9 106.7(2) . . ? C15 N3 C16 126.2(3) . . ? C9 N3 C16 126.5(3) . . ? N3 C16 C45 111.4(3) . . ? C16 C45 C47 114.8(3) . . ? O4 Co1 O4 96.44(11) . 2_556 ? O4 Co1 N7 111.68(9) . . ? O4 Co1 N7 103.86(9) 2_556 . ? O4 Co1 N7 103.86(9) . 2_556 ? O4 Co1 N7 111.68(9) 2_556 2_556 ? N7 Co1 N7 125.61(14) . 2_556 ? C32 O1 Co2 126.57(18) . . ? C7 N1 C2 104.7(2) . . ? C7 N1 Co2 124.0(2) . . ? C2 N1 Co2 129.86(18) . . ? N2 C1 C6 131.7(3) . . ? N2 C1 C2 105.8(2) . . ? C6 C1 C2 122.5(3) . . ? O1 Co2 N4 90.24(8) . 6_576 ? O1 Co2 N5 90.31(8) . . ? N4 Co2 N5 92.59(8) 6_576 . ? O1 Co2 N1 87.31(8) . . ? N4 Co2 N1 173.71(8) 6_576 . ? N5 Co2 N1 93.21(9) . . ? O1 Co2 O8 90.48(7) . . ? N4 Co2 O8 86.72(8) 6_576 . ? N5 Co2 O8 178.95(8) . . ? N1 Co2 O8 87.51(8) . . ? O1 Co2 O5 174.66(7) . 1_565 ? N4 Co2 O5 89.94(9) 6_576 1_565 ? N5 Co2 O5 84.35(8) . 1_565 ? N1 Co2 O5 93.04(9) . 1_565 ? O8 Co2 O5 94.86(7) . 1_565 ? C7 N2 C1 106.3(2) . . ? C7 N2 C8 125.2(3) . . ? C1 N2 C8 127.0(3) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 N1 131.1(3) . . ? C1 C2 N1 109.0(2) . . ? O6 S3 O7 114.12(14) . . ? O6 S3 O5 113.09(13) . . ? O7 S3 O5 112.68(13) . . ? O6 S3 C31 105.65(13) . . ? O7 S3 C31 106.71(12) . . ? O5 S3 C31 103.53(12) . . ? C4 C3 C2 117.6(3) . . ? C33 O4 Co1 107.03(18) . . ? C3 C4 C5 121.4(3) . . ? C24 N5 C19 104.7(2) . . ? C24 N5 Co2 121.80(18) . . ? C19 N5 Co2 132.71(18) . . ? C6 C5 C4 122.1(3) . . ? S3 O5 Co2 170.51(14) . 1_545 ? C24 N6 C18 105.9(2) . . ? C24 N6 C25 127.1(2) . . ? C18 N6 C25 126.7(2) . . ? C5 C6 C1 116.4(3) . . ? C42 N7 C37 104.8(2) . . ? C42 N7 Co1 127.1(2) . . ? C37 N7 Co1 127.25(19) . . ? N1 C7 N2 114.2(3) . . ? C42 N8 C36 107.4(2) . . ? C42 N8 C43 125.1(3) . . ? C36 N8 C43 127.5(3) . . ? N2 C8 C47 111.6(3) . . ? N3 C9 C14 131.6(3) . . ? N3 C9 C10 105.8(2) . . ? C14 C9 C10 122.5(3) . . ? C11 C10 C9 119.8(3) . . ? C11 C10 N4 131.3(3) . . ? C9 C10 N4 109.0(2) . . ? C12 C11 C10 117.5(3) . . ? C11 C12 C13 121.7(3) . . ? C14 C13 C12 121.8(3) . . ? C13 C14 C9 116.6(3) . . ? N6 C18 C23 131.2(3) . . ? N6 C18 C19 106.2(2) . . ? C23 C18 C19 122.6(3) . . ? C20 C19 C18 120.0(3) . . ? C20 C19 N5 131.3(2) . . ? C18 C19 N5 108.6(2) . . ? C21 C20 C19 117.9(3) . . ? C20 C21 C22 121.3(3) . . ? C23 C22 C21 122.3(3) . . ? C22 C23 C18 115.9(3) . . ? N5 C24 N6 114.6(3) . . ? N6 C25 C44 111.6(2) . . ? C31 C26 C27 119.8(2) . . ? C28 C27 C26 119.1(3) . . ? C28 C27 C32 120.6(2) . . ? C26 C27 C32 120.3(2) . . ? C29 C28 C27 121.1(2) . . ? C28 C29 C30 119.0(2) . . ? C28 C29 C33 122.8(2) . . ? C30 C29 C33 118.2(2) . . ? C31 C30 C29 120.9(3) . . ? C30 C31 C26 120.1(2) . . ? C30 C31 S3 117.8(2) . . ? C26 C31 S3 122.02(19) . . ? O2 C32 O1 125.4(3) . . ? O2 C32 C27 117.7(2) . . ? O1 C32 C27 116.9(2) . . ? O3 C33 O4 122.5(2) . . ? O3 C33 C29 120.5(2) . . ? O4 C33 C29 117.0(3) . . ? C41 C36 N8 133.1(3) . . ? C41 C36 C37 121.7(3) . . ? N8 C36 C37 105.1(3) . . ? C38 C37 N7 130.4(3) . . ? C38 C37 C36 120.3(3) . . ? N7 C37 C36 109.2(3) . . ? C39 C38 C37 117.5(3) . . ? C38 C39 C40 121.5(4) . . ? C41 C40 C39 121.7(4) . . ? C40 C41 C36 117.2(3) . . ? N7 C42 N8 113.4(3) . . ? N8 C43 C46 112.1(3) . . ? C43 C46 C46 111.4(3) . 5_546 ? C8 C47 C45 113.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.505 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.058 data_hll-1 _database_code_depnum_ccdc_archive 'CCDC 831734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Co N4 O5' _chemical_formula_sum 'C26 H24 Co N4 O5' _chemical_formula_weight 531.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number No.11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.3568(8) _cell_length_b 15.2796(14) _cell_length_c 9.5459(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.5170(10) _cell_angle_gamma 90.00 _cell_volume 1221.19(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2998 _cell_measurement_theta_min 2.3844 _cell_measurement_theta_max 25.288 _exptl_crystal_description blcok _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546.9 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7736 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2229 _reflns_number_gt 1940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0422P)^2^+0.2646P] 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 2229 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.90904(4) 0.2500 0.01846(4) 0.03705(14) Uani 1 2 d S . . O1 O 0.8123(2) 0.2500 0.1612(2) 0.0506(5) Uani 1 2 d S . . O2 O 0.5611(3) 0.2500 -0.0128(2) 0.0875(10) Uani 1 2 d S . . O3 O 0.7596(3) 0.2500 0.7990(2) 0.0589(6) Uani 1 2 d S . . O4 O 0.9558(3) 0.2500 0.7300(2) 0.0660(7) Uani 1 2 d S . . N1 N 1.04635(19) 0.14115(11) 0.07499(18) 0.0422(4) Uani 1 1 d . . . N3 N 1.20181(19) 0.03664(11) 0.0561(2) 0.0466(4) Uani 1 1 d . . . C1 C 1.1049(2) 0.10393(14) -0.0132(2) 0.0451(5) Uani 1 1 d . . . H1 H 1.0809 0.1228 -0.1140 0.054 Uiso 1 1 calc R . . C2 C 1.1117(2) 0.09357(13) 0.2154(2) 0.0425(5) Uani 1 1 d . . . C3 C 1.0932(3) 0.10334(15) 0.3504(3) 0.0546(6) Uani 1 1 d . . . H3 H 1.0277 0.1466 0.3594 0.066 Uiso 1 1 calc R . . C4 C 1.1762(3) 0.04596(18) 0.4709(3) 0.0712(7) Uani 1 1 d . . . H4 H 1.1668 0.0509 0.5636 0.085 Uiso 1 1 calc R . . C5 C 1.2743(3) -0.01935(18) 0.4582(3) 0.0736(8) Uani 1 1 d . . . H5 H 1.3276 -0.0570 0.5421 0.088 Uiso 1 1 calc R . . C6 C 1.2938(3) -0.02938(15) 0.3259(3) 0.0618(6) Uani 1 1 d . . . H6 H 1.3595 -0.0727 0.3177 0.074 Uiso 1 1 calc R . . C7 C 1.2106(2) 0.02831(13) 0.2043(2) 0.0456(5) Uani 1 1 d . . . C8 C 1.2921(3) -0.01377(16) -0.0090(3) 0.0579(6) Uani 1 1 d . . . H8A H 1.2328 -0.0150 -0.1222 0.069 Uiso 1 1 calc R . . H8B H 1.3038 -0.0736 0.0286 0.069 Uiso 1 1 calc R . . C9 C 1.4547(3) 0.02480(15) 0.0364(3) 0.0553(6) Uani 1 1 d . . . H9A H 1.5156 0.0237 0.1494 0.066 Uiso 1 1 calc R . . H9B H 1.4431 0.0854 0.0029 0.066 Uiso 1 1 calc R . . C19 C 0.6634(3) 0.2500 0.1221(3) 0.0373(6) Uani 1 2 d S . . C20 C 0.6178(3) 0.2500 0.2539(3) 0.0327(6) Uani 1 2 d S . . C21 C 0.7321(3) 0.2500 0.4091(3) 0.0336(6) Uani 1 2 d S . . H21 H 0.8398 0.2500 0.4325 0.040 Uiso 1 2 calc SR . . C22 C 0.6880(3) 0.2500 0.5299(3) 0.0358(6) Uani 1 2 d S . . C23 C 0.5270(3) 0.2500 0.4946(3) 0.0397(6) Uani 1 2 d S . . H23 H 0.4963 0.2500 0.5748 0.048 Uiso 1 2 calc SR . . C24 C 0.4126(3) 0.2500 0.3406(3) 0.0427(7) Uani 1 2 d S . . H24 H 0.3049 0.2500 0.3173 0.051 Uiso 1 2 calc SR . . C25 C 0.4570(3) 0.2500 0.2212(3) 0.0403(6) Uani 1 2 d S . . H25 H 0.3789 0.2500 0.1177 0.048 Uiso 1 2 calc SR . . C26 C 0.8123(4) 0.2500 0.6967(3) 0.0472(7) Uani 1 2 d S . . O1W O 0.2616(6) 0.2016(4) 0.7466(7) 0.141(2) Uani 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0338(2) 0.0519(2) 0.0312(2) 0.000 0.01973(16) 0.000 O1 0.0385(12) 0.0844(15) 0.0367(10) 0.000 0.0238(9) 0.000 O2 0.0505(14) 0.183(3) 0.0313(12) 0.000 0.0201(11) 0.000 O3 0.0585(14) 0.0936(17) 0.0299(10) 0.000 0.0245(10) 0.000 O4 0.0420(13) 0.1095(19) 0.0406(12) 0.000 0.0132(10) 0.000 N1 0.0383(9) 0.0518(10) 0.0413(9) -0.0016(8) 0.0222(7) 0.0008(7) N3 0.0367(9) 0.0522(10) 0.0560(10) -0.0094(9) 0.0253(8) 0.0000(8) C1 0.0381(11) 0.0578(12) 0.0442(11) -0.0046(9) 0.0228(9) 0.0008(9) C2 0.0366(10) 0.0471(11) 0.0439(11) -0.0016(9) 0.0182(9) -0.0053(9) C3 0.0610(14) 0.0607(14) 0.0484(12) -0.0008(11) 0.0301(11) -0.0009(11) C4 0.0891(19) 0.0768(17) 0.0502(14) 0.0083(13) 0.0334(14) -0.0004(16) C5 0.0790(19) 0.0668(17) 0.0623(16) 0.0182(13) 0.0201(14) 0.0030(14) C6 0.0524(14) 0.0519(14) 0.0725(16) 0.0054(12) 0.0202(12) 0.0048(11) C7 0.0353(11) 0.0477(12) 0.0526(12) -0.0043(10) 0.0185(10) -0.0049(9) C8 0.0449(12) 0.0608(14) 0.0754(16) -0.0212(12) 0.0335(12) -0.0026(10) C9 0.0442(12) 0.0590(14) 0.0710(15) -0.0185(11) 0.0332(12) -0.0023(10) C19 0.0405(16) 0.0448(15) 0.0305(14) 0.000 0.0192(12) 0.000 C20 0.0355(14) 0.0353(13) 0.0315(13) 0.000 0.0188(11) 0.000 C21 0.0316(14) 0.0414(14) 0.0323(13) 0.000 0.0184(11) 0.000 C22 0.0384(15) 0.0419(14) 0.0308(13) 0.000 0.0187(12) 0.000 C23 0.0433(16) 0.0489(16) 0.0377(14) 0.000 0.0279(13) 0.000 C24 0.0314(14) 0.0572(17) 0.0462(16) 0.000 0.0233(13) 0.000 C25 0.0342(15) 0.0524(16) 0.0337(14) 0.000 0.0147(12) 0.000 C26 0.0485(19) 0.0597(19) 0.0339(15) 0.000 0.0188(14) 0.000 O1W 0.106(4) 0.174(5) 0.143(5) -0.063(4) 0.055(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.931(2) 1_554 ? Co1 O1 1.9433(19) . ? Co1 N1 2.0221(16) 4_565 ? Co1 N1 2.0221(16) . ? O1 C19 1.271(3) . ? O2 C19 1.214(3) . ? O3 C26 1.276(4) . ? O3 Co1 1.931(2) 1_556 ? O4 C26 1.233(4) . ? N1 C1 1.321(2) . ? N1 C2 1.402(2) . ? N3 C1 1.335(3) . ? N3 C7 1.386(3) . ? N3 C8 1.470(3) . ? C1 H1 0.9300 . ? C2 C3 1.384(3) . ? C2 C7 1.396(3) . ? C3 C4 1.378(3) . ? C3 H3 0.9300 . ? C4 C5 1.397(4) . ? C4 H4 0.9300 . ? C5 C6 1.362(4) . ? C5 H5 0.9300 . ? C6 C7 1.387(3) . ? C6 H6 0.9300 . ? C8 C9 1.504(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C9 1.517(4) 3_855 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C19 C20 1.499(4) . ? C20 C21 1.387(3) . ? C20 C25 1.394(4) . ? C21 C22 1.387(4) . ? C21 H21 0.9300 . ? C22 C23 1.389(4) . ? C22 C26 1.495(4) . ? C23 C24 1.379(4) . ? C23 H23 0.9300 . ? C24 C25 1.376(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O1W O1W 1.478(12) 4_565 ? 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 O3 Co1 O1 114.98(9) 1_554 . ? O3 Co1 N1 110.83(5) 1_554 4_565 ? O1 Co1 N1 104.60(6) . 4_565 ? O3 Co1 N1 110.83(5) 1_554 . ? O1 Co1 N1 104.60(6) . . ? N1 Co1 N1 110.67(9) 4_565 . ? C19 O1 Co1 125.90(18) . . ? C26 O3 Co1 119.3(2) . 1_556 ? C1 N1 C2 104.94(17) . . ? C1 N1 Co1 125.37(14) . . ? C2 N1 Co1 129.47(13) . . ? C1 N3 C7 107.12(16) . . ? C1 N3 C8 125.85(19) . . ? C7 N3 C8 126.84(19) . . ? N1 C1 N3 113.51(18) . . ? N1 C1 H1 123.2 . . ? N3 C1 H1 123.2 . . ? C3 C2 C7 120.7(2) . . ? C3 C2 N1 130.66(19) . . ? C7 C2 N1 108.61(18) . . ? C4 C3 C2 116.8(2) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 C5 122.0(2) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.7(2) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 116.6(2) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? N3 C7 C6 131.9(2) . . ? N3 C7 C2 105.82(18) . . ? C6 C7 C2 122.2(2) . . ? N3 C8 C9 111.81(17) . . ? N3 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N3 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C9 111.9(2) . 3_855 ? C8 C9 H9A 109.2 . . ? C9 C9 H9A 109.2 3_855 . ? C8 C9 H9B 109.2 . . ? C9 C9 H9B 109.2 3_855 . ? H9A C9 H9B 107.9 . . ? O2 C19 O1 123.6(3) . . ? O2 C19 C20 120.3(3) . . ? O1 C19 C20 116.1(2) . . ? C21 C20 C25 118.7(2) . . ? C21 C20 C19 121.6(2) . . ? C25 C20 C19 119.7(2) . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 119.4(2) . . ? C21 C22 C26 120.4(2) . . ? C23 C22 C26 120.2(2) . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 120.6(2) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? O4 C26 O3 123.5(3) . . ? O4 C26 C22 121.0(3) . . ? O3 C26 C22 115.6(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.335 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.041