# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email yubindong@yahoo.com _publ_contact_author_name 'Yu-Bin Dong' _publ_author_name 'Yu-Bin Dong' # Attachment '2.cif' data_80718dm _database_code_depnum_ccdc_archive 'CCDC 836119' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 Cd Cl6 N12 O8' _chemical_formula_weight 1262.04 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8591(12) _cell_length_b 15.8591(12) _cell_length_c 21.685(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5454.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3435 _cell_measurement_theta_min 2.275 _cell_measurement_theta_max 19.571 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9012 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28197 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5080 _reflns_number_gt 4410 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1049P)^2^+9.5365P] 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' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 5080 _refine_ls_number_parameters 354 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.133 _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 C1 C 0.4315(6) 0.6979(5) 0.9404(4) 0.0381(19) Uani 1 1 d . . . H1 H 0.4403 0.6598 0.9085 0.046 Uiso 1 1 calc R . . C2 C 0.3743(5) 0.7617(6) 0.9311(4) 0.038(2) Uani 1 1 d . . . H2 H 0.3457 0.7664 0.8938 0.046 Uiso 1 1 calc R . . C3 C 0.3595(5) 0.8195(5) 0.9788(3) 0.0270(17) Uani 1 1 d . . . C4 C 0.4064(5) 0.8097(6) 1.0316(4) 0.038(2) Uani 1 1 d . . . H4 H 0.4008 0.8482 1.0637 0.046 Uiso 1 1 calc R . . C5 C 0.4620(5) 0.7426(5) 1.0374(4) 0.0350(19) Uani 1 1 d . . . H5 H 0.4909 0.7361 1.0744 0.042 Uiso 1 1 calc R . . C6 C 0.2929(5) 0.8857(5) 0.9722(4) 0.0350(19) Uani 1 1 d . . . C7 C 0.2937(6) 0.9592(5) 1.0094(4) 0.046(2) Uani 1 1 d . . . H7 H 0.3373 0.9677 1.0374 0.055 Uiso 1 1 calc R . . C8 C 0.2303(7) 1.0182(6) 1.0044(5) 0.060(3) Uani 1 1 d . . . H8 H 0.2314 1.0659 1.0293 0.072 Uiso 1 1 calc R . . C9 C 0.1657(6) 1.0074(6) 0.9633(4) 0.047(2) Uani 1 1 d . . . H9 H 0.1242 1.0485 0.9593 0.056 Uiso 1 1 calc R . . C10 C 0.1625(5) 0.9339(5) 0.9269(3) 0.0295(16) Uani 1 1 d . . . C11 C 0.2247(5) 0.8752(5) 0.9315(3) 0.0296(17) Uani 1 1 d . . . H11 H 0.2221 0.8271 0.9071 0.036 Uiso 1 1 calc R . . C12 C 0.0927(5) 0.9258(4) 0.8832(3) 0.0264(16) Uani 1 1 d . . . C13 C -0.0022(4) 0.8737(5) 0.8207(3) 0.0260(15) Uani 1 1 d . . . C14 C -0.0582(5) 0.8119(4) 0.7906(3) 0.0275(15) Uani 1 1 d . . . C15 C -0.0400(6) 0.7811(6) 0.7316(3) 0.037(2) Uani 1 1 d . . . H15 H 0.0072 0.7995 0.7101 0.044 Uiso 1 1 calc R . . C16 C -0.0953(7) 0.7217(7) 0.7062(4) 0.051(3) Uani 1 1 d . . . H16 H -0.0859 0.7024 0.6664 0.061 Uiso 1 1 calc R . . C17 C -0.1639(5) 0.6910(5) 0.7392(4) 0.036(2) Uani 1 1 d . . . H17 H -0.1986 0.6502 0.7217 0.043 Uiso 1 1 calc R . . C18 C -0.1809(5) 0.7207(5) 0.7978(3) 0.0290(17) Uani 1 1 d . . . C19 C -0.1274(5) 0.7812(5) 0.8233(3) 0.0303(18) Uani 1 1 d . . . H19 H -0.1381 0.8014 0.8628 0.036 Uiso 1 1 calc R . . C20 C -0.2543(5) 0.6907(5) 0.8353(4) 0.0341(18) Uani 1 1 d . . . C21 C -0.2990(5) 0.6182(5) 0.8204(4) 0.0299(17) Uani 1 1 d . . . H21 H -0.2879 0.5894 0.7840 0.036 Uiso 1 1 calc R . . C22 C -0.3606(5) 0.5894(5) 0.8607(4) 0.0353(19) Uani 1 1 d . . . H22 H -0.3896 0.5405 0.8500 0.042 Uiso 1 1 calc R . . C23 C -0.3429(5) 0.7007(5) 0.9243(4) 0.0334(19) Uani 1 1 d . . . H23 H -0.3601 0.7313 0.9587 0.040 Uiso 1 1 calc R . . C24 C -0.2805(5) 0.7335(5) 0.8878(4) 0.0379(19) Uani 1 1 d . . . H24 H -0.2556 0.7846 0.8983 0.045 Uiso 1 1 calc R . . C25 C 0.0259(12) 0.5345(14) 0.0711(8) 0.280(19) Uiso 0.426(12) 1 d PD A 1 H25A H 0.0403 0.5017 0.0349 0.336 Uiso 0.426(12) 1 calc PR A 1 H25B H 0.0780 0.5590 0.0863 0.336 Uiso 0.426(12) 1 calc PR A 1 C25' C 0.0259(12) 0.5345(14) 0.0711(8) 0.280(19) Uiso 0.574(12) 1 d PD A 2 H25C H 0.0606 0.5709 0.0456 0.336 Uiso 0.574(12) 1 calc PR A 2 H25D H 0.0279 0.4787 0.0528 0.336 Uiso 0.574(12) 1 calc PR A 2 Cd1 Cd 0.55863(3) 0.55863(3) 1.0000 0.0222(2) Uani 1 2 d S . . Cl1 Cl 0.88116(19) 0.88116(19) 0.0000 0.0728(11) Uani 1 2 d SD . . Cl2 Cl 0.2899(3) 0.2512(3) 0.9974(4) 0.0628(19) Uani 0.50 1 d PD . . Cl3 Cl -0.0361(6) 0.6148(6) 0.0476(4) 0.086(3) Uiso 0.426(12) 1 d PD A 1 Cl4 Cl -0.0085(16) 0.4672(14) 0.1247(11) 0.243(11) Uiso 0.426(12) 1 d PD A 1 Cl3' Cl 0.0722(8) 0.5283(8) 0.1409(6) 0.168(5) Uiso 0.574(12) 1 d PD A 2 Cl4' Cl -0.0737(9) 0.5691(13) 0.0656(9) 0.239(8) Uiso 0.574(12) 1 d PD A 2 N1 N 0.4757(4) 0.6873(4) 0.9926(3) 0.0319(15) Uani 1 1 d . . . N2 N 0.0555(4) 0.9895(4) 0.8557(3) 0.0300(14) Uani 1 1 d . . . N3 N -0.0048(4) 0.9567(4) 0.8166(3) 0.0299(15) Uani 1 1 d . . . N4 N 0.0563(4) 0.8527(4) 0.8622(3) 0.0303(14) Uani 1 1 d . . . N5 N 0.0762(5) 0.7704(4) 0.8829(4) 0.061(3) Uani 1 1 d . . . H5A H 0.0648 0.7670 0.9231 0.091 Uiso 1 1 d R . . H5B H 0.0451 0.7330 0.8625 0.091 Uiso 1 1 d R . . N6 N -0.3808(4) 0.6260(4) 0.9127(3) 0.0337(14) Uani 1 1 d . . . O1 O 0.8984(11) 0.8113(12) 0.0316(13) 0.305(18) Uani 1 1 d D . . O2 O 0.869(2) 0.9355(17) 0.0455(8) 0.170(12) Uani 0.50 1 d PDU . . O3 O 0.9448(8) 0.9448(8) 0.0000 0.278(16) Uiso 1 2 d SD . . O4 O 0.2372(8) 0.2386(8) 0.9479(4) 0.122(4) Uani 1 1 d D . . O5 O 0.3561(12) 0.1941(13) 1.004(3) 0.22(2) Uani 0.50 1 d PD . . O6 O 0.3311(6) 0.3311(6) 1.0000 0.120(5) Uani 1 2 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(5) 0.031(4) 0.040(4) -0.009(3) 0.004(4) -0.006(4) C2 0.033(4) 0.045(5) 0.038(5) -0.006(4) -0.014(4) 0.011(4) C3 0.030(4) 0.024(4) 0.027(4) 0.000(3) 0.000(3) -0.002(3) C4 0.035(4) 0.040(5) 0.039(5) -0.014(4) -0.011(4) 0.006(4) C5 0.031(5) 0.039(5) 0.035(4) 0.000(4) -0.008(3) 0.006(4) C6 0.030(4) 0.037(5) 0.038(4) 0.001(4) -0.009(4) 0.001(4) C7 0.059(6) 0.037(5) 0.042(5) -0.013(4) -0.024(4) 0.002(4) C8 0.077(7) 0.044(5) 0.060(6) -0.018(5) -0.029(6) 0.022(5) C9 0.049(6) 0.037(5) 0.054(6) -0.012(4) -0.021(5) 0.019(4) C10 0.032(4) 0.033(4) 0.024(3) 0.001(3) -0.003(3) 0.000(4) C11 0.031(4) 0.026(4) 0.032(4) 0.002(3) -0.005(4) -0.005(3) C12 0.030(4) 0.025(4) 0.024(3) 0.000(3) 0.006(3) 0.001(3) C13 0.017(4) 0.025(4) 0.036(4) 0.008(3) 0.003(3) -0.002(3) C14 0.030(4) 0.024(4) 0.029(4) 0.007(3) -0.013(4) 0.001(4) C15 0.046(5) 0.038(5) 0.026(4) 0.004(3) 0.014(4) -0.003(4) C16 0.066(7) 0.055(6) 0.032(5) -0.007(5) 0.014(5) -0.005(5) C17 0.044(5) 0.031(4) 0.032(5) -0.007(3) 0.002(4) -0.007(4) C18 0.031(4) 0.032(4) 0.025(4) 0.009(3) -0.005(3) -0.008(3) C19 0.033(4) 0.035(4) 0.023(4) -0.007(3) 0.002(3) 0.003(4) C20 0.030(4) 0.042(5) 0.030(4) 0.007(4) -0.005(3) -0.006(4) C21 0.028(4) 0.034(4) 0.028(4) 0.006(3) -0.001(3) -0.006(3) C22 0.032(4) 0.031(4) 0.043(5) 0.000(4) -0.009(4) -0.006(3) C23 0.034(4) 0.033(4) 0.033(4) 0.000(3) 0.000(4) -0.010(3) C24 0.039(5) 0.031(5) 0.044(4) 0.002(4) 0.000(4) -0.014(4) Cd1 0.0197(2) 0.0197(2) 0.0272(3) 0.0013(2) -0.0013(2) -0.0026(3) Cl1 0.0823(18) 0.0823(18) 0.054(2) 0.0013(18) -0.0013(18) -0.017(2) Cl2 0.064(3) 0.068(3) 0.057(3) 0.025(5) -0.022(4) -0.024(3) N1 0.025(3) 0.029(3) 0.041(4) 0.009(3) 0.000(3) 0.000(3) N2 0.029(3) 0.027(3) 0.034(3) 0.003(3) -0.001(3) -0.003(3) N3 0.022(3) 0.029(4) 0.038(4) -0.003(3) -0.006(3) 0.001(3) N4 0.031(3) 0.025(3) 0.035(3) 0.006(3) -0.005(3) -0.002(3) N5 0.078(6) 0.029(4) 0.075(6) 0.025(4) -0.049(5) -0.014(4) N6 0.030(4) 0.033(4) 0.038(4) 0.006(3) -0.007(3) 0.000(3) O1 0.150(14) 0.23(2) 0.53(5) 0.27(3) 0.07(2) 0.062(14) O2 0.24(2) 0.22(2) 0.047(9) -0.084(13) 0.030(13) -0.02(2) O4 0.147(11) 0.151(11) 0.068(6) 0.027(7) -0.032(7) -0.026(8) O5 0.069(15) 0.13(2) 0.48(6) -0.01(3) -0.08(3) -0.042(15) O6 0.099(7) 0.099(7) 0.161(14) -0.021(9) 0.021(9) -0.011(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(11) . ? C1 C2 1.374(12) . ? C1 H1 0.9300 . ? C2 C3 1.401(11) . ? C2 H2 0.9300 . ? C3 C4 1.375(11) . ? C3 C6 1.495(11) . ? C4 C5 1.387(11) . ? C4 H4 0.9300 . ? C5 N1 1.327(10) . ? C5 H5 0.9300 . ? C6 C11 1.405(11) . ? C6 C7 1.418(12) . ? C7 C8 1.377(13) . ? C7 H7 0.9300 . ? C8 C9 1.369(13) . ? C8 H8 0.9300 . ? C9 C10 1.408(11) . ? C9 H9 0.9300 . ? C10 C11 1.360(11) . ? C10 C12 1.463(10) . ? C11 H11 0.9300 . ? C12 N2 1.314(9) . ? C12 N4 1.373(9) . ? C13 N3 1.320(10) . ? C13 N4 1.334(10) . ? C13 C14 1.476(10) . ? C14 C19 1.395(11) . ? C14 C15 1.398(11) . ? C15 C16 1.400(14) . ? C15 H15 0.9300 . ? C16 C17 1.390(13) . ? C16 H16 0.9300 . ? C17 C18 1.382(11) . ? C17 H17 0.9300 . ? C18 C19 1.395(11) . ? C18 C20 1.497(11) . ? C19 H19 0.9300 . ? C20 C24 1.389(12) . ? C20 C21 1.390(11) . ? C21 C22 1.389(11) . ? C21 H21 0.9300 . ? C22 N6 1.308(11) . ? C22 H22 0.9300 . ? C23 N6 1.352(10) . ? C23 C24 1.369(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 Cl4 1.670(10) . ? C25 Cl3 1.687(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? Cd1 N3 2.329(6) 5_546 ? Cd1 N3 2.329(6) 4_455 ? Cd1 N6 2.377(6) 7_567 ? Cd1 N6 2.377(6) 1_655 ? Cd1 N1 2.433(6) . ? Cd1 N1 2.433(6) 7_557 ? Cl1 O2 1.324(14) 7 ? Cl1 O2 1.324(14) . ? Cl1 O1 1.331(12) 7 ? Cl1 O1 1.331(12) . ? Cl1 O3 1.428(18) . ? Cl2 Cl2 0.874(12) 7_557 ? Cl2 O4 1.373(10) . ? Cl2 O5 1.395(17) . ? Cl2 O6 1.426(12) . ? Cl2 O4 1.456(13) 7_557 ? N2 N3 1.380(8) . ? N3 Cd1 2.329(6) 3_554 ? N4 N5 1.416(9) . ? N5 H5A 0.8913 . ? N5 H5B 0.8899 . ? N6 Cd1 2.377(6) 1_455 ? O3 O2 1.57(3) 7 ? O4 Cl2 1.456(13) 7_557 ? O6 Cl2 1.426(12) 7_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.1(7) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 C2 C3 119.0(7) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 116.7(7) . . ? C4 C3 C6 122.8(7) . . ? C2 C3 C6 120.5(7) . . ? C3 C4 C5 120.5(8) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 123.0(7) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C11 C6 C7 117.4(8) . . ? C11 C6 C3 121.4(7) . . ? C7 C6 C3 121.1(7) . . ? C8 C7 C6 120.5(8) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.8(9) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.7(8) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.9(7) . . ? C11 C10 C12 122.5(7) . . ? C9 C10 C12 117.6(7) . . ? C10 C11 C6 121.6(7) . . ? C10 C11 H11 119.2 . . ? C6 C11 H11 119.2 . . ? N2 C12 N4 108.1(6) . . ? N2 C12 C10 124.5(7) . . ? N4 C12 C10 127.4(7) . . ? N3 C13 N4 108.5(7) . . ? N3 C13 C14 127.9(7) . . ? N4 C13 C14 123.4(6) . . ? C19 C14 C15 120.4(7) . . ? C19 C14 C13 118.6(6) . . ? C15 C14 C13 120.9(8) . . ? C14 C15 C16 117.7(8) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 121.6(8) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C18 C17 C16 120.4(8) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 118.7(7) . . ? C17 C18 C20 122.9(7) . . ? C19 C18 C20 118.4(7) . . ? C18 C19 C14 121.1(7) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C24 C20 C21 116.2(7) . . ? C24 C20 C18 121.6(7) . . ? C21 C20 C18 122.2(7) . . ? C22 C21 C20 119.1(8) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? N6 C22 C21 124.6(8) . . ? N6 C22 H22 117.7 . . ? C21 C22 H22 117.7 . . ? N6 C23 C24 123.1(8) . . ? N6 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C23 C24 C20 120.4(8) . . ? C23 C24 H24 119.8 . . ? C20 C24 H24 119.8 . . ? Cl4 C25 Cl3 120.1(14) . . ? Cl4 C25 H25A 107.3 . . ? Cl3 C25 H25A 107.3 . . ? Cl4 C25 H25B 107.3 . . ? Cl3 C25 H25B 107.3 . . ? H25A C25 H25B 106.9 . . ? N3 Cd1 N3 82.9(3) 5_546 4_455 ? N3 Cd1 N6 159.9(2) 5_546 7_567 ? N3 Cd1 N6 88.1(2) 4_455 7_567 ? N3 Cd1 N6 88.1(2) 5_546 1_655 ? N3 Cd1 N6 159.9(2) 4_455 1_655 ? N6 Cd1 N6 105.7(3) 7_567 1_655 ? N3 Cd1 N1 110.1(2) 5_546 . ? N3 Cd1 N1 88.5(2) 4_455 . ? N6 Cd1 N1 87.5(2) 7_567 . ? N6 Cd1 N1 77.8(2) 1_655 . ? N3 Cd1 N1 88.5(2) 5_546 7_557 ? N3 Cd1 N1 110.1(2) 4_455 7_557 ? N6 Cd1 N1 77.8(2) 7_567 7_557 ? N6 Cd1 N1 87.5(2) 1_655 7_557 ? N1 Cd1 N1 155.7(3) . 7_557 ? O2 Cl1 O2 139(3) 7 . ? O2 Cl1 O1 101.0(17) 7 7 ? O2 Cl1 O1 97.1(17) . 7 ? O2 Cl1 O1 97.1(17) 7 . ? O2 Cl1 O1 101.0(17) . . ? O1 Cl1 O1 127(2) 7 . ? O2 Cl1 O3 69.3(13) 7 . ? O2 Cl1 O3 69.3(13) . . ? O1 Cl1 O3 116.3(10) 7 . ? O1 Cl1 O3 116.3(10) . . ? Cl2 Cl2 O4 77.2(10) 7_557 . ? Cl2 Cl2 O5 166(3) 7_557 . ? O4 Cl2 O5 117(2) . . ? Cl2 Cl2 O6 72.2(3) 7_557 . ? O4 Cl2 O6 116.1(7) . . ? O5 Cl2 O6 103.1(9) . . ? Cl2 Cl2 O4 66.9(10) 7_557 7_557 ? O4 Cl2 O4 105.9(9) . 7_557 ? O5 Cl2 O4 104(2) . 7_557 ? O6 Cl2 O4 111.0(7) . 7_557 ? C5 N1 C1 116.7(7) . . ? C5 N1 Cd1 126.5(5) . . ? C1 N1 Cd1 116.3(5) . . ? C12 N2 N3 107.5(6) . . ? C13 N3 N2 108.2(6) . . ? C13 N3 Cd1 138.2(5) . 3_554 ? N2 N3 Cd1 111.9(4) . 3_554 ? C13 N4 C12 107.8(6) . . ? C13 N4 N5 126.9(6) . . ? C12 N4 N5 125.3(6) . . ? N4 N5 H5A 108.8 . . ? N4 N5 H5B 109.4 . . ? H5A N5 H5B 109.6 . . ? C22 N6 C23 116.2(7) . . ? C22 N6 Cd1 125.8(6) . 1_455 ? C23 N6 Cd1 115.2(5) . 1_455 ? Cl1 O3 O2 52.2(9) . 7 ? Cl2 O4 Cl2 35.8(5) . 7_557 ? Cl2 O6 Cl2 35.7(6) . 7_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.6(14) . . . . ? C1 C2 C3 C4 2.1(13) . . . . ? C1 C2 C3 C6 -175.3(8) . . . . ? C2 C3 C4 C5 -3.2(13) . . . . ? C6 C3 C4 C5 174.1(8) . . . . ? C3 C4 C5 N1 2.9(14) . . . . ? C4 C3 C6 C11 -153.8(8) . . . . ? C2 C3 C6 C11 23.4(13) . . . . ? C4 C3 C6 C7 22.6(13) . . . . ? C2 C3 C6 C7 -160.2(9) . . . . ? C11 C6 C7 C8 -1.1(15) . . . . ? C3 C6 C7 C8 -177.7(9) . . . . ? C6 C7 C8 C9 -0.5(18) . . . . ? C7 C8 C9 C10 2.1(17) . . . . ? C8 C9 C10 C11 -2.0(14) . . . . ? C8 C9 C10 C12 -179.4(9) . . . . ? C9 C10 C11 C6 0.4(12) . . . . ? C12 C10 C11 C6 177.6(7) . . . . ? C7 C6 C11 C10 1.2(13) . . . . ? C3 C6 C11 C10 177.7(7) . . . . ? C11 C10 C12 N2 -146.7(8) . . . . ? C9 C10 C12 N2 30.6(11) . . . . ? C11 C10 C12 N4 31.1(12) . . . . ? C9 C10 C12 N4 -151.6(8) . . . . ? N3 C13 C14 C19 -95.3(9) . . . . ? N4 C13 C14 C19 78.4(10) . . . . ? N3 C13 C14 C15 88.1(10) . . . . ? N4 C13 C14 C15 -98.2(9) . . . . ? C19 C14 C15 C16 2.6(12) . . . . ? C13 C14 C15 C16 179.1(8) . . . . ? C14 C15 C16 C17 -3.0(14) . . . . ? C15 C16 C17 C18 2.1(15) . . . . ? C16 C17 C18 C19 -0.7(13) . . . . ? C16 C17 C18 C20 179.4(9) . . . . ? C17 C18 C19 C14 0.3(12) . . . . ? C20 C18 C19 C14 -179.7(7) . . . . ? C15 C14 C19 C18 -1.3(12) . . . . ? C13 C14 C19 C18 -177.9(7) . . . . ? C17 C18 C20 C24 -166.1(8) . . . . ? C19 C18 C20 C24 14.0(12) . . . . ? C17 C18 C20 C21 15.1(12) . . . . ? C19 C18 C20 C21 -164.9(8) . . . . ? C24 C20 C21 C22 -5.6(12) . . . . ? C18 C20 C21 C22 173.3(7) . . . . ? C20 C21 C22 N6 0.4(13) . . . . ? N6 C23 C24 C20 1.4(13) . . . . ? C21 C20 C24 C23 4.7(12) . . . . ? C18 C20 C24 C23 -174.2(8) . . . . ? C4 C5 N1 C1 -1.2(12) . . . . ? C4 C5 N1 Cd1 -172.7(6) . . . . ? C2 C1 N1 C5 0.1(13) . . . . ? C2 C1 N1 Cd1 172.4(7) . . . . ? N3 Cd1 N1 C5 149.2(6) 5_546 . . . ? N3 Cd1 N1 C5 67.4(7) 4_455 . . . ? N6 Cd1 N1 C5 -20.8(7) 7_567 . . . ? N6 Cd1 N1 C5 -127.4(7) 1_655 . . . ? N1 Cd1 N1 C5 -73.3(6) 7_557 . . . ? N3 Cd1 N1 C1 -22.3(6) 5_546 . . . ? N3 Cd1 N1 C1 -104.2(6) 4_455 . . . ? N6 Cd1 N1 C1 167.7(6) 7_567 . . . ? N6 Cd1 N1 C1 61.1(6) 1_655 . . . ? N1 Cd1 N1 C1 115.2(6) 7_557 . . . ? N4 C12 N2 N3 -0.2(8) . . . . ? C10 C12 N2 N3 177.9(6) . . . . ? N4 C13 N3 N2 1.4(8) . . . . ? C14 C13 N3 N2 175.9(7) . . . . ? N4 C13 N3 Cd1 164.7(6) . . . 3_554 ? C14 C13 N3 Cd1 -20.8(13) . . . 3_554 ? C12 N2 N3 C13 -0.7(8) . . . . ? C12 N2 N3 Cd1 -168.8(5) . . . 3_554 ? N3 C13 N4 C12 -1.6(8) . . . . ? C14 C13 N4 C12 -176.3(7) . . . . ? N3 C13 N4 N5 176.4(8) . . . . ? C14 C13 N4 N5 1.7(12) . . . . ? N2 C12 N4 C13 1.1(8) . . . . ? C10 C12 N4 C13 -177.0(7) . . . . ? N2 C12 N4 N5 -176.9(8) . . . . ? C10 C12 N4 N5 5.0(13) . . . . ? C21 C22 N6 C23 5.7(13) . . . . ? C21 C22 N6 Cd1 -154.4(6) . . . 1_455 ? C24 C23 N6 C22 -6.6(12) . . . . ? C24 C23 N6 Cd1 155.6(7) . . . 1_455 ? O2 Cl1 O3 O2 180.000(2) . . . 7 ? O1 Cl1 O3 O2 -92.3(18) 7 . . 7 ? O1 Cl1 O3 O2 87.7(18) . . . 7 ? O5 Cl2 O4 Cl2 176(2) . . . 7_557 ? O6 Cl2 O4 Cl2 -62.5(5) . . . 7_557 ? O4 Cl2 O4 Cl2 61.2(9) 7_557 . . 7_557 ? O4 Cl2 O6 Cl2 65.4(10) . . . 7_557 ? O5 Cl2 O6 Cl2 -166(3) . . . 7_557 ? O4 Cl2 O6 Cl2 -55.6(10) 7_557 . . 7_557 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.271 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.136 # Attachment '3.cif' data_80703cm _database_code_depnum_ccdc_archive 'CCDC 836120' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Cd Cl8 N12 O8' _chemical_formula_weight 1330.92 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.9014(16) _cell_length_b 15.9014(16) _cell_length_c 21.666(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5478.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5808 _cell_measurement_theta_min 2.272 _cell_measurement_theta_max 27.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8344 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28653 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.60 _reflns_number_total 5166 _reflns_number_gt 4444 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1005P)^2^+4.6766P] 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' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 5166 _refine_ls_number_parameters 387 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9606(4) 0.7586(4) 0.2852(3) 0.0335(16) Uani 1 1 d . . . H1 H 0.9915 0.7641 0.3226 0.040 Uiso 1 1 calc R . . C2 C 0.9035(4) 0.6932(4) 0.2802(3) 0.0344(16) Uani 1 1 d . . . H2 H 0.8964 0.6547 0.3133 0.041 Uiso 1 1 calc R . . C3 C 0.8566(4) 0.6841(4) 0.2262(3) 0.0259(14) Uani 1 1 d . . . C4 C 0.8724(4) 0.7419(4) 0.1794(3) 0.0326(15) Uani 1 1 d . . . H4 H 0.8436 0.7378 0.1411 0.039 Uiso 1 1 calc R . . C5 C 0.9303(5) 0.8052(4) 0.1888(3) 0.0350(15) Uani 1 1 d . . . H5 H 0.9390 0.8445 0.1564 0.042 Uiso 1 1 calc R . . C6 C 0.7895(4) 0.6184(4) 0.2201(3) 0.0294(15) Uani 1 1 d . . . C7 C 0.7901(5) 0.5481(4) 0.2573(4) 0.0399(17) Uani 1 1 d . . . H7 H 0.8339 0.5410 0.2867 0.048 Uiso 1 1 calc R . . C8 C 0.7282(5) 0.4880(5) 0.2524(4) 0.0471(19) Uani 1 1 d . . . H8 H 0.7306 0.4391 0.2776 0.057 Uiso 1 1 calc R . . C9 C 0.6624(5) 0.4982(5) 0.2113(3) 0.0377(17) Uani 1 1 d . . . H9 H 0.6192 0.4571 0.2085 0.045 Uiso 1 1 calc R . . C10 C 0.6606(4) 0.5695(4) 0.1742(3) 0.0275(14) Uani 1 1 d . . . C11 C 0.7238(4) 0.6290(4) 0.1788(3) 0.0260(14) Uani 1 1 d . . . H11 H 0.7221 0.6776 0.1534 0.031 Uiso 1 1 calc R . . C12 C 0.5910(4) 0.5779(4) 0.1304(3) 0.0235(12) Uani 1 1 d . . . C13 C 0.4947(4) 0.6285(4) 0.0686(3) 0.0229(12) Uani 1 1 d . . . C14 C 0.4392(4) 0.6909(4) 0.0382(3) 0.0245(12) Uani 1 1 d . . . C15 C 0.4567(4) 0.7217(4) -0.0211(3) 0.0333(16) Uani 1 1 d . . . H15 H 0.5042 0.7024 -0.0435 0.040 Uiso 1 1 calc R . . C16 C 0.4019(5) 0.7817(5) -0.0464(3) 0.0366(17) Uani 1 1 d . . . H16 H 0.4119 0.8022 -0.0869 0.044 Uiso 1 1 calc R . . C17 C 0.3340(4) 0.8116(4) -0.0135(3) 0.0307(16) Uani 1 1 d . . . H17 H 0.2982 0.8529 -0.0312 0.037 Uiso 1 1 calc R . . C18 C 0.3175(4) 0.7806(4) 0.0463(3) 0.0262(14) Uani 1 1 d . . . C19 C 0.3712(4) 0.7207(4) 0.0705(3) 0.0285(14) Uani 1 1 d . . . H19 H 0.3606 0.6996 0.1108 0.034 Uiso 1 1 calc R . . C20 C 0.2454(4) 0.8112(4) 0.0836(3) 0.0273(14) Uani 1 1 d . . . C21 C 0.2024(4) 0.8867(4) 0.0704(3) 0.0281(14) Uani 1 1 d . . . H21 H 0.2165 0.9181 0.0346 0.034 Uiso 1 1 calc R . . C22 C 0.1404(4) 0.9148(4) 0.1093(3) 0.0302(15) Uani 1 1 d . . . H22 H 0.1101 0.9639 0.0980 0.036 Uiso 1 1 calc R . . C23 C 0.1578(4) 0.8019(4) 0.1732(3) 0.0325(16) Uani 1 1 d . . . H23 H 0.1416 0.7713 0.2089 0.039 Uiso 1 1 calc R . . C24 C 0.2178(4) 0.7682(4) 0.1356(3) 0.0325(15) Uani 1 1 d . . . H24 H 0.2409 0.7146 0.1451 0.039 Uiso 1 1 calc R . . Cd1 Cd 0.44174(2) 0.44174(2) 0.0000 0.02089(18) Uani 1 2 d S . . Cl1 Cl 0.73339(13) 0.73339(13) 0.0000 0.0649(9) Uani 1 2 d S . . Cl2 Cl 0.12388(16) 0.12388(16) 0.0000 0.0741(10) Uani 1 2 d S . . N1 N 0.9744(3) 0.8148(3) 0.2401(3) 0.0290(12) Uani 1 1 d . . . N2 N 0.5530(3) 0.5134(3) 0.1034(2) 0.0275(11) Uani 1 1 d . . . N3 N 0.4933(3) 0.5455(3) 0.0647(3) 0.0266(12) Uani 1 1 d . . . N4 N 0.5558(3) 0.6510(3) 0.1092(2) 0.0256(11) Uani 1 1 d . . . N5 N 0.5757(4) 0.7325(3) 0.1296(3) 0.0424(16) Uani 1 1 d . . . H5A H 0.5249 0.7486 0.1408 0.051 Uiso 1 1 d R . . H5B H 0.6037 0.7596 0.1014 0.051 Uiso 1 1 d R . . N6 N 0.1202(4) 0.8767(4) 0.1624(2) 0.0291(11) Uani 1 1 d . . . O1 O 0.7524(8) 0.7776(6) 0.0534(4) 0.125(4) Uani 1 1 d . . . O2 O 0.6722(7) 0.6722(7) 0.0000 0.154(7) Uani 1 2 d S . . O3 O 0.7812(18) 0.6559(12) 0.0175(12) 0.156(11) Uani 0.50 1 d P . . O4 O 0.1911(11) 0.1176(10) 0.0299(9) 0.251(12) Uani 1 1 d . A . O5 O 0.0741(14) 0.1344(18) 0.0442(7) 0.211(12) Uani 0.70 1 d P A 1 O6 O 0.0611(13) 0.0611(13) 0.0000 0.30(4) Uani 0.60 2 d SP A 2 C25 C 0.4708(6) 0.9742(5) 0.0923(4) 0.183(10) Uani 0.50 1 d PDU B 3 H25 H 0.4468 0.9336 0.1228 0.220 Uiso 0.50 1 calc PR B 3 Cl3 Cl 0.5366(3) 0.9205(3) 0.0454(2) 0.1349(17) Uani 0.50 1 d PD B 3 Cl4 Cl 0.3883(5) 1.0347(5) 0.0634(3) 0.104(2) Uani 0.50 1 d PD B 3 Cl5 Cl 0.5400(5) 1.0417(5) 0.1321(4) 0.114(2) Uani 0.50 1 d PD B 3 C25' C 0.4708(6) 0.9742(5) 0.0923(4) 0.183(10) Uani 0.50 1 d PDU C 4 H25' H 0.4195 0.9678 0.0660 0.220 Uiso 0.50 1 calc PR C 4 Cl3' Cl 0.5366(3) 0.9205(3) 0.0454(2) 0.1349(17) Uani 0.50 1 d PD C 4 Cl6 Cl 0.4342(4) 0.9161(3) 0.1536(2) 0.0708(14) Uani 0.50 1 d PD C 4 Cl7 Cl 0.4741(9) 1.0767(6) 0.0899(6) 0.160(4) Uani 0.50 1 d PDU C 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(4) 0.037(4) 0.031(4) -0.002(3) -0.009(3) -0.006(3) C2 0.034(4) 0.027(3) 0.042(4) 0.008(3) -0.010(3) -0.006(3) C3 0.020(3) 0.023(3) 0.034(3) -0.003(3) -0.004(3) 0.002(3) C4 0.032(4) 0.032(4) 0.033(4) 0.003(3) -0.008(3) -0.006(3) C5 0.039(4) 0.028(3) 0.037(4) 0.007(3) -0.003(3) -0.004(3) C6 0.029(4) 0.025(3) 0.034(3) -0.001(3) 0.001(3) -0.001(3) C7 0.042(4) 0.031(4) 0.047(4) 0.007(4) -0.017(4) 0.005(3) C8 0.054(5) 0.037(4) 0.050(4) 0.020(4) -0.023(4) -0.011(3) C9 0.040(4) 0.030(4) 0.043(4) 0.002(3) -0.014(3) -0.012(3) C10 0.024(3) 0.029(3) 0.029(3) -0.003(3) -0.001(3) 0.006(3) C11 0.024(3) 0.024(3) 0.030(3) -0.002(3) 0.000(3) 0.007(3) C12 0.020(3) 0.022(3) 0.029(3) -0.001(2) 0.002(3) -0.003(2) C13 0.021(3) 0.024(3) 0.023(3) -0.002(3) 0.002(3) -0.002(2) C14 0.024(3) 0.022(3) 0.028(3) -0.007(2) 0.002(3) -0.002(3) C15 0.031(4) 0.032(4) 0.037(4) -0.001(3) 0.007(3) 0.002(3) C16 0.040(4) 0.042(4) 0.028(3) 0.005(3) 0.005(3) 0.003(3) C17 0.036(4) 0.025(3) 0.031(4) 0.001(3) -0.005(3) -0.002(3) C18 0.028(3) 0.023(3) 0.028(3) -0.002(3) 0.006(3) 0.002(3) C19 0.029(3) 0.028(3) 0.028(3) 0.004(3) 0.001(3) -0.001(3) C20 0.022(3) 0.030(3) 0.030(3) -0.007(3) -0.006(3) -0.001(3) C21 0.031(3) 0.028(3) 0.026(3) 0.000(3) -0.003(3) 0.001(3) C22 0.030(3) 0.027(3) 0.034(4) -0.001(3) -0.008(3) 0.005(3) C23 0.038(4) 0.024(3) 0.035(4) -0.002(3) 0.003(3) 0.000(3) C24 0.037(4) 0.021(3) 0.040(4) 0.003(3) 0.004(3) 0.009(3) Cd1 0.0179(2) 0.0179(2) 0.0270(3) 0.0012(2) -0.0012(2) -0.0025(2) Cl1 0.0742(13) 0.0742(13) 0.0463(16) -0.0021(15) 0.0021(15) -0.0306(17) Cl2 0.0891(16) 0.0891(16) 0.0440(16) 0.0104(17) -0.0104(17) -0.030(2) N1 0.026(3) 0.025(3) 0.036(3) -0.006(2) -0.003(2) 0.004(2) N2 0.024(3) 0.026(3) 0.032(3) 0.000(2) -0.005(3) 0.002(2) N3 0.020(2) 0.023(3) 0.037(3) -0.007(2) 0.001(2) -0.006(2) N4 0.024(3) 0.019(2) 0.034(3) -0.005(2) 0.000(2) -0.001(2) N5 0.045(4) 0.022(3) 0.060(4) -0.015(3) -0.023(3) 0.004(3) N6 0.025(3) 0.029(3) 0.033(3) -0.005(3) 0.002(3) 0.003(2) O1 0.207(12) 0.099(7) 0.069(5) 0.003(5) -0.036(7) -0.035(7) O2 0.148(9) 0.148(9) 0.166(15) -0.061(12) 0.061(12) -0.058(12) O3 0.22(3) 0.069(12) 0.18(2) 0.034(14) 0.06(2) 0.019(14) O4 0.231(17) 0.172(13) 0.35(3) -0.117(15) -0.205(19) 0.074(12) O5 0.20(2) 0.37(4) 0.066(9) -0.061(14) 0.086(12) -0.05(2) O6 0.27(4) 0.27(4) 0.36(6) 0.22(4) -0.22(4) -0.19(4) C25 0.186(11) 0.178(10) 0.186(11) -0.004(5) 0.000(5) 0.011(5) Cl3 0.183(5) 0.109(3) 0.112(3) -0.011(2) 0.053(3) 0.000(3) Cl4 0.102(5) 0.144(7) 0.067(4) -0.012(4) 0.008(3) 0.036(5) Cl5 0.125(6) 0.102(5) 0.115(5) -0.019(4) 0.018(5) -0.007(5) C25' 0.186(11) 0.178(10) 0.186(11) -0.004(5) 0.000(5) 0.011(5) Cl3' 0.183(5) 0.109(3) 0.112(3) -0.011(2) 0.053(3) 0.000(3) Cl6 0.090(4) 0.058(3) 0.064(3) -0.001(2) 0.022(3) -0.001(3) Cl7 0.183(7) 0.135(6) 0.161(6) 0.005(5) 0.027(6) -0.028(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(9) . ? C1 C2 1.384(9) . ? C1 H1 0.9500 . ? C2 C3 1.395(9) . ? C2 H2 0.9500 . ? C3 C4 1.391(10) . ? C3 C6 1.499(9) . ? C4 C5 1.378(10) . ? C4 H4 0.9500 . ? C5 N1 1.323(9) . ? C5 H5 0.9500 . ? C6 C7 1.379(10) . ? C6 C11 1.386(9) . ? C7 C8 1.376(10) . ? C7 H7 0.9500 . ? C8 C9 1.383(10) . ? C8 H8 0.9500 . ? C9 C10 1.391(10) . ? C9 H9 0.9500 . ? C10 C11 1.384(9) . ? C10 C12 1.463(9) . ? C11 H11 0.9500 . ? C12 N2 1.326(8) . ? C12 N4 1.370(8) . ? C13 N3 1.323(8) . ? C13 N4 1.358(8) . ? C13 C14 1.482(9) . ? C14 C19 1.373(9) . ? C14 C15 1.404(9) . ? C15 C16 1.404(10) . ? C15 H15 0.9500 . ? C16 C17 1.378(10) . ? C16 H16 0.9500 . ? C17 C18 1.412(9) . ? C17 H17 0.9500 . ? C18 C19 1.381(9) . ? C18 C20 1.486(9) . ? C19 H19 0.9500 . ? C20 C24 1.389(9) . ? C20 C21 1.411(9) . ? C21 C22 1.372(10) . ? C21 H21 0.9500 . ? C22 N6 1.339(9) . ? C22 H22 0.9500 . ? C23 N6 1.351(9) . ? C23 C24 1.365(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cd1 N3 2.314(5) . ? Cd1 N3 2.314(5) 7 ? Cd1 N6 2.375(5) 5_545 ? Cd1 N6 2.375(5) 4_454 ? Cd1 N1 2.429(5) 4_464 ? Cd1 N1 2.429(5) 5_645 ? Cl1 O2 1.377(15) . ? Cl1 O1 1.388(8) . ? Cl1 O1 1.388(8) 7 ? Cl1 O3 1.50(2) . ? Cl1 O3 1.50(2) 7 ? Cl2 O5 1.254(14) . ? Cl2 O5 1.254(14) 7 ? Cl2 O4 1.255(13) . ? Cl2 O4 1.255(13) 7 ? Cl2 O6 1.41(3) . ? N1 Cd1 2.429(5) 3_655 ? N2 N3 1.366(7) . ? N4 N5 1.405(7) . ? N5 H5A 0.8811 . ? N5 H5B 0.8700 . ? N6 Cd1 2.375(5) 3 ? O2 O3 1.79(3) 7 ? C25 Cl3 1.690(7) . ? C25 Cl4 1.744(9) . ? C25 Cl5 1.763(9) . ? C25 H25 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.6(6) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 116.5(6) . . ? C4 C3 C6 121.7(6) . . ? C2 C3 C6 121.8(6) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 124.2(6) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C7 C6 C11 118.7(6) . . ? C7 C6 C3 120.6(6) . . ? C11 C6 C3 120.6(6) . . ? C8 C7 C6 120.9(7) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.6(7) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 118.9(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 C12 122.3(6) . . ? C9 C10 C12 117.7(6) . . ? C6 C11 C10 120.8(6) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? N2 C12 N4 108.7(5) . . ? N2 C12 C10 124.1(5) . . ? N4 C12 C10 127.1(5) . . ? N3 C13 N4 108.5(5) . . ? N3 C13 C14 129.0(6) . . ? N4 C13 C14 122.4(5) . . ? C19 C14 C15 120.1(6) . . ? C19 C14 C13 118.3(5) . . ? C15 C14 C13 121.5(6) . . ? C16 C15 C14 118.2(7) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 121.2(7) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 118.4(6) . . ? C19 C18 C20 119.7(6) . . ? C17 C18 C20 121.9(6) . . ? C14 C19 C18 122.1(6) . . ? C14 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C24 C20 C21 115.5(6) . . ? C24 C20 C18 121.6(6) . . ? C21 C20 C18 122.9(6) . . ? C22 C21 C20 120.0(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N6 C22 C21 123.6(6) . . ? N6 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N6 C23 C24 123.5(6) . . ? N6 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C20 120.8(6) . . ? C23 C24 H24 119.6 . . ? C20 C24 H24 119.6 . . ? N3 Cd1 N3 82.1(3) . 7 ? N3 Cd1 N6 88.48(18) . 5_545 ? N3 Cd1 N6 159.00(19) 7 5_545 ? N3 Cd1 N6 159.00(19) . 4_454 ? N3 Cd1 N6 88.48(18) 7 4_454 ? N6 Cd1 N6 106.1(2) 5_545 4_454 ? N3 Cd1 N1 87.50(18) . 4_464 ? N3 Cd1 N1 110.17(18) 7 4_464 ? N6 Cd1 N1 88.0(2) 5_545 4_464 ? N6 Cd1 N1 78.2(2) 4_454 4_464 ? N3 Cd1 N1 110.17(18) . 5_645 ? N3 Cd1 N1 87.50(18) 7 5_645 ? N6 Cd1 N1 78.2(2) 5_545 5_645 ? N6 Cd1 N1 88.0(2) 4_454 5_645 ? N1 Cd1 N1 157.0(2) 4_464 5_645 ? O2 Cl1 O1 120.8(4) . . ? O2 Cl1 O1 120.8(4) . 7 ? O1 Cl1 O1 118.4(9) . 7 ? O2 Cl1 O3 77.1(10) . . ? O1 Cl1 O3 95.5(12) . . ? O1 Cl1 O3 97.6(11) 7 . ? O2 Cl1 O3 77.1(10) . 7 ? O1 Cl1 O3 97.6(11) . 7 ? O1 Cl1 O3 95.5(12) 7 7 ? O3 Cl1 O3 154(2) . 7 ? O5 Cl2 O5 139(2) . 7 ? O5 Cl2 O4 98.9(12) . . ? O5 Cl2 O4 103.4(15) 7 . ? O5 Cl2 O4 103.4(15) . 7 ? O5 Cl2 O4 98.9(12) 7 7 ? O4 Cl2 O4 113.8(18) . 7 ? O5 Cl2 O6 69.4(12) . . ? O5 Cl2 O6 69.4(12) 7 . ? O4 Cl2 O6 123.1(9) . . ? O4 Cl2 O6 123.1(9) 7 . ? C5 N1 C1 116.6(6) . . ? C5 N1 Cd1 117.4(4) . 3_655 ? C1 N1 Cd1 125.4(4) . 3_655 ? C12 N2 N3 107.5(5) . . ? C13 N3 N2 108.7(5) . . ? C13 N3 Cd1 139.1(4) . . ? N2 N3 Cd1 110.7(4) . . ? C13 N4 C12 106.6(5) . . ? C13 N4 N5 127.5(5) . . ? C12 N4 N5 125.8(5) . . ? N4 N5 H5A 98.5 . . ? N4 N5 H5B 110.6 . . ? H5A N5 H5B 121.2 . . ? C22 N6 C23 116.2(6) . . ? C22 N6 Cd1 126.1(4) . 3 ? C23 N6 Cd1 115.3(4) . 3 ? Cl1 O2 O3 54.4(7) . 7 ? Cl3 C25 Cl4 121.9(6) . . ? Cl3 C25 Cl5 102.5(6) . . ? Cl4 C25 Cl5 108.0(6) . . ? Cl3 C25 H25 107.9 . . ? Cl4 C25 H25 107.9 . . ? Cl5 C25 H25 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.7(11) . . . . ? C1 C2 C3 C4 1.6(10) . . . . ? C1 C2 C3 C6 -175.4(7) . . . . ? C2 C3 C4 C5 -1.9(10) . . . . ? C6 C3 C4 C5 175.1(7) . . . . ? C3 C4 C5 N1 1.3(12) . . . . ? C4 C3 C6 C7 161.2(7) . . . . ? C2 C3 C6 C7 -22.1(10) . . . . ? C4 C3 C6 C11 -21.6(10) . . . . ? C2 C3 C6 C11 155.1(7) . . . . ? C11 C6 C7 C8 2.0(11) . . . . ? C3 C6 C7 C8 179.2(7) . . . . ? C6 C7 C8 C9 -2.0(13) . . . . ? C7 C8 C9 C10 1.0(12) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? C8 C9 C10 C12 179.0(7) . . . . ? C7 C6 C11 C10 -1.0(10) . . . . ? C3 C6 C11 C10 -178.3(6) . . . . ? C9 C10 C11 C6 0.1(10) . . . . ? C12 C10 C11 C6 -178.9(6) . . . . ? C11 C10 C12 N2 147.7(6) . . . . ? C9 C10 C12 N2 -31.3(9) . . . . ? C11 C10 C12 N4 -30.4(10) . . . . ? C9 C10 C12 N4 150.5(7) . . . . ? N3 C13 C14 C19 95.5(8) . . . . ? N4 C13 C14 C19 -81.3(8) . . . . ? N3 C13 C14 C15 -86.9(8) . . . . ? N4 C13 C14 C15 96.4(7) . . . . ? C19 C14 C15 C16 -1.4(10) . . . . ? C13 C14 C15 C16 -179.0(6) . . . . ? C14 C15 C16 C17 1.7(11) . . . . ? C15 C16 C17 C18 -1.1(11) . . . . ? C16 C17 C18 C19 0.3(10) . . . . ? C16 C17 C18 C20 179.6(6) . . . . ? C15 C14 C19 C18 0.6(10) . . . . ? C13 C14 C19 C18 178.3(6) . . . . ? C17 C18 C19 C14 -0.1(10) . . . . ? C20 C18 C19 C14 -179.4(6) . . . . ? C19 C18 C20 C24 -15.7(9) . . . . ? C17 C18 C20 C24 165.0(6) . . . . ? C19 C18 C20 C21 161.9(6) . . . . ? C17 C18 C20 C21 -17.5(9) . . . . ? C24 C20 C21 C22 2.6(9) . . . . ? C18 C20 C21 C22 -175.1(6) . . . . ? C20 C21 C22 N6 3.9(10) . . . . ? N6 C23 C24 C20 1.6(11) . . . . ? C21 C20 C24 C23 -5.2(10) . . . . ? C18 C20 C24 C23 172.5(6) . . . . ? C4 C5 N1 C1 -0.3(11) . . . . ? C4 C5 N1 Cd1 -172.1(6) . . . 3_655 ? C2 C1 N1 C5 -0.1(10) . . . . ? C2 C1 N1 Cd1 171.1(5) . . . 3_655 ? N4 C12 N2 N3 0.1(7) . . . . ? C10 C12 N2 N3 -178.3(5) . . . . ? N4 C13 N3 N2 0.7(7) . . . . ? C14 C13 N3 N2 -176.4(6) . . . . ? N4 C13 N3 Cd1 -163.0(5) . . . . ? C14 C13 N3 Cd1 19.9(10) . . . . ? C12 N2 N3 C13 -0.5(7) . . . . ? C12 N2 N3 Cd1 168.2(4) . . . . ? N3 Cd1 N3 C13 69.9(6) 7 . . . ? N6 Cd1 N3 C13 -128.8(6) 5_545 . . . ? N6 Cd1 N3 C13 6.0(10) 4_454 . . . ? N1 Cd1 N3 C13 -40.8(6) 4_464 . . . ? N1 Cd1 N3 C13 154.3(6) 5_645 . . . ? N3 Cd1 N3 N2 -93.6(4) 7 . . . ? N6 Cd1 N3 N2 67.6(4) 5_545 . . . ? N6 Cd1 N3 N2 -157.6(5) 4_454 . . . ? N1 Cd1 N3 N2 155.6(4) 4_464 . . . ? N1 Cd1 N3 N2 -9.2(4) 5_645 . . . ? N3 C13 N4 C12 -0.6(7) . . . . ? C14 C13 N4 C12 176.7(5) . . . . ? N3 C13 N4 N5 -176.3(6) . . . . ? C14 C13 N4 N5 1.0(10) . . . . ? N2 C12 N4 C13 0.3(7) . . . . ? C10 C12 N4 C13 178.7(6) . . . . ? N2 C12 N4 N5 176.1(6) . . . . ? C10 C12 N4 N5 -5.5(10) . . . . ? C21 C22 N6 C23 -7.5(10) . . . . ? C21 C22 N6 Cd1 154.0(5) . . . 3 ? C24 C23 N6 C22 4.7(10) . . . . ? C24 C23 N6 Cd1 -158.7(6) . . . 3 ? O1 Cl1 O2 O3 91.3(12) . . . 7 ? O1 Cl1 O2 O3 -88.7(12) 7 . . 7 ? O3 Cl1 O2 O3 180.0 . . . 7 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.151 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.127 # Attachment '3.cif' data_80707am _database_code_depnum_ccdc_archive 'CCDC 836121' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Cd Cl8 N12 O8' _chemical_formula_weight 1330.92 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8632(18) _cell_length_b 15.8632(18) _cell_length_c 21.760(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5475.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6241 _cell_measurement_theta_min 2.269 _cell_measurement_theta_max 27.195 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8477 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29167 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.60 _reflns_number_total 5163 _reflns_number_gt 4832 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0757P)^2^+13.3740P] 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' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 5163 _refine_ls_number_parameters 395 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5395(4) 0.7410(4) 0.2854(3) 0.0301(13) Uani 1 1 d . . . H1 H 0.5087 0.7354 0.3226 0.036 Uiso 1 1 calc R . . C2 C 0.5964(4) 0.8074(4) 0.2804(3) 0.0293(13) Uani 1 1 d . . . H2 H 0.6028 0.8464 0.3132 0.035 Uiso 1 1 calc R . . C3 C 0.6436(4) 0.8163(4) 0.2275(3) 0.0247(12) Uani 1 1 d . . . C4 C 0.6278(4) 0.7585(4) 0.1807(3) 0.0304(13) Uani 1 1 d . . . H4 H 0.6574 0.7624 0.1429 0.036 Uiso 1 1 calc R . . C5 C 0.5695(4) 0.6959(4) 0.1894(3) 0.0296(12) Uani 1 1 d . . . H5 H 0.5595 0.6578 0.1566 0.035 Uiso 1 1 calc R . . C6 C 0.7105(4) 0.8816(4) 0.2220(3) 0.0240(12) Uani 1 1 d . . . C7 C 0.7103(4) 0.9537(4) 0.2588(3) 0.0360(14) Uani 1 1 d . . . H7 H 0.6664 0.9615 0.2879 0.043 Uiso 1 1 calc R . . C8 C 0.7724(4) 1.0136(4) 0.2538(3) 0.0405(15) Uani 1 1 d . . . H8 H 0.7703 1.0627 0.2788 0.049 Uiso 1 1 calc R . . C9 C 0.8382(4) 1.0030(4) 0.2126(3) 0.0342(14) Uani 1 1 d . . . H9 H 0.8814 1.0443 0.2092 0.041 Uiso 1 1 calc R . . C10 C 0.8400(3) 0.9306(3) 0.1762(2) 0.0238(11) Uani 1 1 d . . . C11 C 0.7767(4) 0.8721(3) 0.1805(3) 0.0239(12) Uani 1 1 d . . . H11 H 0.7779 0.8240 0.1545 0.029 Uiso 1 1 calc R . . C12 C 0.9100(3) 0.9229(3) 0.1318(2) 0.0214(11) Uani 1 1 d . . . C13 C 1.0046(3) 0.8716(4) 0.0696(2) 0.0228(11) Uani 1 1 d . . . C14 C 1.0605(4) 0.8098(3) 0.0393(2) 0.0223(10) Uani 1 1 d . . . C15 C 1.0429(4) 0.7786(4) -0.0186(3) 0.0293(13) Uani 1 1 d . . . H15 H 0.9949 0.7978 -0.0407 0.035 Uiso 1 1 calc R . . C16 C 1.0969(4) 0.7184(4) -0.0441(3) 0.0334(14) Uani 1 1 d . . . H16 H 1.0862 0.6975 -0.0843 0.040 Uiso 1 1 calc R . . C17 C 1.1651(4) 0.6892(4) -0.0117(2) 0.0271(13) Uani 1 1 d . . . H17 H 1.2008 0.6478 -0.0296 0.033 Uiso 1 1 calc R . . C18 C 1.1829(3) 0.7197(3) 0.0474(2) 0.0227(11) Uani 1 1 d . . . C19 C 1.1294(4) 0.7803(4) 0.0719(2) 0.0234(12) Uani 1 1 d . . . H19 H 1.1403 0.8019 0.1118 0.028 Uiso 1 1 calc R . . C20 C 1.2551(4) 0.6887(4) 0.0843(3) 0.0271(12) Uani 1 1 d . . . C21 C 1.2986(4) 0.6150(4) 0.0706(2) 0.0254(12) Uani 1 1 d . . . H21 H 1.2855 0.5844 0.0343 0.030 Uiso 1 1 calc R . . C22 C 1.3609(4) 0.5862(4) 0.1098(3) 0.0266(12) Uani 1 1 d . . . H22 H 1.3912 0.5369 0.0984 0.032 Uiso 1 1 calc R . . C23 C 1.3433(4) 0.6989(4) 0.1736(3) 0.0287(13) Uani 1 1 d . . . H23 H 1.3593 0.7298 0.2091 0.034 Uiso 1 1 calc R . . C24 C 1.2835(4) 0.7326(4) 0.1362(3) 0.0309(13) Uani 1 1 d . . . H24 H 1.2608 0.7865 0.1453 0.037 Uiso 1 1 calc R . . Cd1 Cd 1.05816(2) 1.05816(2) 0.0000 0.01844(15) Uani 1 2 d S . . Cl1 Cl 0.12554(14) 0.87446(14) 0.2500 0.0659(8) Uani 1 2 d S . . Cl2 Cl 0.76932(13) 0.76932(13) 0.0000 0.0761(10) Uani 1 2 d S . . N1 N 0.5261(3) 0.6855(3) 0.2413(2) 0.0261(10) Uani 1 1 d . . . N2 N 0.9454(3) 0.9866(3) 0.1038(2) 0.0241(9) Uani 1 1 d . . . N3 N 1.0059(3) 0.9546(3) 0.0651(2) 0.0224(9) Uani 1 1 d . . . N4 N 0.9452(3) 0.8502(3) 0.1119(2) 0.0262(10) Uani 1 1 d . . . N5 N 0.9283(4) 0.7685(3) 0.1333(3) 0.0522(18) Uani 1 1 d . . . H5B H 0.9740 0.7475 0.1502 0.063 Uiso 1 1 d R . . H5A H 0.9158 0.7399 0.0997 0.063 Uiso 1 1 d R . . N6 N 1.3810(3) 0.6242(3) 0.1630(2) 0.0274(10) Uani 1 1 d . . . O1 O 0.2122(9) 0.8867(13) 0.2547(13) 0.208(9) Uani 0.75 1 d P C . O2 O 0.0574(9) 0.9426(9) 0.2500 0.23(2) Uani 0.50 2 d SP C . O4 O 0.7457(7) 0.7269(7) 0.0503(4) 0.127(3) Uani 1 1 d U . . O5 O 0.8303(5) 0.8303(5) 0.0000 0.140(6) Uani 1 2 d S . . O6 O 0.7096(13) 0.8367(14) 0.0251(14) 0.186(13) Uani 0.50 1 d P . . C25 C 0.0406(6) 0.5335(6) 0.0890(4) 0.121(5) Uani 0.50 1 d PD A 1 H25 H 0.0231 0.5754 0.0572 0.145 Uiso 0.50 1 calc PR A 1 Cl3 Cl 0.0642(3) 0.5818(2) 0.15663(15) 0.1078(11) Uani 0.50 1 d PD A 1 Cl4 Cl 0.1206(3) 0.4709(3) 0.06297(18) 0.0622(11) Uani 0.50 1 d PD A 1 Cl5 Cl -0.0412(5) 0.4735(8) 0.1113(9) 0.291(11) Uani 0.50 1 d PD A 1 C25' C 0.0406(6) 0.5335(6) 0.0890(4) 0.121(5) Uani 0.50 1 d PD B 2 H25' H 0.0892 0.5543 0.0640 0.145 Uiso 0.50 1 calc PR B 2 Cl3' Cl 0.0642(3) 0.5818(2) 0.15663(15) 0.1078(11) Uani 0.50 1 d PD B 2 Cl6 Cl 0.0520(8) 0.4298(5) 0.0766(5) 0.158(3) Uani 0.50 1 d PDU B 2 Cl7 Cl -0.0397(4) 0.5772(4) 0.0474(3) 0.095(2) Uani 0.50 1 d PD B 2 O3 O 0.1136(12) 0.9256(13) 0.2947(8) 0.101(5) Uani 0.50 1 d PU C 3 O3' O 0.1008(9) 0.838(2) 0.3020(8) 0.137(10) Uani 0.50 1 d P C 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.037(3) 0.024(3) 0.000(3) 0.007(2) -0.004(3) C2 0.032(3) 0.028(3) 0.028(3) -0.011(2) 0.006(2) -0.004(3) C3 0.022(3) 0.024(3) 0.028(3) 0.006(2) 0.003(2) 0.007(2) C4 0.029(3) 0.033(3) 0.029(3) -0.003(3) 0.008(3) -0.005(3) C5 0.030(3) 0.031(3) 0.028(3) -0.008(2) 0.004(3) 0.002(2) C6 0.024(3) 0.022(3) 0.026(3) 0.002(2) 0.003(2) -0.002(2) C7 0.039(3) 0.030(3) 0.039(3) -0.008(3) 0.019(3) 0.002(3) C8 0.051(4) 0.029(3) 0.042(4) -0.011(3) 0.018(4) -0.008(3) C9 0.036(3) 0.030(3) 0.037(3) -0.003(3) 0.012(3) -0.011(3) C10 0.028(3) 0.024(3) 0.020(2) 0.003(2) 0.002(2) 0.003(2) C11 0.024(3) 0.022(3) 0.026(3) 0.001(2) 0.000(2) 0.001(2) C12 0.022(3) 0.021(3) 0.022(2) 0.002(2) -0.003(2) -0.0004(19) C13 0.018(3) 0.028(3) 0.023(2) 0.004(2) -0.003(2) -0.002(2) C14 0.022(3) 0.019(3) 0.026(3) 0.007(2) 0.005(2) 0.000(2) C15 0.035(3) 0.025(3) 0.029(3) 0.000(2) -0.007(3) 0.004(3) C16 0.038(3) 0.040(4) 0.022(3) -0.008(3) -0.007(3) 0.005(3) C17 0.031(3) 0.025(3) 0.025(3) -0.001(2) -0.001(2) 0.003(2) C18 0.024(3) 0.019(3) 0.025(3) 0.006(2) -0.001(2) -0.002(2) C19 0.025(3) 0.027(3) 0.018(2) 0.002(2) -0.001(2) -0.001(2) C20 0.020(3) 0.033(3) 0.028(3) 0.007(2) 0.004(2) 0.004(2) C21 0.031(3) 0.028(3) 0.017(2) 0.001(2) 0.004(2) 0.003(2) C22 0.026(3) 0.024(3) 0.030(3) 0.001(2) 0.007(2) 0.005(2) C23 0.033(3) 0.026(3) 0.027(3) -0.005(2) -0.004(2) 0.007(2) C24 0.041(4) 0.023(3) 0.028(3) -0.003(2) 0.002(3) 0.010(3) Cd1 0.01753(17) 0.01753(17) 0.0203(2) -0.00111(16) 0.00111(16) -0.0024(2) Cl1 0.0798(13) 0.0798(13) 0.0381(13) 0.0033(12) 0.0033(12) 0.0177(16) Cl2 0.0890(16) 0.0890(16) 0.0503(16) -0.0061(16) 0.0061(16) -0.0472(19) N1 0.025(2) 0.024(2) 0.030(3) 0.006(2) -0.001(2) 0.0009(18) N2 0.022(2) 0.026(2) 0.024(2) 0.0014(18) -0.002(2) 0.000(2) N3 0.019(2) 0.022(2) 0.026(2) 0.0028(19) 0.0014(18) -0.0009(17) N4 0.026(2) 0.019(2) 0.034(2) 0.0092(18) 0.007(2) 0.003(2) N5 0.059(4) 0.025(3) 0.073(4) 0.021(3) 0.041(3) 0.011(3) N6 0.018(2) 0.033(3) 0.032(2) 0.004(2) 0.002(2) 0.0005(18) O1 0.088(10) 0.25(2) 0.29(2) 0.12(2) 0.014(14) -0.052(11) O2 0.17(2) 0.17(2) 0.37(6) 0.14(3) 0.14(3) 0.15(3) O4 0.162(6) 0.117(6) 0.102(5) 0.007(5) 0.021(5) -0.031(5) O5 0.125(7) 0.125(7) 0.170(13) 0.037(10) -0.037(10) -0.063(9) O6 0.103(15) 0.133(17) 0.32(4) -0.15(2) -0.040(18) 0.012(13) C25 0.124(12) 0.127(12) 0.113(10) -0.030(9) -0.035(9) 0.047(9) Cl3 0.138(3) 0.095(2) 0.090(2) -0.0040(16) -0.025(2) 0.026(2) Cl4 0.079(3) 0.068(3) 0.0391(19) 0.0040(18) 0.000(2) 0.018(2) Cl5 0.072(5) 0.255(14) 0.55(3) -0.263(18) 0.024(9) -0.038(6) C25' 0.124(12) 0.127(12) 0.113(10) -0.030(9) -0.035(9) 0.047(9) Cl3' 0.138(3) 0.095(2) 0.090(2) -0.0040(16) -0.025(2) 0.026(2) Cl6 0.206(7) 0.130(5) 0.137(5) -0.019(5) -0.043(5) 0.001(6) Cl7 0.124(5) 0.075(3) 0.087(4) -0.007(3) -0.054(4) 0.018(3) O3 0.115(8) 0.112(8) 0.077(6) -0.042(6) 0.007(6) 0.006(6) O3' 0.052(8) 0.29(3) 0.071(10) 0.096(14) 0.006(8) 0.018(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.321(8) . ? C1 C2 1.391(8) . ? C1 H1 0.9500 . ? C2 C3 1.381(8) . ? C2 H2 0.9500 . ? C3 C4 1.393(9) . ? C3 C6 1.488(8) . ? C4 C5 1.369(8) . ? C4 H4 0.9500 . ? C5 N1 1.333(7) . ? C5 H5 0.9500 . ? C6 C11 1.393(8) . ? C6 C7 1.396(8) . ? C7 C8 1.374(9) . ? C7 H7 0.9500 . ? C8 C9 1.386(9) . ? C8 H8 0.9500 . ? C9 C10 1.397(8) . ? C9 H9 0.9500 . ? C10 C11 1.370(8) . ? C10 C12 1.477(7) . ? C11 H11 0.9500 . ? C12 N2 1.306(7) . ? C12 N4 1.352(7) . ? C13 N3 1.321(7) . ? C13 N4 1.359(7) . ? C13 C14 1.477(7) . ? C14 C15 1.384(8) . ? C14 C19 1.384(8) . ? C15 C16 1.398(9) . ? C15 H15 0.9500 . ? C16 C17 1.373(9) . ? C16 H16 0.9500 . ? C17 C18 1.403(8) . ? C17 H17 0.9500 . ? C18 C19 1.388(8) . ? C18 C20 1.483(8) . ? C19 H19 0.9500 . ? C20 C21 1.390(8) . ? C20 C24 1.400(8) . ? C21 C22 1.383(8) . ? C21 H21 0.9500 . ? C22 N6 1.345(8) . ? C22 H22 0.9500 . ? C23 N6 1.348(7) . ? C23 C24 1.358(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cd1 N3 2.323(4) 7 ? Cd1 N3 2.323(4) . ? Cd1 N6 2.369(4) 5_755 ? Cd1 N6 2.369(4) 4_574 ? Cd1 N1 2.429(5) 5_655 ? Cd1 N1 2.429(5) 4_564 ? Cl1 O3 1.281(14) 8_665 ? Cl1 O3 1.281(14) . ? Cl1 O3' 1.331(14) 8_665 ? Cl1 O3' 1.331(14) . ? Cl1 O1 1.392(15) . ? Cl1 O1 1.392(14) 8_665 ? Cl1 O2 1.53(2) . ? Cl2 O4 1.337(8) 7 ? Cl2 O4 1.337(8) . ? Cl2 O5 1.368(12) . ? Cl2 O6 1.53(2) . ? Cl2 O6 1.53(2) 7 ? N1 Cd1 2.429(5) 3_645 ? N2 N3 1.374(6) . ? N4 N5 1.403(6) . ? N5 H5B 0.8781 . ? N5 H5A 0.8843 . ? N6 Cd1 2.369(4) 3_745 ? O1 O3' 1.48(3) 8_665 ? O2 O3 1.35(2) . ? O2 O3 1.35(2) 8_665 ? C25 Cl5 1.680(9) . ? C25 Cl3 1.700(6) . ? C25 Cl4 1.709(7) . ? C25 H25 1.0000 . ? O3' O1 1.48(3) 8_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(5) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.6(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 116.4(5) . . ? C2 C3 C6 121.7(5) . . ? C4 C3 C6 121.9(5) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.8(5) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C11 C6 C7 117.6(5) . . ? C11 C6 C3 121.0(5) . . ? C7 C6 C3 121.5(5) . . ? C8 C7 C6 121.3(5) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 120.5(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.8(6) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C11 C10 C9 120.2(5) . . ? C11 C10 C12 122.7(5) . . ? C9 C10 C12 117.0(5) . . ? C10 C11 C6 121.6(5) . . ? C10 C11 H11 119.2 . . ? C6 C11 H11 119.2 . . ? N2 C12 N4 109.4(5) . . ? N2 C12 C10 124.4(5) . . ? N4 C12 C10 126.1(5) . . ? N3 C13 N4 108.0(5) . . ? N3 C13 C14 128.2(5) . . ? N4 C13 C14 123.6(5) . . ? C15 C14 C19 120.4(5) . . ? C15 C14 C13 121.5(5) . . ? C19 C14 C13 118.1(5) . . ? C14 C15 C16 118.8(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C17 C16 C15 120.7(5) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.8(6) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 117.9(5) . . ? C19 C18 C20 119.5(5) . . ? C17 C18 C20 122.5(5) . . ? C14 C19 C18 121.3(5) . . ? C14 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C21 C20 C24 115.5(5) . . ? C21 C20 C18 123.1(5) . . ? C24 C20 C18 121.4(5) . . ? C22 C21 C20 120.0(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N6 C22 C21 123.6(5) . . ? N6 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N6 C23 C24 123.6(5) . . ? N6 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C20 120.9(5) . . ? C23 C24 H24 119.6 . . ? C20 C24 H24 119.6 . . ? N3 Cd1 N3 82.4(2) 7 . ? N3 Cd1 N6 159.00(16) 7 5_755 ? N3 Cd1 N6 88.33(16) . 5_755 ? N3 Cd1 N6 88.33(16) 7 4_574 ? N3 Cd1 N6 159.00(16) . 4_574 ? N6 Cd1 N6 106.1(2) 5_755 4_574 ? N3 Cd1 N1 87.43(15) 7 5_655 ? N3 Cd1 N1 110.14(16) . 5_655 ? N6 Cd1 N1 78.12(17) 5_755 5_655 ? N6 Cd1 N1 88.10(17) 4_574 5_655 ? N3 Cd1 N1 110.14(16) 7 4_564 ? N3 Cd1 N1 87.43(15) . 4_564 ? N6 Cd1 N1 88.10(17) 5_755 4_564 ? N6 Cd1 N1 78.12(17) 4_574 4_564 ? N1 Cd1 N1 157.1(2) 5_655 4_564 ? O3 Cl1 O3 113.0(19) 8_665 . ? O3 Cl1 O3' 65.6(13) 8_665 8_665 ? O3 Cl1 O3' 121.6(11) . 8_665 ? O3 Cl1 O3' 121.6(11) 8_665 . ? O3 Cl1 O3' 65.6(13) . . ? O3' Cl1 O3' 169(2) 8_665 . ? O3 Cl1 O1 131.3(13) 8_665 . ? O3 Cl1 O1 90.1(14) . . ? O3' Cl1 O1 65.8(15) 8_665 . ? O3' Cl1 O1 106.8(12) . . ? O3 Cl1 O1 90.1(14) 8_665 8_665 ? O3 Cl1 O1 131.3(13) . 8_665 ? O3' Cl1 O1 106.8(12) 8_665 8_665 ? O3' Cl1 O1 65.8(15) . 8_665 ? O1 Cl1 O1 106.3(18) . 8_665 ? O3 Cl1 O2 56.5(9) 8_665 . ? O3 Cl1 O2 56.5(9) . . ? O3' Cl1 O2 95.7(11) 8_665 . ? O3' Cl1 O2 95.7(11) . . ? O1 Cl1 O2 126.9(9) . . ? O1 Cl1 O2 126.9(9) 8_665 . ? O4 Cl2 O4 112.8(9) 7 . ? O4 Cl2 O5 123.6(4) 7 . ? O4 Cl2 O5 123.6(4) . . ? O4 Cl2 O6 100.1(10) 7 . ? O4 Cl2 O6 83.5(14) . . ? O5 Cl2 O6 86.8(8) . . ? O4 Cl2 O6 83.5(14) 7 7 ? O4 Cl2 O6 100.1(10) . 7 ? O5 Cl2 O6 86.8(8) . 7 ? O6 Cl2 O6 173.6(17) . 7 ? C1 N1 C5 116.7(5) . . ? C1 N1 Cd1 125.9(4) . 3_645 ? C5 N1 Cd1 117.0(4) . 3_645 ? C12 N2 N3 107.5(4) . . ? C13 N3 N2 108.2(4) . . ? C13 N3 Cd1 139.1(4) . . ? N2 N3 Cd1 111.2(3) . . ? C12 N4 C13 106.9(4) . . ? C12 N4 N5 127.1(5) . . ? C13 N4 N5 125.9(5) . . ? N4 N5 H5B 109.5 . . ? N4 N5 H5A 104.0 . . ? H5B N5 H5A 109.7 . . ? C22 N6 C23 115.8(5) . . ? C22 N6 Cd1 125.9(4) . 3_745 ? C23 N6 Cd1 115.7(4) . 3_745 ? Cl1 O1 O3' 55.1(11) . 8_665 ? O3 O2 O3 104.9(18) . 8_665 ? O3 O2 Cl1 52.4(9) . . ? O3 O2 Cl1 52.4(9) 8_665 . ? Cl5 C25 Cl3 100.1(6) . . ? Cl5 C25 Cl4 109.9(6) . . ? Cl3 C25 Cl4 112.7(5) . . ? Cl5 C25 H25 111.2 . . ? Cl3 C25 H25 111.2 . . ? Cl4 C25 H25 111.2 . . ? Cl1 O3 O2 71.1(12) . . ? Cl1 O3' O1 59.1(9) . 8_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.4(10) . . . . ? C1 C2 C3 C4 2.5(9) . . . . ? C1 C2 C3 C6 -174.6(6) . . . . ? C2 C3 C4 C5 -1.5(9) . . . . ? C6 C3 C4 C5 175.6(6) . . . . ? C3 C4 C5 N1 -0.8(10) . . . . ? C2 C3 C6 C11 156.2(6) . . . . ? C4 C3 C6 C11 -20.7(9) . . . . ? C2 C3 C6 C7 -22.6(9) . . . . ? C4 C3 C6 C7 160.5(6) . . . . ? C11 C6 C7 C8 0.8(10) . . . . ? C3 C6 C7 C8 179.7(6) . . . . ? C6 C7 C8 C9 -1.3(11) . . . . ? C7 C8 C9 C10 0.3(10) . . . . ? C8 C9 C10 C11 1.3(9) . . . . ? C8 C9 C10 C12 178.4(6) . . . . ? C9 C10 C11 C6 -1.8(9) . . . . ? C12 C10 C11 C6 -178.8(5) . . . . ? C7 C6 C11 C10 0.7(9) . . . . ? C3 C6 C11 C10 -178.1(5) . . . . ? C11 C10 C12 N2 144.5(6) . . . . ? C9 C10 C12 N2 -32.6(8) . . . . ? C11 C10 C12 N4 -32.8(8) . . . . ? C9 C10 C12 N4 150.1(6) . . . . ? N3 C13 C14 C15 -87.3(7) . . . . ? N4 C13 C14 C15 97.9(6) . . . . ? N3 C13 C14 C19 96.0(7) . . . . ? N4 C13 C14 C19 -78.8(7) . . . . ? C19 C14 C15 C16 -1.4(8) . . . . ? C13 C14 C15 C16 -178.1(6) . . . . ? C14 C15 C16 C17 1.5(9) . . . . ? C15 C16 C17 C18 -0.7(10) . . . . ? C16 C17 C18 C19 0.0(8) . . . . ? C16 C17 C18 C20 178.9(6) . . . . ? C15 C14 C19 C18 0.7(8) . . . . ? C13 C14 C19 C18 177.5(5) . . . . ? C17 C18 C19 C14 0.1(8) . . . . ? C20 C18 C19 C14 -178.9(5) . . . . ? C19 C18 C20 C21 163.5(5) . . . . ? C17 C18 C20 C21 -15.4(8) . . . . ? C19 C18 C20 C24 -16.2(8) . . . . ? C17 C18 C20 C24 164.9(6) . . . . ? C24 C20 C21 C22 4.9(8) . . . . ? C18 C20 C21 C22 -174.8(5) . . . . ? C20 C21 C22 N6 2.5(9) . . . . ? N6 C23 C24 C20 2.3(10) . . . . ? C21 C20 C24 C23 -7.2(9) . . . . ? C18 C20 C24 C23 172.5(6) . . . . ? C2 C1 N1 C5 -0.9(9) . . . . ? C2 C1 N1 Cd1 171.9(5) . . . 3_645 ? C4 C5 N1 C1 2.0(9) . . . . ? C4 C5 N1 Cd1 -171.4(5) . . . 3_645 ? N4 C12 N2 N3 -0.6(6) . . . . ? C10 C12 N2 N3 -178.3(5) . . . . ? N4 C13 N3 N2 -1.3(6) . . . . ? C14 C13 N3 N2 -176.8(5) . . . . ? N4 C13 N3 Cd1 -165.4(4) . . . . ? C14 C13 N3 Cd1 19.1(9) . . . . ? C12 N2 N3 C13 1.2(6) . . . . ? C12 N2 N3 Cd1 170.1(3) . . . . ? N3 Cd1 N3 C13 70.1(5) 7 . . . ? N6 Cd1 N3 C13 -128.8(6) 5_755 . . . ? N6 Cd1 N3 C13 5.5(8) 4_574 . . . ? N1 Cd1 N3 C13 154.5(5) 5_655 . . . ? N1 Cd1 N3 C13 -40.7(5) 4_564 . . . ? N3 Cd1 N3 N2 -93.7(3) 7 . . . ? N6 Cd1 N3 N2 67.4(3) 5_755 . . . ? N6 Cd1 N3 N2 -158.2(4) 4_574 . . . ? N1 Cd1 N3 N2 -9.3(4) 5_655 . . . ? N1 Cd1 N3 N2 155.6(3) 4_564 . . . ? N2 C12 N4 C13 -0.2(6) . . . . ? C10 C12 N4 C13 177.4(5) . . . . ? N2 C12 N4 N5 175.8(6) . . . . ? C10 C12 N4 N5 -6.5(9) . . . . ? N3 C13 N4 C12 1.0(6) . . . . ? C14 C13 N4 C12 176.7(5) . . . . ? N3 C13 N4 N5 -175.1(6) . . . . ? C14 C13 N4 N5 0.6(9) . . . . ? C21 C22 N6 C23 -7.4(9) . . . . ? C21 C22 N6 Cd1 153.8(4) . . . 3_745 ? C24 C23 N6 C22 5.0(9) . . . . ? C24 C23 N6 Cd1 -158.2(5) . . . 3_745 ? O3 Cl1 O1 O3' -3.5(19) 8_665 . . 8_665 ? O3 Cl1 O1 O3' -125.0(14) . . . 8_665 ? O3' Cl1 O1 O3' 170.6(17) . . . 8_665 ? O1 Cl1 O1 O3' 101.5(14) 8_665 . . 8_665 ? O2 Cl1 O1 O3' -78.5(14) . . . 8_665 ? O3 Cl1 O2 O3 180.000(5) 8_665 . . . ? O3' Cl1 O2 O3 -124.3(13) 8_665 . . . ? O3' Cl1 O2 O3 55.7(13) . . . . ? O1 Cl1 O2 O3 -60.4(17) . . . . ? O1 Cl1 O2 O3 119.6(17) 8_665 . . . ? O3 Cl1 O2 O3 180.000(5) . . . 8_665 ? O3' Cl1 O2 O3 55.7(13) 8_665 . . 8_665 ? O3' Cl1 O2 O3 -124.3(13) . . . 8_665 ? O1 Cl1 O2 O3 119.6(17) . . . 8_665 ? O1 Cl1 O2 O3 -60.4(17) 8_665 . . 8_665 ? O3 Cl1 O3 O2 0.000(2) 8_665 . . . ? O3' Cl1 O3 O2 74.6(17) 8_665 . . . ? O3' Cl1 O3 O2 -115.6(11) . . . . ? O1 Cl1 O3 O2 135.9(10) . . . . ? O1 Cl1 O3 O2 -112.1(16) 8_665 . . . ? O3 O2 O3 Cl1 0.000(3) 8_665 . . . ? O3 Cl1 O3' O1 74(2) 8_665 . . 8_665 ? O3 Cl1 O3' O1 177.1(16) . . . 8_665 ? O3' Cl1 O3' O1 -52.0(11) 8_665 . . 8_665 ? O1 Cl1 O3' O1 -101(2) . . . 8_665 ? O2 Cl1 O3' O1 128.0(11) . . . 8_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.119 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.107 # Attachment '4.cif' data_80709am _database_code_depnum_ccdc_archive 'CCDC 836122' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H36 Cd Cl6 N12 O8' _chemical_formula_weight 1246.00 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8638(16) _cell_length_b 15.8638(16) _cell_length_c 21.568(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5427.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8751 _exptl_absorpt_correction_T_max 0.9142 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28127 _diffrn_reflns_av_R_equivalents 0.1009 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5057 _reflns_number_gt 4326 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0667P)^2^+15.7411P] 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' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack -0.01(5) _refine_ls_number_reflns 5057 _refine_ls_number_parameters 376 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1969(5) 0.0694(6) 0.8093(4) 0.0347(19) Uani 1 1 d . . . H1 H 0.1573 0.0616 0.8418 0.042 Uiso 1 1 calc R . . C2 C 0.2602(5) 0.1267(6) 0.8188(4) 0.036(2) Uani 1 1 d . . . H2 H 0.2644 0.1556 0.8573 0.043 Uiso 1 1 calc R . . C3 C 0.3186(5) 0.1422(5) 0.7717(3) 0.0256(18) Uani 1 1 d . . . C4 C 0.3098(5) 0.0946(5) 0.7200(4) 0.036(2) Uani 1 1 d . . . H4 H 0.3496 0.1003 0.6873 0.043 Uiso 1 1 calc R . . C5 C 0.2436(5) 0.0371(5) 0.7136(4) 0.0307(19) Uani 1 1 d . . . H5 H 0.2386 0.0060 0.6762 0.037 Uiso 1 1 calc R . . C6 C 0.3839(5) 0.2081(5) 0.7787(4) 0.0265(17) Uani 1 1 d . . . C7 C 0.3735(5) 0.2762(5) 0.8191(3) 0.0245(17) Uani 1 1 d . . . H7 H 0.3240 0.2789 0.8437 0.029 Uiso 1 1 calc R . . C8 C 0.4323(5) 0.3392(5) 0.8245(3) 0.0287(17) Uani 1 1 d . . . C9 C 0.5041(6) 0.3363(6) 0.7877(4) 0.043(2) Uani 1 1 d . . . H9 H 0.5443 0.3805 0.7896 0.051 Uiso 1 1 calc R . . C10 C 0.5165(6) 0.2690(6) 0.7486(6) 0.059(3) Uani 1 1 d . . . H10 H 0.5678 0.2648 0.7261 0.071 Uiso 1 1 calc R . . C11 C 0.4565(5) 0.2082(6) 0.7416(4) 0.044(2) Uani 1 1 d . . . H11 H 0.4639 0.1655 0.7112 0.053 Uiso 1 1 calc R . . C12 C 0.4251(4) 0.4085(5) 0.8674(3) 0.0240(16) Uani 1 1 d . . . C13 C 0.3727(5) 0.5049(5) 0.9310(3) 0.0256(16) Uani 1 1 d . . . C14 C 0.3105(4) 0.5590(5) 0.9617(3) 0.0213(14) Uani 1 1 d . . . C15 C 0.2782(5) 0.5401(5) 1.0190(4) 0.033(2) Uani 1 1 d . . . H15 H 0.2952 0.4908 1.0406 0.040 Uiso 1 1 calc R . . C16 C 0.2201(6) 0.5950(6) 1.0444(4) 0.041(2) Uani 1 1 d . . . H16 H 0.2001 0.5846 1.0852 0.049 Uiso 1 1 calc R . . C17 C 0.1896(5) 0.6658(5) 1.0122(4) 0.035(2) Uani 1 1 d . . . H17 H 0.1488 0.7018 1.0307 0.042 Uiso 1 1 calc R . . C18 C 0.2195(5) 0.6817(5) 0.9540(3) 0.0246(17) Uani 1 1 d . . . C19 C 0.2819(5) 0.6289(5) 0.9285(4) 0.0278(18) Uani 1 1 d . . . H19 H 0.3046 0.6410 0.8887 0.033 Uiso 1 1 calc R . . C20 C 0.1901(5) 0.7536(5) 0.9161(3) 0.0266(17) Uani 1 1 d . . . C21 C 0.2328(5) 0.7838(5) 0.8642(3) 0.0302(18) Uani 1 1 d . . . H21 H 0.2870 0.7617 0.8549 0.036 Uiso 1 1 calc R . . C22 C 0.1997(5) 0.8436(5) 0.8266(4) 0.0270(18) Uani 1 1 d . . . H22 H 0.2309 0.8605 0.7911 0.032 Uiso 1 1 calc R . . C23 C 0.0865(5) 0.8588(5) 0.8899(4) 0.033(2) Uani 1 1 d . . . H23 H 0.0359 0.8875 0.9002 0.040 Uiso 1 1 calc R . . C24 C 0.1151(5) 0.7982(5) 0.9304(3) 0.0258(17) Uani 1 1 d . . . H24 H 0.0850 0.7863 0.9675 0.031 Uiso 1 1 calc R . . C25 C 0.0191(9) 0.5250(9) 0.9033(6) 0.150(16) Uani 0.50 1 d PDU . . Cd1 Cd 0.55916(3) 0.55916(3) 1.0000 0.01999(19) Uani 1 2 d S . . Cl1 Cl 0.3763(2) 0.6237(2) 0.7500 0.0964(17) Uani 1 2 d S . . Cl2 Cl 0.2542(5) 0.2830(4) 1.0026(8) 0.063(3) Uani 0.50 1 d P . . Cl3 Cl -0.0453(9) 0.4571(10) 0.8626(7) 0.197(6) Uani 0.50 1 d PD . . Cl4 Cl 0.0808(8) 0.4660(10) 0.9523(6) 0.177(6) Uani 0.50 1 d PD . . Cl5 Cl 0.0875(8) 0.5568(10) 0.8461(6) 0.166(4) Uani 0.50 1 d PD . . Cl6 Cl -0.0339(9) 0.6053(11) 0.9402(6) 0.195(6) Uani 0.50 1 d PD . . N1 N 0.1867(4) 0.0245(4) 0.7588(3) 0.0263(15) Uani 1 1 d . . . N2 N 0.4557(4) 0.5062(4) 0.9336(3) 0.0304(16) Uani 1 1 d . . . N3 N 0.4878(4) 0.4461(4) 0.8948(3) 0.0261(14) Uani 1 1 d . . . N4 N 0.3515(4) 0.4436(4) 0.8896(3) 0.0261(13) Uani 1 1 d . . . N5 N 0.2691(4) 0.4242(5) 0.8681(4) 0.048(2) Uani 1 1 d . . . H5A H 0.2433 0.4724 0.8551 0.072 Uiso 1 1 d R . . H5B H 0.2390 0.4011 0.8997 0.072 Uiso 1 1 d R . . N6 N 0.1251(4) 0.8799(4) 0.8372(3) 0.0315(15) Uani 1 1 d . . . O1 O 0.4335(16) 0.6193(19) 0.7110(8) 0.337(16) Uani 1 1 d . . . O2 O 0.3082(12) 0.6143(11) 0.7224(11) 0.274(14) Uani 1 1 d . . . O3 O 0.3279(6) 0.3279(6) 1.0000 0.120(5) Uani 1 2 d S . . O4 O 0.2289(7) 0.2443(9) 0.9491(4) 0.124(4) Uani 1 1 d . . . O5 O 0.203(2) 0.3490(14) 1.012(2) 0.221(19) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(4) 0.040(5) 0.047(5) 0.000(4) 0.003(3) -0.002(4) C2 0.034(5) 0.037(5) 0.036(4) -0.008(4) -0.004(4) -0.007(4) C3 0.021(4) 0.024(4) 0.031(4) -0.004(3) -0.005(3) 0.004(3) C4 0.030(5) 0.034(5) 0.042(5) -0.010(4) 0.010(4) 0.002(4) C5 0.030(5) 0.026(5) 0.036(4) -0.007(3) -0.004(4) -0.004(4) C6 0.021(4) 0.026(4) 0.032(4) 0.002(3) -0.002(3) -0.005(3) C7 0.016(4) 0.031(4) 0.026(4) 0.000(3) -0.004(3) 0.003(3) C8 0.029(4) 0.029(4) 0.028(4) -0.008(3) -0.006(4) -0.004(4) C9 0.033(5) 0.050(6) 0.044(5) -0.020(4) 0.012(4) -0.019(4) C10 0.038(5) 0.068(7) 0.070(7) -0.034(7) 0.026(6) -0.020(5) C11 0.033(5) 0.051(5) 0.049(5) -0.021(5) 0.011(4) 0.001(4) C12 0.023(5) 0.023(4) 0.026(3) 0.007(3) -0.004(3) -0.003(3) C13 0.030(5) 0.018(4) 0.028(4) 0.007(3) -0.007(3) -0.004(3) C14 0.022(4) 0.023(4) 0.020(3) -0.006(3) -0.002(3) 0.006(4) C15 0.025(4) 0.033(5) 0.042(5) 0.020(4) -0.007(3) -0.002(4) C16 0.046(6) 0.042(5) 0.035(5) 0.009(4) 0.010(4) 0.003(5) C17 0.029(4) 0.036(5) 0.039(5) -0.004(4) 0.003(4) 0.002(4) C18 0.022(4) 0.027(4) 0.026(4) -0.005(3) -0.002(3) 0.007(3) C19 0.028(4) 0.027(4) 0.028(4) -0.003(3) 0.002(3) -0.002(4) C20 0.030(4) 0.024(4) 0.026(4) -0.008(3) -0.006(3) 0.010(3) C21 0.022(4) 0.034(5) 0.035(4) -0.003(4) 0.005(3) 0.007(4) C22 0.024(4) 0.029(4) 0.028(4) 0.001(3) 0.001(3) 0.010(3) C23 0.031(5) 0.037(5) 0.032(4) -0.012(4) 0.001(3) 0.005(4) C24 0.028(4) 0.030(4) 0.019(4) -0.005(3) 0.006(3) 0.003(4) C25 0.148(18) 0.148(19) 0.154(18) 0.008(10) -0.016(10) 0.009(10) Cd1 0.0166(2) 0.0166(2) 0.0267(3) -0.0023(3) 0.0023(3) -0.0016(3) Cl1 0.122(3) 0.122(3) 0.045(2) -0.003(3) -0.003(3) 0.046(3) Cl2 0.075(6) 0.066(5) 0.048(3) -0.005(6) 0.020(6) -0.024(5) Cl3 0.171(12) 0.206(15) 0.214(14) 0.019(12) -0.041(10) 0.008(11) Cl4 0.143(10) 0.244(16) 0.146(9) 0.052(10) -0.021(8) -0.036(10) Cl5 0.157(10) 0.189(12) 0.152(10) -0.020(9) -0.035(8) 0.001(10) Cl6 0.188(14) 0.252(17) 0.146(10) 0.040(11) 0.003(10) 0.064(12) N1 0.019(3) 0.020(3) 0.039(4) -0.002(3) -0.009(3) 0.000(2) N2 0.030(4) 0.024(3) 0.037(4) -0.003(3) -0.001(3) -0.004(3) N3 0.019(3) 0.027(3) 0.032(3) 0.002(3) -0.001(3) 0.002(3) N4 0.018(3) 0.028(3) 0.033(3) -0.004(3) -0.005(2) 0.004(3) N5 0.019(3) 0.056(5) 0.068(5) -0.025(4) -0.018(3) 0.007(4) N6 0.031(4) 0.025(4) 0.038(4) -0.007(3) -0.005(3) -0.003(3) O1 0.34(3) 0.53(4) 0.142(13) -0.088(18) 0.174(18) -0.05(3) O2 0.209(18) 0.211(17) 0.40(3) 0.14(2) -0.22(2) -0.064(14) O3 0.109(7) 0.109(7) 0.143(13) 0.034(10) -0.034(10) -0.036(10) O4 0.098(8) 0.205(14) 0.070(6) -0.038(7) 0.012(6) -0.058(8) O5 0.19(3) 0.059(14) 0.41(6) -0.11(3) 0.03(4) -0.031(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.312(10) . ? C1 C2 1.370(11) . ? C1 H1 0.9500 . ? C2 C3 1.397(12) . ? C2 H2 0.9500 . ? C3 C4 1.353(11) . ? C3 C6 1.481(11) . ? C4 C5 1.399(11) . ? C4 H4 0.9500 . ? C5 N1 1.343(10) . ? C5 H5 0.9500 . ? C6 C7 1.397(11) . ? C6 C11 1.402(11) . ? C7 C8 1.372(10) . ? C7 H7 0.9500 . ? C8 C9 1.388(11) . ? C8 C12 1.441(10) . ? C9 C10 1.374(13) . ? C9 H9 0.9500 . ? C10 C11 1.364(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 N3 1.302(9) . ? C12 N4 1.379(9) . ? C13 N2 1.318(10) . ? C13 N4 1.363(9) . ? C13 C14 1.465(10) . ? C14 C15 1.372(10) . ? C14 C19 1.397(11) . ? C15 C16 1.380(12) . ? C15 H15 0.9500 . ? C16 C17 1.406(12) . ? C16 H16 0.9500 . ? C17 C18 1.367(11) . ? C17 H17 0.9500 . ? C18 C19 1.408(10) . ? C18 C20 1.479(11) . ? C19 H19 0.9500 . ? C20 C21 1.393(11) . ? C20 C24 1.418(10) . ? C21 C22 1.354(11) . ? C21 H21 0.9500 . ? C22 N6 1.335(10) . ? C22 H22 0.9500 . ? C23 N6 1.334(11) . ? C23 C24 1.376(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 Cl5 1.717(10) . ? C25 Cl4 1.718(10) . ? C25 Cl6 1.721(9) . ? C25 Cl3 1.725(10) . ? Cd1 N2 2.335(6) . ? Cd1 N2 2.335(6) 7_557 ? Cd1 N6 2.359(6) 3_655 ? Cd1 N6 2.359(6) 6_566 ? Cd1 N1 2.426(6) 3 ? Cd1 N1 2.426(6) 6_556 ? Cl1 O1 1.239(15) . ? Cl1 O1 1.239(15) 8_666 ? Cl1 O2 1.242(14) 8_666 ? Cl1 O2 1.242(14) . ? Cl2 Cl2 0.656(15) 7_557 ? Cl2 O5 1.34(3) . ? Cl2 O4 1.359(18) 7_557 ? Cl2 O4 1.367(16) . ? Cl2 O3 1.370(14) . ? Cl2 O5 1.99(3) 7_557 ? N1 Cd1 2.426(6) 4_454 ? N2 N3 1.366(9) . ? N4 N5 1.421(8) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N6 Cd1 2.359(6) 4_464 ? O3 Cl2 1.370(14) 7_557 ? O4 Cl2 1.359(18) 7_557 ? O5 Cl2 1.99(3) 7_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 125.2(8) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C1 C2 C3 119.6(8) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 115.7(8) . . ? C4 C3 C6 123.4(8) . . ? C2 C3 C6 120.9(7) . . ? C3 C4 C5 121.4(8) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? N1 C5 C4 122.1(7) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C7 C6 C11 116.9(7) . . ? C7 C6 C3 121.8(7) . . ? C11 C6 C3 121.1(7) . . ? C8 C7 C6 122.4(7) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 119.0(7) . . ? C7 C8 C12 123.8(7) . . ? C9 C8 C12 117.2(7) . . ? C10 C9 C8 119.6(8) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 121.2(9) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C6 120.7(8) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? N3 C12 N4 107.7(6) . . ? N3 C12 C8 125.5(7) . . ? N4 C12 C8 126.7(7) . . ? N2 C13 N4 106.6(7) . . ? N2 C13 C14 130.1(7) . . ? N4 C13 C14 123.2(7) . . ? C15 C14 C19 120.9(7) . . ? C15 C14 C13 122.1(7) . . ? C19 C14 C13 116.9(6) . . ? C14 C15 C16 118.0(8) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C15 C16 C17 122.6(8) . . ? C15 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C18 C17 C16 118.7(8) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 119.6(7) . . ? C17 C18 C20 122.8(7) . . ? C19 C18 C20 117.7(7) . . ? C14 C19 C18 120.0(7) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C24 114.2(7) . . ? C21 C20 C18 123.8(7) . . ? C24 C20 C18 121.9(7) . . ? C22 C21 C20 122.3(7) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? N6 C22 C21 122.9(7) . . ? N6 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? N6 C23 C24 124.4(7) . . ? N6 C23 H23 117.8 . . ? C24 C23 H23 117.8 . . ? C23 C24 C20 119.2(7) . . ? C23 C24 H24 120.4 . . ? C20 C24 H24 120.4 . . ? Cl5 C25 Cl4 104.1(10) . . ? Cl5 C25 Cl6 115.0(10) . . ? Cl4 C25 Cl6 113.3(11) . . ? Cl5 C25 Cl3 101.1(10) . . ? Cl4 C25 Cl3 108.1(10) . . ? Cl6 C25 Cl3 114.0(12) . . ? N2 Cd1 N2 82.5(3) . 7_557 ? N2 Cd1 N6 159.5(2) . 3_655 ? N2 Cd1 N6 88.3(2) 7_557 3_655 ? N2 Cd1 N6 88.3(2) . 6_566 ? N2 Cd1 N6 159.5(2) 7_557 6_566 ? N6 Cd1 N6 105.8(3) 3_655 6_566 ? N2 Cd1 N1 87.9(2) . 3 ? N2 Cd1 N1 109.9(2) 7_557 3 ? N6 Cd1 N1 78.0(2) 3_655 3 ? N6 Cd1 N1 87.9(2) 6_566 3 ? N2 Cd1 N1 109.9(2) . 6_556 ? N2 Cd1 N1 87.9(2) 7_557 6_556 ? N6 Cd1 N1 87.9(2) 3_655 6_556 ? N6 Cd1 N1 78.0(2) 6_566 6_556 ? N1 Cd1 N1 156.6(3) 3 6_556 ? O1 Cl1 O1 112(3) . 8_666 ? O1 Cl1 O2 106.6(15) . 8_666 ? O1 Cl1 O2 107.8(16) 8_666 8_666 ? O1 Cl1 O2 107.8(16) . . ? O1 Cl1 O2 106.6(15) 8_666 . ? O2 Cl1 O2 116(2) 8_666 . ? Cl2 Cl2 O5 172.8(14) 7_557 . ? Cl2 Cl2 O4 77(3) 7_557 7_557 ? O5 Cl2 O4 108(2) . 7_557 ? Cl2 Cl2 O4 75(2) 7_557 . ? O5 Cl2 O4 107(2) . . ? O4 Cl2 O4 109.2(9) 7_557 . ? Cl2 Cl2 O3 76.1(3) 7_557 . ? O5 Cl2 O3 96.8(12) . . ? O4 Cl2 O3 117.3(12) 7_557 . ? O4 Cl2 O3 116.7(9) . . ? Cl2 Cl2 O5 4.8(9) 7_557 7_557 ? O5 Cl2 O5 168.1(19) . 7_557 ? O4 Cl2 O5 78.7(14) 7_557 7_557 ? O4 Cl2 O5 78.7(14) . 7_557 ? O3 Cl2 O5 71.4(8) . 7_557 ? C1 N1 C5 116.0(6) . . ? C1 N1 Cd1 117.8(5) . 4_454 ? C5 N1 Cd1 125.8(5) . 4_454 ? C13 N2 N3 109.6(6) . . ? C13 N2 Cd1 137.2(5) . . ? N3 N2 Cd1 111.4(4) . . ? C12 N3 N2 108.3(6) . . ? C13 N4 C12 107.8(6) . . ? C13 N4 N5 126.5(6) . . ? C12 N4 N5 125.4(6) . . ? N4 N5 H5A 109.4 . . ? N4 N5 H5B 108.9 . . ? H5A N5 H5B 109.5 . . ? C23 N6 C22 116.4(7) . . ? C23 N6 Cd1 125.4(5) . 4_464 ? C22 N6 Cd1 115.6(5) . 4_464 ? Cl2 O3 Cl2 27.7(7) . 7_557 ? Cl2 O4 Cl2 27.9(6) 7_557 . ? Cl2 O5 Cl2 2.4(5) . 7_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.9(14) . . . . ? C1 C2 C3 C4 -3.4(12) . . . . ? C1 C2 C3 C6 175.5(8) . . . . ? C2 C3 C4 C5 3.4(12) . . . . ? C6 C3 C4 C5 -175.4(8) . . . . ? C3 C4 C5 N1 -1.8(13) . . . . ? C4 C3 C6 C7 154.9(8) . . . . ? C2 C3 C6 C7 -23.8(12) . . . . ? C4 C3 C6 C11 -20.3(13) . . . . ? C2 C3 C6 C11 160.9(8) . . . . ? C11 C6 C7 C8 -2.3(12) . . . . ? C3 C6 C7 C8 -177.7(7) . . . . ? C6 C7 C8 C9 1.2(12) . . . . ? C6 C7 C8 C12 -177.5(7) . . . . ? C7 C8 C9 C10 -2.6(14) . . . . ? C12 C8 C9 C10 176.2(9) . . . . ? C8 C9 C10 C11 5.2(17) . . . . ? C9 C10 C11 C6 -6.5(18) . . . . ? C7 C6 C11 C10 4.8(14) . . . . ? C3 C6 C11 C10 -179.7(9) . . . . ? C7 C8 C12 N3 147.1(8) . . . . ? C9 C8 C12 N3 -31.6(11) . . . . ? C7 C8 C12 N4 -28.7(12) . . . . ? C9 C8 C12 N4 152.6(8) . . . . ? N2 C13 C14 C15 -89.7(11) . . . . ? N4 C13 C14 C15 94.3(9) . . . . ? N2 C13 C14 C19 93.5(9) . . . . ? N4 C13 C14 C19 -82.5(10) . . . . ? C19 C14 C15 C16 -3.6(12) . . . . ? C13 C14 C15 C16 179.7(8) . . . . ? C14 C15 C16 C17 4.0(13) . . . . ? C15 C16 C17 C18 -1.2(14) . . . . ? C16 C17 C18 C19 -2.1(12) . . . . ? C16 C17 C18 C20 178.9(8) . . . . ? C15 C14 C19 C18 0.5(11) . . . . ? C13 C14 C19 C18 177.3(7) . . . . ? C17 C18 C19 C14 2.5(12) . . . . ? C20 C18 C19 C14 -178.5(7) . . . . ? C17 C18 C20 C21 163.5(8) . . . . ? C19 C18 C20 C21 -15.6(11) . . . . ? C17 C18 C20 C24 -16.0(12) . . . . ? C19 C18 C20 C24 164.9(7) . . . . ? C24 C20 C21 C22 -7.8(12) . . . . ? C18 C20 C21 C22 172.7(7) . . . . ? C20 C21 C22 N6 2.0(13) . . . . ? N6 C23 C24 C20 -0.6(13) . . . . ? C21 C20 C24 C23 7.0(11) . . . . ? C18 C20 C24 C23 -173.4(7) . . . . ? C2 C1 N1 C5 -0.1(13) . . . . ? C2 C1 N1 Cd1 -172.6(7) . . . 4_454 ? C4 C5 N1 C1 0.1(12) . . . . ? C4 C5 N1 Cd1 171.8(6) . . . 4_454 ? N4 C13 N2 N3 -0.6(8) . . . . ? C14 C13 N2 N3 -177.1(7) . . . . ? N4 C13 N2 Cd1 -163.2(6) . . . . ? C14 C13 N2 Cd1 20.3(12) . . . . ? N2 Cd1 N2 C13 68.3(7) 7_557 . . . ? N6 Cd1 N2 C13 4.1(12) 3_655 . . . ? N6 Cd1 N2 C13 -130.1(8) 6_566 . . . ? N1 Cd1 N2 C13 -42.1(8) 3 . . . ? N1 Cd1 N2 C13 153.3(7) 6_556 . . . ? N2 Cd1 N2 N3 -94.1(5) 7_557 . . . ? N6 Cd1 N2 N3 -158.3(6) 3_655 . . . ? N6 Cd1 N2 N3 67.5(5) 6_566 . . . ? N1 Cd1 N2 N3 155.5(5) 3 . . . ? N1 Cd1 N2 N3 -9.1(5) 6_556 . . . ? N4 C12 N3 N2 -1.2(8) . . . . ? C8 C12 N3 N2 -177.7(7) . . . . ? C13 N2 N3 C12 1.1(8) . . . . ? Cd1 N2 N3 C12 168.5(4) . . . . ? N2 C13 N4 C12 -0.2(8) . . . . ? C14 C13 N4 C12 176.7(6) . . . . ? N2 C13 N4 N5 -174.5(7) . . . . ? C14 C13 N4 N5 2.4(12) . . . . ? N3 C12 N4 C13 0.9(8) . . . . ? C8 C12 N4 C13 177.3(7) . . . . ? N3 C12 N4 N5 175.3(7) . . . . ? C8 C12 N4 N5 -8.3(12) . . . . ? C24 C23 N6 C22 -5.4(12) . . . . ? C24 C23 N6 Cd1 155.3(6) . . . 4_464 ? C21 C22 N6 C23 4.8(12) . . . . ? C21 C22 N6 Cd1 -157.9(7) . . . 4_464 ? O5 Cl2 O3 Cl2 -179(4) . . . 7_557 ? O4 Cl2 O3 Cl2 67(3) 7_557 . . 7_557 ? O4 Cl2 O3 Cl2 -65(2) . . . 7_557 ? O5 Cl2 O3 Cl2 1(3) 7_557 . . 7_557 ? O5 Cl2 O4 Cl2 173(2) . . . 7_557 ? O4 Cl2 O4 Cl2 -70.0(19) 7_557 . . 7_557 ? O3 Cl2 O4 Cl2 65.9(11) . . . 7_557 ? O5 Cl2 O4 Cl2 3.7(17) 7_557 . . 7_557 ? O5 Cl2 O5 Cl2 7(26) 7_557 . . 7_557 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5B Cl4 0.91 2.94 3.559(15) 126.6 . N5 H5B Cl2 0.91 2.91 3.673(17) 141.9 . N5 H5B O5 0.91 2.62 3.48(4) 159.1 . N5 H5A Cl5 0.91 2.82 3.598(15) 144.5 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.366 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.112 # Attachment '2.cif' data_2'' _database_code_depnum_ccdc_archive 'CCDC 846267' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 Cd Cl6 N12 O8' _chemical_formula_weight 1262.04 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8178(16) _cell_length_b 15.8178(16) _cell_length_c 21.503(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5380.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12995 _cell_measurement_theta_min 2.626 _cell_measurement_theta_max 27.824 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7909 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28003 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.60 _reflns_number_total 5072 _reflns_number_gt 4691 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0885P)^2^+16.3240P] 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 -0.01(5) _refine_ls_number_reflns 5072 _refine_ls_number_parameters 394 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7543(5) 0.9642(4) 0.2876(3) 0.0336(16) Uani 1 1 d . . . H1 H 0.7595 0.9962 0.3248 0.040 Uiso 1 1 calc R . . C2 C 0.6883(5) 0.9093(5) 0.2838(3) 0.0328(15) Uani 1 1 d . . . H2 H 0.6496 0.9039 0.3173 0.039 Uiso 1 1 calc R . . C3 C 0.6781(4) 0.8602(5) 0.2290(3) 0.0289(15) Uani 1 1 d . . . C4 C 0.7381(4) 0.8753(4) 0.1825(3) 0.0304(15) Uani 1 1 d . . . H4 H 0.7343 0.8456 0.1441 0.036 Uiso 1 1 calc R . . C5 C 0.8014(4) 0.9316(5) 0.1914(3) 0.0330(14) Uani 1 1 d . . . H5 H 0.8408 0.9397 0.1586 0.040 Uiso 1 1 calc R . . C6 C 0.6119(4) 0.7947(4) 0.2239(3) 0.0283(14) Uani 1 1 d . . . C7 C 0.5386(5) 0.7960(5) 0.2593(4) 0.0416(18) Uani 1 1 d . . . H7 H 0.5299 0.8405 0.2884 0.050 Uiso 1 1 calc R . . C8 C 0.4789(5) 0.7348(6) 0.2531(4) 0.050(2) Uani 1 1 d . . . H8 H 0.4285 0.7383 0.2769 0.060 Uiso 1 1 calc R . . C9 C 0.4901(5) 0.6673(5) 0.2129(3) 0.043(2) Uani 1 1 d . . . H9 H 0.4486 0.6241 0.2098 0.052 Uiso 1 1 calc R . . C10 C 0.5636(4) 0.6641(4) 0.1769(3) 0.0272(13) Uani 1 1 d . . . C11 C 0.6228(4) 0.7274(4) 0.1816(3) 0.0244(13) Uani 1 1 d . . . H11 H 0.6716 0.7259 0.1559 0.029 Uiso 1 1 calc R . . C12 C 0.5727(4) 0.5937(4) 0.1328(3) 0.0250(13) Uani 1 1 d . . . C13 C 0.6243(4) 0.4982(4) 0.0697(3) 0.0245(12) Uani 1 1 d . . . C14 C 0.6872(4) 0.4435(5) 0.0390(3) 0.0269(12) Uani 1 1 d . . . C15 C 0.7199(5) 0.4627(5) -0.0198(3) 0.0361(18) Uani 1 1 d . . . H15 H 0.7016 0.5109 -0.0425 0.043 Uiso 1 1 calc R . . C16 C 0.7805(5) 0.4078(6) -0.0433(3) 0.0441(19) Uani 1 1 d . . . H16 H 0.8044 0.4204 -0.0828 0.053 Uiso 1 1 calc R . . C17 C 0.8075(5) 0.3374(5) -0.0135(3) 0.0347(17) Uani 1 1 d . . . H17 H 0.8478 0.3012 -0.0325 0.042 Uiso 1 1 calc R . . C18 C 0.7755(4) 0.3184(4) 0.0459(3) 0.0281(14) Uani 1 1 d . . . C19 C 0.7164(4) 0.3720(4) 0.0717(3) 0.0279(14) Uani 1 1 d . . . H19 H 0.6951 0.3606 0.1121 0.033 Uiso 1 1 calc R . . C20 C 0.8074(4) 0.2459(4) 0.0824(3) 0.0288(14) Uani 1 1 d . . . C21 C 0.8799(4) 0.2023(4) 0.0691(3) 0.0293(14) Uani 1 1 d . . . H21 H 0.9103 0.2151 0.0321 0.035 Uiso 1 1 calc R . . C22 C 0.9099(4) 0.1395(5) 0.1088(3) 0.0322(15) Uani 1 1 d . . . H22 H 0.9592 0.1091 0.0971 0.039 Uiso 1 1 calc R . . C23 C 0.7984(5) 0.1563(4) 0.1737(3) 0.0318(15) Uani 1 1 d . . . H23 H 0.7682 0.1392 0.2097 0.038 Uiso 1 1 calc R . . C24 C 0.7625(4) 0.2180(4) 0.1355(3) 0.0334(15) Uani 1 1 d . . . H24 H 0.7086 0.2410 0.1450 0.040 Uiso 1 1 calc R . . Cd1 Cd 0.44034(3) 0.44034(3) 0.0000 0.02419(19) Uani 1 2 d S . . Cl1 Cl 0.12046(16) 0.12046(16) 0.0000 0.0672(9) Uani 1 2 d SD . . Cl2 Cl 0.2536(3) 0.7907(3) 0.2449(2) 0.0516(11) Uani 0.50 1 d P . . N1 N 0.8123(3) 0.9768(3) 0.2435(3) 0.0307(12) Uani 1 1 d . . . N2 N 0.5088(4) 0.5554(4) 0.1065(3) 0.0321(12) Uani 1 1 d . . . N3 N 0.5421(4) 0.4950(3) 0.0670(3) 0.0316(13) Uani 1 1 d . . . N4 N 0.6464(3) 0.5586(4) 0.1116(2) 0.0292(12) Uani 1 1 d . . . N5 N 0.7285(4) 0.5783(5) 0.1322(4) 0.060(2) Uani 1 1 d . . . H5A H 0.7661 0.5380 0.1387 0.072 Uiso 1 1 d R . . H5B H 0.7469 0.6060 0.0990 0.072 Uiso 1 1 d R . . N6 N 0.8728(4) 0.1200(4) 0.1623(2) 0.0302(11) Uani 1 1 d . . . O3 O 0.2629(7) 0.7356(6) 0.1975(3) 0.093(3) Uani 1 1 d . . . O4 O 0.1730(5) 0.8270(5) 0.2500 0.076(3) Uani 1 2 d S . . O5 O 0.3070(13) 0.8601(12) 0.2453(14) 0.130(8) Uani 0.50 1 d P . . O1 O 0.0961(10) 0.1756(11) 0.0488(7) 0.076(4) Uani 0.50 1 d PU A 1 O2 O 0.1381(17) 0.0582(13) 0.0446(9) 0.130(7) Uani 0.50 1 d PDU A 1 O1' O 0.112(2) 0.2090(18) -0.0013(18) 0.163(10) Uani 0.50 1 d PU A 2 O2' O 0.0751(18) 0.0529(15) 0.0296(13) 0.164(11) Uani 0.50 1 d PDU A 2 C25' C 0.9647(11) 0.4625(11) 0.0671(7) 0.200(11) Uani 0.50 1 d PDU B 3 H25A H 0.9416 0.4905 0.0296 0.240 Uiso 0.50 1 calc PR B 3 H25B H 0.9167 0.4362 0.0896 0.240 Uiso 0.50 1 calc PR B 3 Cl4 Cl 1.0329(5) 0.3848(5) 0.0444(3) 0.0903(19) Uani 0.50 1 d PD B 3 Cl4' Cl 1.0088(17) 0.5358(13) 0.1130(11) 0.279(10) Uani 0.50 1 d PDU B 3 C25 C 0.9647(11) 0.4625(11) 0.0671(7) 0.200(11) Uani 0.50 1 d PDU C 4 H25C H 0.9453 0.4099 0.0466 0.240 Uiso 0.50 1 calc PR C 4 H25D H 0.9468 0.5112 0.0415 0.240 Uiso 0.50 1 calc PR C 4 Cl3 Cl 0.9228(7) 0.4698(9) 0.1394(4) 0.180(7) Uani 0.50 1 d PD C 4 Cl3' Cl 1.0707(11) 0.4616(18) 0.0750(13) 0.302(11) Uani 0.50 1 d PDU C 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.039(4) 0.019(3) -0.011(3) -0.002(3) 0.003(3) C2 0.039(4) 0.043(4) 0.016(3) -0.012(3) 0.012(3) -0.004(3) C3 0.027(3) 0.040(4) 0.019(3) -0.002(3) -0.005(3) -0.003(3) C4 0.036(4) 0.039(4) 0.017(3) -0.007(3) 0.001(3) -0.007(3) C5 0.032(3) 0.036(4) 0.031(3) 0.002(3) 0.007(3) -0.004(3) C6 0.034(4) 0.033(4) 0.017(3) -0.003(3) -0.001(3) 0.001(3) C7 0.044(4) 0.048(4) 0.033(4) -0.011(3) 0.012(3) -0.005(3) C8 0.048(4) 0.069(5) 0.034(4) -0.025(4) 0.018(4) -0.015(4) C9 0.043(4) 0.049(5) 0.039(4) -0.023(4) 0.017(3) -0.019(4) C10 0.031(3) 0.036(3) 0.014(3) -0.004(2) 0.000(3) 0.003(3) C11 0.028(3) 0.033(3) 0.013(3) 0.000(3) -0.005(2) -0.001(3) C12 0.028(3) 0.029(3) 0.019(3) -0.002(2) -0.002(2) -0.002(3) C13 0.034(4) 0.023(3) 0.016(3) 0.004(2) -0.005(2) 0.000(2) C14 0.030(3) 0.033(3) 0.017(3) -0.003(3) -0.001(2) 0.004(3) C15 0.048(4) 0.049(5) 0.012(3) 0.002(3) 0.000(3) 0.012(3) C16 0.054(5) 0.063(5) 0.015(3) 0.008(3) 0.006(3) 0.008(4) C17 0.036(4) 0.051(4) 0.016(3) -0.002(3) 0.003(3) 0.006(3) C18 0.038(4) 0.032(3) 0.015(3) -0.002(2) -0.008(3) 0.006(3) C19 0.036(4) 0.034(3) 0.013(3) -0.002(2) -0.005(3) 0.002(3) C20 0.036(4) 0.031(3) 0.020(3) -0.001(3) -0.005(3) 0.000(3) C21 0.032(3) 0.037(4) 0.019(3) -0.005(3) -0.003(3) 0.002(3) C22 0.028(3) 0.036(4) 0.032(4) -0.008(3) -0.001(3) 0.004(3) C23 0.037(4) 0.039(4) 0.019(3) 0.001(3) 0.001(3) 0.006(3) C24 0.033(4) 0.041(4) 0.026(3) 0.000(3) -0.002(3) 0.012(3) Cd1 0.0242(2) 0.0242(2) 0.0242(3) -0.00351(19) 0.00351(19) -0.0029(3) Cl1 0.0806(14) 0.0806(14) 0.0405(15) -0.0042(14) 0.0042(14) -0.0190(18) Cl2 0.061(2) 0.053(2) 0.040(2) -0.016(2) -0.018(2) 0.0189(19) N1 0.029(3) 0.030(3) 0.033(3) -0.008(3) -0.006(3) 0.006(2) N2 0.034(3) 0.034(3) 0.028(3) -0.002(3) 0.004(2) -0.001(3) N3 0.031(3) 0.028(3) 0.036(3) -0.006(2) 0.004(2) -0.002(2) N4 0.033(3) 0.037(3) 0.018(2) -0.009(2) -0.007(2) 0.006(3) N5 0.037(4) 0.084(6) 0.058(5) -0.045(4) -0.019(3) 0.016(4) N6 0.034(3) 0.028(3) 0.029(3) -0.005(2) -0.008(2) 0.003(2) O3 0.141(8) 0.095(7) 0.045(4) -0.021(4) -0.027(5) 0.033(5) O4 0.085(4) 0.085(4) 0.058(6) 0.006(5) 0.006(5) 0.020(6) O5 0.096(13) 0.087(13) 0.21(2) -0.048(17) -0.008(18) 0.030(11) O1 0.068(7) 0.095(8) 0.065(7) -0.031(7) -0.005(6) -0.004(6) O2 0.139(11) 0.153(11) 0.097(10) 0.029(9) -0.035(8) -0.018(9) O1' 0.177(13) 0.146(12) 0.165(13) -0.003(10) 0.022(10) 0.015(9) O2' 0.172(13) 0.167(13) 0.153(13) 0.037(9) 0.022(9) 0.011(9) C25' 0.199(12) 0.201(12) 0.200(12) -0.004(5) -0.004(5) -0.002(5) Cl4 0.096(5) 0.107(5) 0.068(4) -0.007(3) 0.002(3) -0.008(4) Cl4' 0.289(11) 0.272(12) 0.276(12) 0.002(7) 0.001(7) -0.005(7) C25 0.199(12) 0.201(12) 0.200(12) -0.004(5) -0.004(5) -0.002(5) Cl3 0.159(9) 0.278(15) 0.104(6) -0.088(8) -0.073(6) 0.140(10) Cl3' 0.297(13) 0.311(13) 0.297(13) 0.013(7) 0.001(7) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(9) . ? C1 C2 1.360(10) . ? C1 H1 0.9500 . ? C2 C3 1.421(9) . ? C2 H2 0.9500 . ? C3 C4 1.400(9) . ? C3 C6 1.476(10) . ? C4 C5 1.355(10) . ? C4 H4 0.9500 . ? C5 N1 1.339(9) . ? C5 H5 0.9500 . ? C6 C7 1.389(10) . ? C6 C11 1.411(9) . ? C7 C8 1.359(11) . ? C7 H7 0.9500 . ? C8 C9 1.385(10) . ? C8 H8 0.9500 . ? C9 C10 1.398(10) . ? C9 H9 0.9500 . ? C10 C11 1.375(9) . ? C10 C12 1.470(8) . ? C11 H11 0.9500 . ? C12 N2 1.306(8) . ? C12 N4 1.369(8) . ? C13 N3 1.302(9) . ? C13 N4 1.359(8) . ? C13 C14 1.475(9) . ? C14 C15 1.400(9) . ? C14 C19 1.410(9) . ? C15 C16 1.387(11) . ? C15 H15 0.9500 . ? C16 C17 1.354(11) . ? C16 H16 0.9500 . ? C17 C18 1.406(9) . ? C17 H17 0.9500 . ? C18 C19 1.379(9) . ? C18 C20 1.478(9) . ? C19 H19 0.9500 . ? C20 C21 1.369(10) . ? C20 C24 1.414(10) . ? C21 C22 1.394(10) . ? C21 H21 0.9500 . ? C22 N6 1.327(9) . ? C22 H22 0.9500 . ? C23 N6 1.332(9) . ? C23 C24 1.397(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cd1 N3 2.326(6) . ? Cd1 N3 2.326(6) 7 ? Cd1 N6 2.368(5) 3_544 ? Cd1 N6 2.368(5) 6_455 ? Cd1 N1 2.416(6) 3_644 ? Cd1 N1 2.416(6) 6_465 ? Cl1 O2 1.403(10) . ? Cl1 O2 1.403(10) 7 ? Cl1 O1' 1.41(3) 7 ? Cl1 O1' 1.41(3) . ? Cl1 O1 1.419(15) . ? Cl1 O1 1.419(15) 7 ? Cl1 O2' 1.435(10) 7 ? Cl1 O2' 1.435(10) . ? Cl2 Cl2 1.013(9) 8_665 ? Cl2 O3 1.349(8) . ? Cl2 O5 1.39(2) . ? Cl2 O4 1.403(10) . ? Cl2 O3 1.511(10) 8_665 ? N1 Cd1 2.416(6) 4_565 ? N2 N3 1.384(8) . ? N4 N5 1.408(8) . ? N5 H5A 0.8835 . ? N5 H5B 0.8875 . ? N6 Cd1 2.368(5) 4 ? O3 Cl2 1.511(10) 8_665 ? O4 Cl2 1.403(10) 8_665 ? O2' O2' 1.37(5) 7 ? C25' Cl4' 1.675(10) . ? C25' Cl4 1.706(10) . ? C25' H25A 0.9900 . ? C25' H25B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 125.4(6) . . ? N1 C1 H1 117.3 . . ? C2 C1 H1 117.3 . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 115.0(6) . . ? C4 C3 C6 123.1(6) . . ? C2 C3 C6 121.8(6) . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N1 C5 C4 124.4(6) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C7 C6 C11 117.8(6) . . ? C7 C6 C3 122.7(6) . . ? C11 C6 C3 119.4(6) . . ? C8 C7 C6 121.0(7) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 121.5(7) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C10 118.7(7) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C11 C10 C9 119.9(6) . . ? C11 C10 C12 122.2(6) . . ? C9 C10 C12 117.8(6) . . ? C10 C11 C6 121.0(6) . . ? C10 C11 H11 119.5 . . ? C6 C11 H11 119.5 . . ? N2 C12 N4 109.1(5) . . ? N2 C12 C10 123.6(6) . . ? N4 C12 C10 127.2(6) . . ? N3 C13 N4 108.3(6) . . ? N3 C13 C14 129.1(6) . . ? N4 C13 C14 122.4(6) . . ? C15 C14 C19 120.2(6) . . ? C15 C14 C13 121.8(6) . . ? C19 C14 C13 117.9(5) . . ? C16 C15 C14 116.6(7) . . ? C16 C15 H15 121.7 . . ? C14 C15 H15 121.7 . . ? C17 C16 C15 124.0(7) . . ? C17 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? C16 C17 C18 119.5(7) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 118.5(6) . . ? C19 C18 C20 119.7(6) . . ? C17 C18 C20 121.7(6) . . ? C18 C19 C14 121.1(6) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C21 C20 C24 115.7(6) . . ? C21 C20 C18 124.4(6) . . ? C24 C20 C18 119.9(6) . . ? C20 C21 C22 121.0(6) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? N6 C22 C21 123.1(6) . . ? N6 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? N6 C23 C24 123.5(6) . . ? N6 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C20 119.2(6) . . ? C23 C24 H24 120.4 . . ? C20 C24 H24 120.4 . . ? N3 Cd1 N3 82.5(3) . 7 ? N3 Cd1 N6 159.95(19) . 3_544 ? N3 Cd1 N6 88.22(19) 7 3_544 ? N3 Cd1 N6 88.22(19) . 6_455 ? N3 Cd1 N6 159.95(19) 7 6_455 ? N6 Cd1 N6 105.7(3) 3_544 6_455 ? N3 Cd1 N1 88.42(19) . 3_644 ? N3 Cd1 N1 110.03(19) 7 3_644 ? N6 Cd1 N1 78.1(2) 3_544 3_644 ? N6 Cd1 N1 87.3(2) 6_455 3_644 ? N3 Cd1 N1 110.03(19) . 6_465 ? N3 Cd1 N1 88.42(19) 7 6_465 ? N6 Cd1 N1 87.3(2) 3_544 6_465 ? N6 Cd1 N1 78.1(2) 6_455 6_465 ? N1 Cd1 N1 155.8(2) 3_644 6_465 ? O2 Cl1 O2 138(2) . 7 ? O2 Cl1 O1' 73.7(18) . 7 ? O2 Cl1 O1' 137.0(19) 7 7 ? O2 Cl1 O1' 137.0(19) . . ? O2 Cl1 O1' 73.7(18) 7 . ? O1' Cl1 O1' 101(3) 7 . ? O2 Cl1 O1 88.8(13) . . ? O2 Cl1 O1 101.1(13) 7 . ? O1' Cl1 O1 108.3(15) 7 . ? O1' Cl1 O1 51.5(15) . . ? O2 Cl1 O1 101.1(13) . 7 ? O2 Cl1 O1 88.8(13) 7 7 ? O1' Cl1 O1 51.5(15) 7 7 ? O1' Cl1 O1 108.3(15) . 7 ? O1 Cl1 O1 151.9(14) . 7 ? O2 Cl1 O2' 95.8(19) . 7 ? O2 Cl1 O2' 43.5(13) 7 7 ? O1' Cl1 O2' 134.6(19) 7 7 ? O1' Cl1 O2' 114.6(19) . 7 ? O1 Cl1 O2' 115.7(15) . 7 ? O1 Cl1 O2' 89.7(15) 7 7 ? O2 Cl1 O2' 43.5(13) . . ? O2 Cl1 O2' 95.8(19) 7 . ? O1' Cl1 O2' 114.6(19) 7 . ? O1' Cl1 O2' 134.6(19) . . ? O1 Cl1 O2' 89.7(15) . . ? O1 Cl1 O2' 115.7(15) 7 . ? O2' Cl1 O2' 57(2) 7 . ? Cl2 Cl2 O3 78.1(7) 8_665 . ? Cl2 Cl2 O5 165.2(13) 8_665 . ? O3 Cl2 O5 116.7(13) . . ? Cl2 Cl2 O4 68.8(2) 8_665 . ? O3 Cl2 O4 115.0(5) . . ? O5 Cl2 O4 103.2(8) . . ? Cl2 Cl2 O3 60.9(6) 8_665 8_665 ? O3 Cl2 O3 104.2(6) . 8_665 ? O5 Cl2 O3 111.8(13) . 8_665 ? O4 Cl2 O3 105.6(5) . 8_665 ? C1 N1 C5 115.2(6) . . ? C1 N1 Cd1 128.0(4) . 4_565 ? C5 N1 Cd1 116.5(4) . 4_565 ? C12 N2 N3 106.9(5) . . ? C13 N3 N2 109.0(5) . . ? C13 N3 Cd1 137.2(5) . . ? N2 N3 Cd1 111.9(4) . . ? C13 N4 C12 106.6(5) . . ? C13 N4 N5 127.0(6) . . ? C12 N4 N5 126.3(5) . . ? N4 N5 H5A 120.8 . . ? N4 N5 H5B 99.2 . . ? H5A N5 H5B 105.3 . . ? C22 N6 C23 116.7(6) . . ? C22 N6 Cd1 125.7(5) . 4 ? C23 N6 Cd1 115.2(4) . 4 ? Cl2 O3 Cl2 41.0(4) . 8_665 ? Cl2 O4 Cl2 42.3(5) 8_665 . ? O2' O2' Cl1 61.6(12) 7 . ? Cl4' C25' Cl4 113.8(14) . . ? Cl4' C25' H25A 108.8 . . ? Cl4 C25' H25A 108.8 . . ? Cl4' C25' H25B 108.8 . . ? Cl4 C25' H25B 108.8 . . ? H25A C25' H25B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.0(12) . . . . ? C1 C2 C3 C4 -1.4(10) . . . . ? C1 C2 C3 C6 175.1(7) . . . . ? C2 C3 C4 C5 1.5(11) . . . . ? C6 C3 C4 C5 -175.0(7) . . . . ? C3 C4 C5 N1 -0.2(12) . . . . ? C4 C3 C6 C7 -159.8(7) . . . . ? C2 C3 C6 C7 24.0(11) . . . . ? C4 C3 C6 C11 20.5(10) . . . . ? C2 C3 C6 C11 -155.8(7) . . . . ? C11 C6 C7 C8 -0.4(12) . . . . ? C3 C6 C7 C8 179.8(8) . . . . ? C6 C7 C8 C9 2.2(15) . . . . ? C7 C8 C9 C10 -1.8(14) . . . . ? C8 C9 C10 C11 -0.4(12) . . . . ? C8 C9 C10 C12 -177.7(8) . . . . ? C9 C10 C11 C6 2.1(10) . . . . ? C12 C10 C11 C6 179.3(6) . . . . ? C7 C6 C11 C10 -1.7(10) . . . . ? C3 C6 C11 C10 178.1(6) . . . . ? C11 C10 C12 N2 -148.6(7) . . . . ? C9 C10 C12 N2 28.7(10) . . . . ? C11 C10 C12 N4 30.2(10) . . . . ? C9 C10 C12 N4 -152.5(7) . . . . ? N3 C13 C14 C15 90.3(9) . . . . ? N4 C13 C14 C15 -95.5(8) . . . . ? N3 C13 C14 C19 -92.0(8) . . . . ? N4 C13 C14 C19 82.2(8) . . . . ? C19 C14 C15 C16 0.7(10) . . . . ? C13 C14 C15 C16 178.3(7) . . . . ? C14 C15 C16 C17 1.4(13) . . . . ? C15 C16 C17 C18 -2.1(13) . . . . ? C16 C17 C18 C19 0.7(11) . . . . ? C16 C17 C18 C20 -175.5(7) . . . . ? C17 C18 C19 C14 1.3(10) . . . . ? C20 C18 C19 C14 177.5(6) . . . . ? C15 C14 C19 C18 -2.0(10) . . . . ? C13 C14 C19 C18 -179.7(6) . . . . ? C19 C18 C20 C21 -162.2(7) . . . . ? C17 C18 C20 C21 13.9(10) . . . . ? C19 C18 C20 C24 17.1(10) . . . . ? C17 C18 C20 C24 -166.8(7) . . . . ? C24 C20 C21 C22 -5.1(10) . . . . ? C18 C20 C21 C22 174.2(6) . . . . ? C20 C21 C22 N6 -2.5(11) . . . . ? N6 C23 C24 C20 -1.6(11) . . . . ? C21 C20 C24 C23 7.0(10) . . . . ? C18 C20 C24 C23 -172.5(6) . . . . ? C2 C1 N1 C5 1.3(11) . . . . ? C2 C1 N1 Cd1 -172.1(5) . . . 4_565 ? C4 C5 N1 C1 -1.2(11) . . . . ? C4 C5 N1 Cd1 173.0(6) . . . 4_565 ? N4 C12 N2 N3 -0.8(7) . . . . ? C10 C12 N2 N3 178.2(6) . . . . ? N4 C13 N3 N2 1.3(7) . . . . ? C14 C13 N3 N2 176.1(6) . . . . ? N4 C13 N3 Cd1 163.6(5) . . . . ? C14 C13 N3 Cd1 -21.6(11) . . . . ? C12 N2 N3 C13 -0.3(7) . . . . ? C12 N2 N3 Cd1 -167.4(4) . . . . ? N3 Cd1 N3 C13 -66.1(6) 7 . . . ? N6 Cd1 N3 C13 -3.1(11) 3_544 . . . ? N6 Cd1 N3 C13 131.7(7) 6_455 . . . ? N1 Cd1 N3 C13 44.4(7) 3_644 . . . ? N1 Cd1 N3 C13 -151.6(6) 6_465 . . . ? N3 Cd1 N3 N2 95.8(4) 7 . . . ? N6 Cd1 N3 N2 158.8(5) 3_544 . . . ? N6 Cd1 N3 N2 -66.4(4) 6_455 . . . ? N1 Cd1 N3 N2 -153.7(4) 3_644 . . . ? N1 Cd1 N3 N2 10.3(5) 6_465 . . . ? N3 C13 N4 C12 -1.8(7) . . . . ? C14 C13 N4 C12 -177.0(6) . . . . ? N3 C13 N4 N5 174.9(7) . . . . ? C14 C13 N4 N5 -0.3(11) . . . . ? N2 C12 N4 C13 1.6(7) . . . . ? C10 C12 N4 C13 -177.3(6) . . . . ? N2 C12 N4 N5 -175.1(7) . . . . ? C10 C12 N4 N5 6.0(11) . . . . ? C21 C22 N6 C23 8.0(10) . . . . ? C21 C22 N6 Cd1 -153.8(5) . . . 4 ? C24 C23 N6 C22 -6.0(10) . . . . ? C24 C23 N6 Cd1 157.8(6) . . . 4 ? O5 Cl2 O3 Cl2 179.2(12) . . . 8_665 ? O4 Cl2 O3 Cl2 -59.6(4) . . . 8_665 ? O3 Cl2 O3 Cl2 55.5(5) 8_665 . . 8_665 ? O3 Cl2 O4 Cl2 64.9(6) . . . 8_665 ? O5 Cl2 O4 Cl2 -166.9(15) . . . 8_665 ? O3 Cl2 O4 Cl2 -49.5(6) 8_665 . . 8_665 ? O2 Cl1 O2' O2' -150(4) . . . 7 ? O2 Cl1 O2' O2' 20(3) 7 . . 7 ? O1' Cl1 O2' O2' -129(3) 7 . . 7 ? O1' Cl1 O2' O2' 93(3) . . . 7 ? O1 Cl1 O2' O2' 121(3) . . . 7 ? O1 Cl1 O2' O2' -71(3) 7 . . 7 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.268 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.130 # Attachment '3.cif' data_3''' _database_code_depnum_ccdc_archive 'CCDC 846268' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Cd Cl8 N12 O8' _chemical_formula_weight 1330.92 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8545(8) _cell_length_b 15.8545(8) _cell_length_c 21.596(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5428.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15880 _cell_measurement_theta_min 2.566 _cell_measurement_theta_max 28.095 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7820 _exptl_absorpt_correction_T_max 0.8603 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28920 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.60 _reflns_number_total 5121 _reflns_number_gt 4915 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0890P)^2^+14.6195P] 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(4) _refine_ls_number_reflns 5121 _refine_ls_number_parameters 399 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.092 _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 C1 C 0.0870(3) 0.8602(3) 0.1087(2) 0.0263(11) Uani 1 1 d . . . H1 H 0.0370 0.8896 0.0977 0.032 Uiso 1 1 calc R . . C2 C 0.1162(4) 0.7986(4) 0.0690(2) 0.0269(11) Uani 1 1 d . . . H2 H 0.0861 0.7859 0.0321 0.032 Uiso 1 1 calc R . . C3 C 0.1899(4) 0.7553(3) 0.0833(2) 0.0257(11) Uani 1 1 d . . . C4 C 0.2340(3) 0.7829(4) 0.1357(2) 0.0287(12) Uani 1 1 d . . . H4 H 0.2878 0.7597 0.1451 0.034 Uiso 1 1 calc R . . C5 C 0.1996(4) 0.8432(4) 0.1733(2) 0.0278(11) Uani 1 1 d . . . H5 H 0.2302 0.8592 0.2092 0.033 Uiso 1 1 calc R . . C6 C 0.2211(3) 0.6827(3) 0.0461(2) 0.0237(10) Uani 1 1 d . . . C7 C 0.1902(3) 0.6644(4) -0.0133(2) 0.0263(12) Uani 1 1 d . . . H7 H 0.1485 0.6998 -0.0313 0.032 Uiso 1 1 calc R . . C8 C 0.2193(4) 0.5963(4) -0.0454(3) 0.0330(13) Uani 1 1 d . . . H8 H 0.1988 0.5861 -0.0861 0.040 Uiso 1 1 calc R . . C9 C 0.2783(4) 0.5416(4) -0.0201(3) 0.0302(12) Uani 1 1 d . . . H9 H 0.2962 0.4928 -0.0420 0.036 Uiso 1 1 calc R . . C10 C 0.3105(3) 0.5599(3) 0.0384(2) 0.0228(10) Uani 1 1 d . . . C11 C 0.2815(3) 0.6292(3) 0.0715(2) 0.0240(11) Uani 1 1 d . . . H11 H 0.3030 0.6402 0.1117 0.029 Uiso 1 1 calc R . . C12 C 0.3728(3) 0.5040(3) 0.0692(2) 0.0221(10) Uani 1 1 d . . . C13 C 0.4236(3) 0.4093(3) 0.1320(2) 0.0217(10) Uani 1 1 d . . . C14 C 0.4326(4) 0.3389(3) 0.1764(2) 0.0254(11) Uani 1 1 d . . . C15 C 0.5043(4) 0.3373(4) 0.2130(3) 0.0336(13) Uani 1 1 d . . . H15 H 0.5452 0.3809 0.2100 0.040 Uiso 1 1 calc R . . C16 C 0.5158(4) 0.2708(4) 0.2544(3) 0.0383(14) Uani 1 1 d . . . H16 H 0.5652 0.2682 0.2793 0.046 Uiso 1 1 calc R . . C17 C 0.4550(4) 0.2085(4) 0.2590(3) 0.0351(13) Uani 1 1 d . . . H17 H 0.4627 0.1641 0.2880 0.042 Uiso 1 1 calc R . . C18 C 0.3833(3) 0.2093(3) 0.2225(2) 0.0238(11) Uani 1 1 d . . . C19 C 0.3734(3) 0.2754(3) 0.1807(2) 0.0245(11) Uani 1 1 d . . . H19 H 0.3251 0.2768 0.1547 0.029 Uiso 1 1 calc R . . C20 C 0.3179(4) 0.1425(4) 0.2281(2) 0.0261(12) Uani 1 1 d . . . C21 C 0.3086(3) 0.0947(4) 0.2816(3) 0.0275(11) Uani 1 1 d . . . H21 H 0.3476 0.1010 0.3147 0.033 Uiso 1 1 calc R . . C22 C 0.2430(4) 0.0382(3) 0.2869(3) 0.0290(12) Uani 1 1 d . . . H22 H 0.2378 0.0068 0.3242 0.035 Uiso 1 1 calc R . . C23 C 0.1963(4) 0.0689(4) 0.1896(2) 0.0289(11) Uani 1 1 d . . . H23 H 0.1574 0.0595 0.1569 0.035 Uiso 1 1 calc R . . C24 C 0.2602(4) 0.1268(4) 0.1805(3) 0.0287(12) Uani 1 1 d . . . H24 H 0.2650 0.1557 0.1421 0.034 Uiso 1 1 calc R . . Cd1 Cd 0.55898(2) 0.55898(2) 0.0000 0.01914(15) Uani 1 2 d S . . Cl1 Cl 0.37550(13) 0.62450(13) 0.2500 0.0650(8) Uani 1 2 d SD . . Cl2 Cl 0.26882(12) 0.26882(12) 0.0000 0.0757(10) Uani 1 2 d SD . . Cl3 Cl 0.0639(3) 0.4158(2) 0.40464(14) 0.1027(10) Uani 1 1 d D . . C25 C 0.0406(6) 0.4644(6) 0.3360(4) 0.115(5) Uani 0.50 1 d PD A 3 H25 H 0.0190 0.4248 0.3036 0.138 Uiso 0.50 1 calc PR A 3 Cl4 Cl 0.1211(3) 0.5277(3) 0.31035(16) 0.0532(9) Uani 0.50 1 d PD A 3 Cl5 Cl -0.0365(7) 0.5249(8) 0.3688(7) 0.204(5) Uani 0.50 1 d PDU A 3 C25' C 0.0406(6) 0.4644(6) 0.3360(4) 0.115(5) Uani 0.50 1 d PD A 4 H25' H 0.0905 0.4475 0.3105 0.138 Uiso 0.50 1 calc PR A 4 Cl4' Cl 0.0426(8) 0.5706(5) 0.3269(4) 0.146(3) Uani 0.50 1 d PDU A 4 Cl5' Cl -0.0394(4) 0.4196(3) 0.2944(2) 0.0848(16) Uani 0.50 1 d PD A 4 N1 N 0.1256(3) 0.8812(3) 0.1625(2) 0.0261(9) Uani 1 1 d . . . N2 N 0.4559(3) 0.5063(3) 0.0655(2) 0.0244(9) Uani 1 1 d . . . N3 N 0.4882(3) 0.4461(3) 0.1046(2) 0.0254(9) Uani 1 1 d . . . N4 N 0.3508(3) 0.4440(3) 0.1112(2) 0.0255(9) Uani 1 1 d . . . N5 N 0.2689(3) 0.4260(4) 0.1318(3) 0.0473(16) Uani 1 1 d . . . H5A H 0.2402 0.4712 0.1432 0.057 Uiso 1 1 d R . . H5B H 0.2405 0.4141 0.0975 0.057 Uiso 1 1 d R . . N6 N 0.1864(3) 0.0255(3) 0.2420(2) 0.0253(9) Uani 1 1 d . . . O3 O 0.2268(5) 0.2452(8) 0.0523(3) 0.117(4) Uani 1 1 d . . . O4 O 0.3299(5) 0.3299(5) 0.0000 0.115(4) Uani 1 2 d S . . O5 O 0.2131(10) 0.3372(13) -0.0207(18) 0.230(19) Uani 0.50 1 d PD . . O2 O 0.401(2) 0.5465(8) 0.2231(8) 0.22(2) Uani 0.50 1 d PD B 1 O2' O 0.414(2) 0.6096(14) 0.3059(7) 0.155(11) Uani 0.50 1 d PD B 2 O1 O 0.3163(14) 0.5993(9) 0.2954(9) 0.111(7) Uani 0.50 1 d PD B . O1' O 0.2861(7) 0.6147(18) 0.2424(12) 0.169(12) Uani 0.50 1 d PD B . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.026(3) 0.028(3) 0.005(2) 0.004(2) 0.005(2) C2 0.032(3) 0.033(3) 0.016(2) 0.001(2) -0.001(2) 0.002(2) C3 0.030(3) 0.022(3) 0.025(2) 0.005(2) 0.004(2) 0.001(2) C4 0.024(3) 0.036(3) 0.027(3) 0.002(2) 0.001(2) 0.008(2) C5 0.026(3) 0.032(3) 0.025(3) -0.003(2) -0.001(2) 0.002(2) C6 0.023(3) 0.025(3) 0.023(2) 0.000(2) 0.007(2) -0.001(2) C7 0.021(2) 0.032(3) 0.026(3) 0.004(2) -0.001(2) 0.004(2) C8 0.037(3) 0.040(3) 0.022(3) -0.007(2) -0.007(2) 0.001(3) C9 0.031(3) 0.032(3) 0.028(3) -0.006(2) 0.000(2) 0.006(2) C10 0.023(2) 0.020(2) 0.026(2) 0.003(2) 0.0049(19) 0.000(2) C11 0.024(3) 0.027(3) 0.021(2) 0.000(2) 0.001(2) -0.002(2) C12 0.024(3) 0.021(2) 0.021(2) -0.003(2) 0.005(2) -0.0001(19) C13 0.024(3) 0.022(2) 0.019(2) -0.0029(18) 0.0016(18) -0.0018(19) C14 0.027(3) 0.029(3) 0.020(2) 0.001(2) 0.004(2) 0.005(2) C15 0.030(3) 0.037(3) 0.033(3) 0.009(3) -0.007(2) -0.013(2) C16 0.026(3) 0.049(3) 0.041(3) 0.017(3) -0.010(3) -0.011(2) C17 0.031(3) 0.039(3) 0.035(3) 0.015(3) -0.007(3) -0.001(2) C18 0.021(2) 0.027(3) 0.023(2) 0.003(2) 0.002(2) 0.000(2) C19 0.025(3) 0.023(3) 0.025(2) -0.002(2) 0.001(2) 0.000(2) C20 0.024(3) 0.025(3) 0.029(3) 0.002(2) 0.004(2) 0.005(2) C21 0.025(3) 0.032(3) 0.026(3) 0.004(2) -0.006(2) 0.001(2) C22 0.034(3) 0.028(3) 0.025(3) 0.008(2) -0.002(2) -0.002(2) C23 0.030(3) 0.027(3) 0.029(3) 0.005(2) -0.003(2) -0.001(2) C24 0.030(3) 0.030(3) 0.025(3) 0.003(2) -0.001(2) -0.002(2) Cd1 0.01841(17) 0.01841(17) 0.0206(2) 0.00173(15) -0.00173(15) -0.00256(18) Cl1 0.0797(12) 0.0797(12) 0.0357(12) 0.0037(11) 0.0037(11) 0.0213(15) Cl2 0.0905(15) 0.0905(15) 0.0462(14) 0.0069(14) -0.0069(14) -0.0533(19) Cl3 0.133(3) 0.093(2) 0.0825(18) -0.0036(15) -0.0144(19) -0.0256(19) C25 0.114(11) 0.113(11) 0.119(11) 0.002(9) -0.004(8) -0.036(8) Cl4 0.062(2) 0.065(2) 0.0329(16) -0.0086(15) 0.0027(15) -0.0163(18) Cl5 0.137(7) 0.192(8) 0.284(10) 0.064(8) 0.022(7) -0.008(6) C25' 0.114(11) 0.113(11) 0.119(11) 0.002(9) -0.004(8) -0.036(8) Cl4' 0.216(8) 0.110(5) 0.113(5) 0.015(4) -0.061(5) 0.007(6) Cl5' 0.115(4) 0.069(3) 0.071(3) 0.002(2) -0.045(3) -0.013(3) N1 0.031(3) 0.019(2) 0.028(2) 0.0025(19) 0.002(2) 0.0021(17) N2 0.027(2) 0.020(2) 0.027(2) 0.0018(17) 0.0008(18) -0.0012(16) N3 0.027(2) 0.024(2) 0.025(2) -0.0025(19) 0.0000(17) -0.0011(19) N4 0.020(2) 0.025(2) 0.031(2) 0.004(2) 0.0082(17) 0.0024(19) N5 0.024(2) 0.053(3) 0.065(4) 0.038(3) 0.017(2) 0.008(2) N6 0.022(2) 0.026(2) 0.028(2) 0.0020(19) 0.0043(19) 0.0022(17) O3 0.082(5) 0.210(11) 0.059(4) 0.022(6) 0.001(4) -0.047(6) O4 0.107(6) 0.107(6) 0.132(10) -0.030(8) 0.030(8) -0.051(7) O5 0.104(15) 0.149(19) 0.44(5) 0.21(3) 0.03(2) 0.001(13) O2 0.53(6) 0.071(11) 0.065(10) -0.010(9) 0.15(2) 0.03(2) O2' 0.30(4) 0.143(17) 0.028(7) 0.027(9) -0.058(12) -0.05(2) O1 0.178(19) 0.051(8) 0.103(13) -0.006(8) 0.073(13) -0.008(10) O1' 0.074(11) 0.26(3) 0.17(2) 0.15(2) -0.010(12) -0.054(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.355(7) . ? C1 C2 1.380(8) . ? C1 H1 0.9500 . ? C2 C3 1.390(8) . ? C2 H2 0.9500 . ? C3 C4 1.400(8) . ? C3 C6 1.488(7) . ? C4 C5 1.368(8) . ? C4 H4 0.9500 . ? C5 N1 1.339(7) . ? C5 H5 0.9500 . ? C6 C11 1.391(8) . ? C6 C7 1.403(7) . ? C7 C8 1.364(8) . ? C7 H7 0.9500 . ? C8 C9 1.388(9) . ? C8 H8 0.9500 . ? C9 C10 1.392(7) . ? C9 H9 0.9500 . ? C10 C11 1.390(7) . ? C10 C12 1.485(7) . ? C11 H11 0.9500 . ? C12 N2 1.321(7) . ? C12 N4 1.360(7) . ? C13 N3 1.319(6) . ? C13 N4 1.354(7) . ? C13 C14 1.479(7) . ? C14 C19 1.380(8) . ? C14 C15 1.385(8) . ? C15 C16 1.393(8) . ? C15 H15 0.9500 . ? C16 C17 1.384(8) . ? C16 H16 0.9500 . ? C17 C18 1.383(8) . ? C17 H17 0.9500 . ? C18 C19 1.392(7) . ? C18 C20 1.487(8) . ? C19 H19 0.9500 . ? C20 C21 1.390(7) . ? C20 C24 1.400(8) . ? C21 C22 1.377(8) . ? C21 H21 0.9500 . ? C22 N6 1.335(7) . ? C22 H22 0.9500 . ? C23 N6 1.334(7) . ? C23 C24 1.381(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cd1 N2 2.317(4) 7 ? Cd1 N2 2.317(4) . ? Cd1 N1 2.363(4) 6_565 ? Cd1 N1 2.363(4) 3_654 ? Cd1 N6 2.431(4) 6 ? Cd1 N6 2.431(4) 3_554 ? Cl1 O2' 1.377(9) . ? Cl1 O2' 1.377(9) 8_665 ? Cl1 O1 1.415(9) . ? Cl1 O1 1.415(9) 8_665 ? Cl1 O2 1.427(9) . ? Cl1 O2 1.427(9) 8_665 ? Cl1 O1' 1.435(9) . ? Cl1 O1' 1.435(9) 8_665 ? Cl2 O3 1.363(7) 7 ? Cl2 O3 1.363(7) . ? Cl2 O4 1.369(10) . ? Cl2 O5 1.468(10) 7 ? Cl2 O5 1.468(10) . ? Cl3 C25 1.711(6) . ? C25 Cl5 1.709(9) . ? C25 Cl4 1.716(8) . ? C25 H25 1.0000 . ? N1 Cd1 2.363(4) 4_465 ? N2 N3 1.374(6) . ? N4 N5 1.403(6) . ? N5 H5A 0.8828 . ? N5 H5B 0.8865 . ? N6 Cd1 2.431(4) 4_455 ? O2 O2 1.65(6) 8_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.7(5) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 119.6(5) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 116.4(5) . . ? C2 C3 C6 122.8(5) . . ? C4 C3 C6 120.8(5) . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 124.1(5) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? C11 C6 C7 118.3(5) . . ? C11 C6 C3 119.2(5) . . ? C7 C6 C3 122.5(5) . . ? C8 C7 C6 120.7(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.4(5) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C10 118.3(5) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 120.7(5) . . ? C11 C10 C12 117.5(4) . . ? C9 C10 C12 121.8(5) . . ? C10 C11 C6 120.5(5) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? N2 C12 N4 108.4(4) . . ? N2 C12 C10 128.3(5) . . ? N4 C12 C10 123.1(4) . . ? N3 C13 N4 109.5(4) . . ? N3 C13 C14 123.3(5) . . ? N4 C13 C14 127.2(4) . . ? C19 C14 C15 120.4(5) . . ? C19 C14 C13 121.9(5) . . ? C15 C14 C13 117.7(5) . . ? C14 C15 C16 119.2(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 121.6(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 118.0(5) . . ? C17 C18 C20 121.3(5) . . ? C19 C18 C20 120.7(5) . . ? C14 C19 C18 121.0(5) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C24 116.4(5) . . ? C21 C20 C18 122.1(5) . . ? C24 C20 C18 121.5(5) . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? N6 C22 C21 123.0(5) . . ? N6 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? N6 C23 C24 123.4(5) . . ? N6 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C20 119.5(5) . . ? C23 C24 H24 120.3 . . ? C20 C24 H24 120.3 . . ? N2 Cd1 N2 82.2(2) 7 . ? N2 Cd1 N1 158.78(15) 7 6_565 ? N2 Cd1 N1 88.38(15) . 6_565 ? N2 Cd1 N1 88.38(15) 7 3_654 ? N2 Cd1 N1 158.78(15) . 3_654 ? N1 Cd1 N1 106.3(2) 6_565 3_654 ? N2 Cd1 N6 87.37(15) 7 6 ? N2 Cd1 N6 110.15(15) . 6 ? N1 Cd1 N6 78.05(16) 6_565 6 ? N1 Cd1 N6 88.24(16) 3_654 6 ? N2 Cd1 N6 110.15(15) 7 3_554 ? N2 Cd1 N6 87.37(15) . 3_554 ? N1 Cd1 N6 88.24(16) 6_565 3_554 ? N1 Cd1 N6 78.05(16) 3_654 3_554 ? N6 Cd1 N6 157.1(2) 6 3_554 ? O2' Cl1 O2' 128(2) . 8_665 ? O2' Cl1 O1 68.9(13) . . ? O2' Cl1 O1 126.6(12) 8_665 . ? O2' Cl1 O1 126.6(12) . 8_665 ? O2' Cl1 O1 68.9(13) 8_665 8_665 ? O1 Cl1 O1 148.7(17) . 8_665 ? O2' Cl1 O2 94.6(16) . . ? O2' Cl1 O2 37.4(13) 8_665 . ? O1 Cl1 O2 103.2(12) . . ? O1 Cl1 O2 102.2(12) 8_665 . ? O2' Cl1 O2 37.4(13) . 8_665 ? O2' Cl1 O2 94.6(16) 8_665 8_665 ? O1 Cl1 O2 102.2(12) . 8_665 ? O1 Cl1 O2 103.2(12) 8_665 8_665 ? O2 Cl1 O2 71(3) . 8_665 ? O2' Cl1 O1' 121.6(15) . . ? O2' Cl1 O1' 91.2(16) 8_665 . ? O1 Cl1 O1' 52.7(13) . . ? O1 Cl1 O1' 105.7(9) 8_665 . ? O2 Cl1 O1' 98(2) . . ? O2 Cl1 O1' 150.6(14) 8_665 . ? O2' Cl1 O1' 91.2(16) . 8_665 ? O2' Cl1 O1' 121.6(15) 8_665 8_665 ? O1 Cl1 O1' 105.7(9) . 8_665 ? O1 Cl1 O1' 52.7(13) 8_665 8_665 ? O2 Cl1 O1' 150.6(14) . 8_665 ? O2 Cl1 O1' 98(2) 8_665 8_665 ? O1' Cl1 O1' 103(2) . 8_665 ? O3 Cl2 O3 114.6(8) 7 . ? O3 Cl2 O4 122.7(4) 7 . ? O3 Cl2 O4 122.7(4) . . ? O3 Cl2 O5 99.3(13) 7 7 ? O3 Cl2 O5 86.8(17) . 7 ? O4 Cl2 O5 84.4(9) . 7 ? O3 Cl2 O5 86.8(17) 7 . ? O3 Cl2 O5 99.3(13) . . ? O4 Cl2 O5 84.4(9) . . ? O5 Cl2 O5 168.9(18) 7 . ? Cl5 C25 Cl3 92.7(7) . . ? Cl5 C25 Cl4 109.7(6) . . ? Cl3 C25 Cl4 112.5(5) . . ? Cl5 C25 H25 113.4 . . ? Cl3 C25 H25 113.4 . . ? Cl4 C25 H25 113.4 . . ? C5 N1 C1 115.7(5) . . ? C5 N1 Cd1 115.7(3) . 4_465 ? C1 N1 Cd1 125.6(4) . 4_465 ? C12 N2 N3 108.4(4) . . ? C12 N2 Cd1 138.7(4) . . ? N3 N2 Cd1 111.3(3) . . ? C13 N3 N2 107.0(4) . . ? C13 N4 C12 106.7(4) . . ? C13 N4 N5 126.9(4) . . ? C12 N4 N5 126.2(4) . . ? N4 N5 H5A 113.6 . . ? N4 N5 H5B 104.4 . . ? H5A N5 H5B 98.2 . . ? C23 N6 C22 117.3(5) . . ? C23 N6 Cd1 116.2(4) . 4_455 ? C22 N6 Cd1 126.1(4) . 4_455 ? Cl1 O2 O2 54.7(16) . 8_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.0(9) . . . . ? C1 C2 C3 C4 -5.2(8) . . . . ? C1 C2 C3 C6 174.0(5) . . . . ? C2 C3 C4 C5 6.7(8) . . . . ? C6 C3 C4 C5 -172.6(5) . . . . ? C3 C4 C5 N1 -2.1(9) . . . . ? C2 C3 C6 C11 -163.3(5) . . . . ? C4 C3 C6 C11 16.0(7) . . . . ? C2 C3 C6 C7 14.9(8) . . . . ? C4 C3 C6 C7 -165.9(5) . . . . ? C11 C6 C7 C8 -0.6(8) . . . . ? C3 C6 C7 C8 -178.8(5) . . . . ? C6 C7 C8 C9 2.0(9) . . . . ? C7 C8 C9 C10 -3.0(9) . . . . ? C8 C9 C10 C11 2.8(8) . . . . ? C8 C9 C10 C12 179.1(5) . . . . ? C9 C10 C11 C6 -1.5(8) . . . . ? C12 C10 C11 C6 -178.0(5) . . . . ? C7 C6 C11 C10 0.4(8) . . . . ? C3 C6 C11 C10 178.6(5) . . . . ? C11 C10 C12 N2 -94.4(6) . . . . ? C9 C10 C12 N2 89.2(7) . . . . ? C11 C10 C12 N4 80.2(7) . . . . ? C9 C10 C12 N4 -96.2(6) . . . . ? N3 C13 C14 C19 -146.4(5) . . . . ? N4 C13 C14 C19 30.9(8) . . . . ? N3 C13 C14 C15 31.9(7) . . . . ? N4 C13 C14 C15 -150.7(5) . . . . ? C19 C14 C15 C16 -0.2(9) . . . . ? C13 C14 C15 C16 -178.5(5) . . . . ? C14 C15 C16 C17 -1.1(10) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C16 C17 C18 C19 -0.4(9) . . . . ? C16 C17 C18 C20 -179.5(6) . . . . ? C15 C14 C19 C18 1.3(8) . . . . ? C13 C14 C19 C18 179.6(5) . . . . ? C17 C18 C19 C14 -1.0(8) . . . . ? C20 C18 C19 C14 178.2(5) . . . . ? C17 C18 C20 C21 23.0(8) . . . . ? C19 C18 C20 C21 -156.2(5) . . . . ? C17 C18 C20 C24 -159.6(6) . . . . ? C19 C18 C20 C24 21.2(8) . . . . ? C24 C20 C21 C22 -2.8(8) . . . . ? C18 C20 C21 C22 174.7(5) . . . . ? C20 C21 C22 N6 0.7(9) . . . . ? N6 C23 C24 C20 -0.6(9) . . . . ? C21 C20 C24 C23 2.8(8) . . . . ? C18 C20 C24 C23 -174.8(5) . . . . ? C4 C5 N1 C1 -4.1(8) . . . . ? C4 C5 N1 Cd1 157.6(5) . . . 4_465 ? C2 C1 N1 C5 5.6(8) . . . . ? C2 C1 N1 Cd1 -154.0(4) . . . 4_465 ? N4 C12 N2 N3 1.1(5) . . . . ? C10 C12 N2 N3 176.4(5) . . . . ? N4 C12 N2 Cd1 164.2(4) . . . . ? C10 C12 N2 Cd1 -20.5(9) . . . . ? N2 Cd1 N2 C12 -68.5(5) 7 . . . ? N1 Cd1 N2 C12 130.6(5) 6_565 . . . ? N1 Cd1 N2 C12 -4.0(8) 3_654 . . . ? N6 Cd1 N2 C12 -152.8(5) 6 . . . ? N6 Cd1 N2 C12 42.3(5) 3_554 . . . ? N2 Cd1 N2 N3 94.3(3) 7 . . . ? N1 Cd1 N2 N3 -66.7(3) 6_565 . . . ? N1 Cd1 N2 N3 158.7(4) 3_654 . . . ? N6 Cd1 N2 N3 10.0(4) 6 . . . ? N6 Cd1 N2 N3 -155.0(3) 3_554 . . . ? N4 C13 N3 N2 0.4(5) . . . . ? C14 C13 N3 N2 178.2(4) . . . . ? C12 N2 N3 C13 -0.9(5) . . . . ? Cd1 N2 N3 C13 -169.0(3) . . . . ? N3 C13 N4 C12 0.3(6) . . . . ? C14 C13 N4 C12 -177.4(5) . . . . ? N3 C13 N4 N5 -175.7(6) . . . . ? C14 C13 N4 N5 6.7(9) . . . . ? N2 C12 N4 C13 -0.9(6) . . . . ? C10 C12 N4 C13 -176.4(5) . . . . ? N2 C12 N4 N5 175.1(5) . . . . ? C10 C12 N4 N5 -0.4(8) . . . . ? C24 C23 N6 C22 -1.6(8) . . . . ? C24 C23 N6 Cd1 172.7(5) . . . 4_455 ? C21 C22 N6 C23 1.6(8) . . . . ? C21 C22 N6 Cd1 -172.1(4) . . . 4_455 ? O2' Cl1 O2 O2 -29.1(17) . . . 8_665 ? O2' Cl1 O2 O2 127(4) 8_665 . . 8_665 ? O1 Cl1 O2 O2 -98.5(17) . . . 8_665 ? O1 Cl1 O2 O2 99.9(12) 8_665 . . 8_665 ? O1' Cl1 O2 O2 -151.9(14) . . . 8_665 ? O1' Cl1 O2 O2 72(4) 8_665 . . 8_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.012 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.121 # Attachment '3.cif' data_3'' _database_code_depnum_ccdc_archive 'CCDC 846269' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Cd Cl8 N12 O8' _chemical_formula_weight 1330.92 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.8633(10) _cell_length_b 15.8633(10) _cell_length_c 21.586(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5431.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12729 _cell_measurement_theta_min 2.274 _cell_measurement_theta_max 27.663 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7821 _exptl_absorpt_correction_T_max 0.8817 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28914 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.60 _reflns_number_total 5124 _reflns_number_gt 4835 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0921P)^2^+16.6280P] 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(4) _refine_ls_number_reflns 5124 _refine_ls_number_parameters 399 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.081 _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 C1 C 0.4127(4) -0.3602(4) 0.1090(3) 0.0251(12) Uani 1 1 d . . . H1 H 0.4626 -0.3896 0.0980 0.030 Uiso 1 1 calc R . . C2 C 0.3838(4) -0.2986(4) 0.0692(3) 0.0253(12) Uani 1 1 d . . . H2 H 0.4141 -0.2859 0.0324 0.030 Uiso 1 1 calc R . . C3 C 0.3098(4) -0.2551(4) 0.0831(3) 0.0255(12) Uani 1 1 d . . . C4 C 0.2658(4) -0.2834(4) 0.1356(3) 0.0273(12) Uani 1 1 d . . . H4 H 0.2119 -0.2606 0.1450 0.033 Uiso 1 1 calc R . . C5 C 0.3002(4) -0.3433(4) 0.1732(3) 0.0254(12) Uani 1 1 d . . . H5 H 0.2696 -0.3592 0.2092 0.031 Uiso 1 1 calc R . . C6 C 0.2790(4) -0.1828(4) 0.0462(3) 0.0234(11) Uani 1 1 d . . . C7 C 0.3096(4) -0.1645(4) -0.0133(3) 0.0253(13) Uani 1 1 d . . . H7 H 0.3509 -0.2000 -0.0315 0.030 Uiso 1 1 calc R . . C8 C 0.2807(4) -0.0962(4) -0.0452(3) 0.0311(13) Uani 1 1 d . . . H8 H 0.3018 -0.0859 -0.0857 0.037 Uiso 1 1 calc R . . C9 C 0.2214(4) -0.0414(4) -0.0203(3) 0.0293(13) Uani 1 1 d . . . H9 H 0.2031 0.0070 -0.0425 0.035 Uiso 1 1 calc R . . C10 C 0.1896(3) -0.0600(4) 0.0386(2) 0.0223(11) Uani 1 1 d . . . C11 C 0.2185(4) -0.1289(4) 0.0713(3) 0.0235(12) Uani 1 1 d . . . H11 H 0.1968 -0.1398 0.1115 0.028 Uiso 1 1 calc R . . C12 C 0.1273(4) -0.0038(3) 0.0694(2) 0.0225(11) Uani 1 1 d . . . C13 C 0.0761(3) 0.0908(3) 0.1320(2) 0.0208(11) Uani 1 1 d . . . C14 C 0.0675(4) 0.1612(3) 0.1765(2) 0.0238(11) Uani 1 1 d . . . C15 C -0.0048(4) 0.1627(4) 0.2132(3) 0.0343(14) Uani 1 1 d . . . H15 H -0.0459 0.1193 0.2100 0.041 Uiso 1 1 calc R . . C16 C -0.0155(4) 0.2289(4) 0.2543(4) 0.0391(15) Uani 1 1 d . . . H16 H -0.0645 0.2311 0.2796 0.047 Uiso 1 1 calc R . . C17 C 0.0446(4) 0.2916(4) 0.2589(3) 0.0345(14) Uani 1 1 d . . . H17 H 0.0364 0.3363 0.2875 0.041 Uiso 1 1 calc R . . C18 C 0.1165(4) 0.2907(4) 0.2226(3) 0.0228(12) Uani 1 1 d . . . C19 C 0.1264(4) 0.2248(4) 0.1807(3) 0.0246(12) Uani 1 1 d . . . H19 H 0.1746 0.2237 0.1546 0.030 Uiso 1 1 calc R . . C20 C 0.1820(4) 0.3575(4) 0.2281(3) 0.0246(12) Uani 1 1 d . . . C21 C 0.1912(4) 0.4052(4) 0.2817(3) 0.0259(12) Uani 1 1 d . . . H21 H 0.1523 0.3988 0.3148 0.031 Uiso 1 1 calc R . . C22 C 0.2567(4) 0.4617(4) 0.2869(3) 0.0284(13) Uani 1 1 d . . . H22 H 0.2618 0.4931 0.3242 0.034 Uiso 1 1 calc R . . C23 C 0.3035(4) 0.4310(4) 0.1897(3) 0.0263(12) Uani 1 1 d . . . H23 H 0.3424 0.4400 0.1570 0.032 Uiso 1 1 calc R . . C24 C 0.2395(4) 0.3735(4) 0.1806(3) 0.0282(13) Uani 1 1 d . . . H24 H 0.2346 0.3449 0.1421 0.034 Uiso 1 1 calc R . . Cd1 Cd -0.05905(2) -0.05905(2) 0.0000 0.01846(16) Uani 1 2 d S . . Cl1 Cl 0.12464(14) 0.87536(14) 0.2500 0.0641(8) Uani 1 2 d SD . . Cl2 Cl 0.23112(12) 0.23112(12) 0.0000 0.0742(10) Uani 1 2 d S . . Cl3 Cl 0.4159(2) 0.9363(3) 0.15465(15) 0.1017(10) Uani 1 1 d D . . N1 N 0.3743(3) -0.3812(3) 0.1625(2) 0.0260(10) Uani 1 1 d . . . N2 N 0.0441(3) -0.0064(3) 0.0655(2) 0.0229(10) Uani 1 1 d . . . N3 N 0.0117(3) 0.0542(3) 0.1045(2) 0.0248(10) Uani 1 1 d . . . N4 N 0.1491(3) 0.0560(3) 0.1112(2) 0.0255(10) Uani 1 1 d . . . N5 N 0.2309(3) 0.0744(4) 0.1317(3) 0.0469(17) Uani 1 1 d . . . H5A H 0.2575 0.0290 0.1446 0.056 Uiso 1 1 d R . . H5B H 0.2599 0.0865 0.0978 0.056 Uiso 1 1 d R . . N6 N 0.3137(3) 0.4746(3) 0.2421(2) 0.0242(10) Uani 1 1 d . . . O3 O 0.2725(6) 0.2552(8) 0.0522(3) 0.120(4) Uani 1 1 d . . . O4 O 0.1704(5) 0.1704(5) 0.0000 0.118(5) Uani 1 2 d S . . O5 O 0.2941(12) 0.1583(14) -0.0223(19) 0.220(19) Uani 0.50 1 d P . . C25 C 0.4630(6) 0.9582(6) 0.0852(4) 0.106(4) Uani 0.50 1 d PD A 1 H25 H 0.4229 0.9788 0.0529 0.128 Uiso 0.50 1 calc PR A 1 Cl4 Cl 0.5273(3) 0.8787(3) 0.06015(17) 0.0514(10) Uani 0.50 1 d PD A 1 Cl5 Cl 0.5236(10) 1.0357(9) 0.1166(8) 0.215(6) Uani 0.50 1 d PDU A 1 C25' C 0.4630(6) 0.9582(6) 0.0852(4) 0.106(4) Uani 0.50 1 d PD A 2 H25' H 0.4454 0.9086 0.0597 0.128 Uiso 0.50 1 calc PR A 2 Cl4' Cl 0.5693(5) 0.9562(7) 0.0762(4) 0.139(3) Uani 0.50 1 d PDU A 2 Cl5' Cl 0.4199(4) 1.0397(4) 0.0447(3) 0.0855(18) Uani 0.50 1 d PD A 2 O2' O 0.0501(9) 0.9086(13) 0.2781(9) 0.115(6) Uani 0.50 1 d PDU B 3 O2 O 0.0960(16) 0.8813(14) 0.3093(6) 0.115(6) Uani 0.50 1 d PDU B 4 O1 O 0.1842(13) 0.8997(11) 0.2939(9) 0.111(7) Uani 0.50 1 d PD B . O1' O 0.2128(11) 0.8884(19) 0.2393(13) 0.172(13) Uani 0.50 1 d P B . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(3) 0.026(3) 0.027(3) -0.007(2) -0.003(2) 0.006(2) C2 0.030(3) 0.030(3) 0.016(3) -0.003(2) -0.001(2) 0.000(2) C3 0.032(3) 0.018(3) 0.026(3) -0.004(2) -0.006(2) 0.001(2) C4 0.019(3) 0.035(3) 0.027(3) -0.003(2) -0.001(2) 0.006(2) C5 0.023(3) 0.028(3) 0.026(3) 0.002(2) 0.001(2) 0.002(2) C6 0.022(3) 0.027(3) 0.021(3) -0.002(2) -0.004(2) -0.001(2) C7 0.019(3) 0.030(3) 0.027(3) 0.000(2) 0.001(2) 0.004(2) C8 0.034(3) 0.037(3) 0.023(3) 0.006(3) 0.005(3) 0.004(3) C9 0.030(3) 0.029(3) 0.029(3) 0.003(2) 0.001(2) 0.006(3) C10 0.022(3) 0.020(3) 0.024(3) -0.002(2) -0.005(2) -0.003(2) C11 0.023(3) 0.029(3) 0.019(3) 0.000(2) -0.001(2) -0.001(2) C12 0.026(3) 0.021(3) 0.021(2) 0.004(2) -0.004(2) -0.001(2) C13 0.021(3) 0.020(3) 0.021(2) 0.002(2) -0.001(2) 0.001(2) C14 0.025(3) 0.026(3) 0.020(2) 0.000(2) -0.005(2) 0.002(2) C15 0.029(3) 0.037(3) 0.037(3) -0.010(3) 0.005(3) -0.010(3) C16 0.027(3) 0.049(4) 0.041(4) -0.018(3) 0.010(3) -0.010(3) C17 0.030(3) 0.037(3) 0.037(3) -0.015(3) 0.005(3) 0.000(2) C18 0.021(3) 0.025(3) 0.022(3) -0.003(2) -0.002(2) 0.000(2) C19 0.026(3) 0.021(3) 0.028(3) 0.003(2) -0.002(2) 0.002(2) C20 0.022(3) 0.022(3) 0.030(3) -0.001(2) -0.004(2) 0.005(2) C21 0.020(3) 0.030(3) 0.028(3) -0.004(2) 0.006(2) 0.000(2) C22 0.036(3) 0.025(3) 0.025(3) -0.010(2) 0.001(2) -0.002(2) C23 0.027(3) 0.024(3) 0.028(3) -0.005(2) 0.004(2) 0.002(2) C24 0.030(3) 0.029(3) 0.026(3) -0.003(2) -0.001(2) -0.002(3) Cd1 0.01694(18) 0.01694(18) 0.0215(3) -0.00154(16) 0.00154(16) -0.0026(2) Cl1 0.0787(13) 0.0787(13) 0.0351(13) -0.0021(12) -0.0021(12) 0.0222(16) Cl2 0.0880(16) 0.0880(16) 0.0467(15) -0.0047(15) 0.0047(15) -0.0517(19) Cl3 0.091(2) 0.131(3) 0.083(2) 0.015(2) -0.0026(16) 0.025(2) N1 0.029(3) 0.020(2) 0.029(2) -0.003(2) -0.004(2) 0.0031(18) N2 0.023(2) 0.019(2) 0.027(2) -0.0030(18) -0.0012(19) -0.0017(17) N3 0.026(2) 0.022(2) 0.026(2) 0.001(2) -0.0010(18) -0.002(2) N4 0.019(2) 0.026(2) 0.032(2) -0.002(2) -0.0083(18) 0.001(2) N5 0.024(3) 0.050(4) 0.067(4) -0.038(3) -0.018(3) 0.008(3) N6 0.022(2) 0.023(2) 0.027(2) 0.000(2) -0.004(2) 0.0020(18) O3 0.083(6) 0.217(12) 0.061(5) -0.019(6) -0.003(4) -0.054(7) O4 0.117(7) 0.117(7) 0.120(10) 0.029(8) -0.029(8) -0.059(8) O5 0.078(12) 0.120(17) 0.46(5) -0.18(3) -0.07(2) 0.018(12) C25 0.109(11) 0.108(11) 0.102(10) -0.009(8) -0.008(8) 0.027(8) Cl4 0.063(2) 0.058(2) 0.0331(18) -0.0031(16) -0.0078(16) 0.0169(19) Cl5 0.207(8) 0.183(8) 0.255(8) -0.010(6) 0.040(6) 0.004(6) C25' 0.109(11) 0.108(11) 0.102(10) -0.009(8) -0.008(8) 0.027(8) Cl4' 0.116(5) 0.185(6) 0.117(5) 0.040(5) 0.016(4) -0.004(5) Cl5' 0.076(3) 0.111(5) 0.070(3) 0.045(3) 0.006(3) 0.017(3) O2' 0.102(8) 0.136(9) 0.108(8) -0.022(6) 0.020(6) 0.004(6) O2 0.130(9) 0.122(9) 0.093(8) 0.001(6) 0.015(6) 0.011(7) O1 0.152(18) 0.069(10) 0.112(14) 0.017(10) -0.078(14) -0.022(11) O1' 0.069(11) 0.28(3) 0.16(2) -0.16(2) 0.016(12) -0.063(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.348(8) . ? C1 C2 1.379(8) . ? C1 H1 0.9500 . ? C2 C3 1.394(9) . ? C2 H2 0.9500 . ? C3 C4 1.405(8) . ? C3 C6 1.479(8) . ? C4 C5 1.364(8) . ? C4 H4 0.9500 . ? C5 N1 1.341(7) . ? C5 H5 0.9500 . ? C6 C11 1.396(8) . ? C6 C7 1.403(8) . ? C7 C8 1.362(9) . ? C7 H7 0.9500 . ? C8 C9 1.389(9) . ? C8 H8 0.9500 . ? C9 C10 1.401(8) . ? C9 H9 0.9500 . ? C10 C11 1.379(8) . ? C10 C12 1.487(8) . ? C11 H11 0.9500 . ? C12 N2 1.323(7) . ? C12 N4 1.355(7) . ? C13 N3 1.316(7) . ? C13 N4 1.358(7) . ? C13 C14 1.479(7) . ? C14 C19 1.379(8) . ? C14 C15 1.394(9) . ? C15 C16 1.385(9) . ? C15 H15 0.9500 . ? C16 C17 1.382(9) . ? C16 H16 0.9500 . ? C17 C18 1.383(8) . ? C17 H17 0.9500 . ? C18 C19 1.390(8) . ? C18 C20 1.490(8) . ? C19 H19 0.9500 . ? C20 C21 1.391(8) . ? C20 C24 1.395(9) . ? C21 C22 1.376(8) . ? C21 H21 0.9500 . ? C22 N6 1.339(8) . ? C22 H22 0.9500 . ? C23 N6 1.335(7) . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cd1 N2 2.318(5) . ? Cd1 N2 2.318(5) 7 ? Cd1 N1 2.363(5) 3_444 ? Cd1 N1 2.363(5) 6_445 ? Cd1 N6 2.429(5) 6_455 ? Cd1 N6 2.429(5) 3_544 ? Cl1 O2 1.361(9) 8_665 ? Cl1 O2 1.361(9) . ? Cl1 O1 1.392(9) . ? Cl1 O1 1.392(9) 8_665 ? Cl1 O2' 1.429(9) 8_665 ? Cl1 O2' 1.429(9) . ? Cl1 O1' 1.433(18) . ? Cl1 O1' 1.433(18) 8_665 ? Cl2 O3 1.359(7) 7 ? Cl2 O3 1.359(7) . ? Cl2 O4 1.361(11) . ? Cl2 O5 1.601(19) 7 ? Cl2 O5 1.601(19) . ? Cl3 C25 1.710(6) . ? N1 Cd1 2.363(5) 4_545 ? N2 N3 1.377(7) . ? N4 N5 1.402(7) . ? N5 H5A 0.8793 . ? N5 H5B 0.8846 . ? N6 Cd1 2.429(5) 4 ? C25 Cl5 1.701(9) . ? C25 Cl4 1.710(8) . ? C25 H25 1.0000 . ? O2' O2' 1.53(4) 8_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.0(5) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 119.8(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 115.8(5) . . ? C2 C3 C6 123.1(6) . . ? C4 C3 C6 121.2(5) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 124.1(5) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? C11 C6 C7 117.8(5) . . ? C11 C6 C3 119.5(5) . . ? C7 C6 C3 122.7(5) . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 122.0(6) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C10 117.6(6) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? C11 C10 C9 120.8(5) . . ? C11 C10 C12 117.9(5) . . ? C9 C10 C12 121.2(5) . . ? C10 C11 C6 121.0(5) . . ? C10 C11 H11 119.5 . . ? C6 C11 H11 119.5 . . ? N2 C12 N4 108.5(5) . . ? N2 C12 C10 128.1(5) . . ? N4 C12 C10 123.2(5) . . ? N3 C13 N4 109.4(5) . . ? N3 C13 C14 123.6(5) . . ? N4 C13 C14 126.9(5) . . ? C19 C14 C15 120.5(5) . . ? C19 C14 C13 122.2(5) . . ? C15 C14 C13 117.3(5) . . ? C16 C15 C14 118.5(6) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C17 C16 C15 120.5(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 121.4(6) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C19 118.0(5) . . ? C17 C18 C20 121.5(5) . . ? C19 C18 C20 120.5(5) . . ? C14 C19 C18 121.1(5) . . ? C14 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C24 116.4(5) . . ? C21 C20 C18 121.7(5) . . ? C24 C20 C18 121.8(5) . . ? C22 C21 C20 120.0(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N6 C22 C21 123.4(5) . . ? N6 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N6 C23 C24 123.6(5) . . ? N6 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C20 119.8(5) . . ? C23 C24 H24 120.1 . . ? C20 C24 H24 120.1 . . ? N2 Cd1 N2 82.1(2) . 7 ? N2 Cd1 N1 158.72(16) . 3_444 ? N2 Cd1 N1 88.44(16) 7 3_444 ? N2 Cd1 N1 88.44(16) . 6_445 ? N2 Cd1 N1 158.72(16) 7 6_445 ? N1 Cd1 N1 106.3(2) 3_444 6_445 ? N2 Cd1 N6 110.18(16) . 6_455 ? N2 Cd1 N6 87.31(16) 7 6_455 ? N1 Cd1 N6 88.26(17) 3_444 6_455 ? N1 Cd1 N6 78.06(17) 6_445 6_455 ? N2 Cd1 N6 87.31(16) . 3_544 ? N2 Cd1 N6 110.18(16) 7 3_544 ? N1 Cd1 N6 78.06(17) 3_444 3_544 ? N1 Cd1 N6 88.26(17) 6_445 3_544 ? N6 Cd1 N6 157.2(2) 6_455 3_544 ? O2 Cl1 O2 147(2) 8_665 . ? O2 Cl1 O1 126.4(12) 8_665 . ? O2 Cl1 O1 64.4(13) . . ? O2 Cl1 O1 64.4(13) 8_665 8_665 ? O2 Cl1 O1 126.4(12) . 8_665 ? O1 Cl1 O1 147.0(19) . 8_665 ? O2 Cl1 O2' 45.6(10) 8_665 8_665 ? O2 Cl1 O2' 102.6(15) . 8_665 ? O1 Cl1 O2' 108.0(11) . 8_665 ? O1 Cl1 O2' 99.8(13) 8_665 8_665 ? O2 Cl1 O2' 102.6(15) 8_665 . ? O2 Cl1 O2' 45.6(10) . . ? O1 Cl1 O2' 99.8(13) . . ? O1 Cl1 O2' 108.0(11) 8_665 . ? O2' Cl1 O2' 64.5(18) 8_665 . ? O2 Cl1 O1' 82.4(16) 8_665 . ? O2 Cl1 O1' 117.9(14) . . ? O1 Cl1 O1' 53.7(13) . . ? O1 Cl1 O1' 105.0(10) 8_665 . ? O2' Cl1 O1' 99.9(17) 8_665 . ? O2' Cl1 O1' 145.4(12) . . ? O2 Cl1 O1' 117.9(14) 8_665 8_665 ? O2 Cl1 O1' 82.4(16) . 8_665 ? O1 Cl1 O1' 105.0(10) . 8_665 ? O1 Cl1 O1' 53.7(12) 8_665 8_665 ? O2' Cl1 O1' 145.4(12) 8_665 8_665 ? O2' Cl1 O1' 99.9(17) . 8_665 ? O1' Cl1 O1' 108(3) . 8_665 ? O3 Cl2 O3 114.6(8) 7 . ? O3 Cl2 O4 122.7(4) 7 . ? O3 Cl2 O4 122.7(4) . . ? O3 Cl2 O5 98.7(12) 7 7 ? O3 Cl2 O5 85.6(16) . 7 ? O4 Cl2 O5 86.1(8) . 7 ? O3 Cl2 O5 85.6(16) 7 . ? O3 Cl2 O5 98.7(12) . . ? O4 Cl2 O5 86.1(8) . . ? O5 Cl2 O5 172.1(16) 7 . ? C5 N1 C1 115.7(5) . . ? C5 N1 Cd1 115.7(4) . 4_545 ? C1 N1 Cd1 125.6(4) . 4_545 ? C12 N2 N3 108.2(4) . . ? C12 N2 Cd1 138.9(4) . . ? N3 N2 Cd1 111.2(3) . . ? C13 N3 N2 107.1(4) . . ? C12 N4 C13 106.7(4) . . ? C12 N4 N5 126.2(5) . . ? C13 N4 N5 126.9(5) . . ? N4 N5 H5A 112.0 . . ? N4 N5 H5B 105.5 . . ? H5A N5 H5B 101.0 . . ? C23 N6 C22 116.8(5) . . ? C23 N6 Cd1 116.5(4) . 4 ? C22 N6 Cd1 126.5(4) . 4 ? Cl5 C25 Cl3 92.6(7) . . ? Cl5 C25 Cl4 108.8(7) . . ? Cl3 C25 Cl4 112.8(5) . . ? Cl5 C25 H25 113.6 . . ? Cl3 C25 H25 113.6 . . ? Cl4 C25 H25 113.6 . . ? Cl1 O2' O2' 57.8(9) . 8_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.2(9) . . . . ? C1 C2 C3 C4 -5.2(8) . . . . ? C1 C2 C3 C6 173.9(5) . . . . ? C2 C3 C4 C5 7.0(8) . . . . ? C6 C3 C4 C5 -172.2(5) . . . . ? C3 C4 C5 N1 -2.5(10) . . . . ? C2 C3 C6 C11 -163.0(6) . . . . ? C4 C3 C6 C11 16.1(8) . . . . ? C2 C3 C6 C7 15.5(9) . . . . ? C4 C3 C6 C7 -165.4(5) . . . . ? C11 C6 C7 C8 -0.1(9) . . . . ? C3 C6 C7 C8 -178.7(6) . . . . ? C6 C7 C8 C9 1.1(10) . . . . ? C7 C8 C9 C10 -2.0(10) . . . . ? C8 C9 C10 C11 2.0(9) . . . . ? C8 C9 C10 C12 178.7(6) . . . . ? C9 C10 C11 C6 -1.1(8) . . . . ? C12 C10 C11 C6 -177.9(5) . . . . ? C7 C6 C11 C10 0.1(8) . . . . ? C3 C6 C11 C10 178.7(5) . . . . ? C11 C10 C12 N2 -94.2(7) . . . . ? C9 C10 C12 N2 89.0(7) . . . . ? C11 C10 C12 N4 80.2(7) . . . . ? C9 C10 C12 N4 -96.6(7) . . . . ? N3 C13 C14 C19 -146.0(6) . . . . ? N4 C13 C14 C19 31.3(8) . . . . ? N3 C13 C14 C15 31.8(8) . . . . ? N4 C13 C14 C15 -150.8(6) . . . . ? C19 C14 C15 C16 -0.7(9) . . . . ? C13 C14 C15 C16 -178.6(6) . . . . ? C14 C15 C16 C17 -0.3(11) . . . . ? C15 C16 C17 C18 0.3(11) . . . . ? C16 C17 C18 C19 0.6(10) . . . . ? C16 C17 C18 C20 -179.1(6) . . . . ? C15 C14 C19 C18 1.7(9) . . . . ? C13 C14 C19 C18 179.5(5) . . . . ? C17 C18 C19 C14 -1.6(9) . . . . ? C20 C18 C19 C14 178.1(5) . . . . ? C17 C18 C20 C21 23.3(9) . . . . ? C19 C18 C20 C21 -156.3(6) . . . . ? C17 C18 C20 C24 -159.1(6) . . . . ? C19 C18 C20 C24 21.2(9) . . . . ? C24 C20 C21 C22 -2.9(9) . . . . ? C18 C20 C21 C22 174.8(6) . . . . ? C20 C21 C22 N6 0.5(9) . . . . ? N6 C23 C24 C20 -1.2(10) . . . . ? C21 C20 C24 C23 3.2(9) . . . . ? C18 C20 C24 C23 -174.5(6) . . . . ? C4 C5 N1 C1 -3.9(9) . . . . ? C4 C5 N1 Cd1 157.8(5) . . . 4_545 ? C2 C1 N1 C5 5.8(9) . . . . ? C2 C1 N1 Cd1 -153.8(5) . . . 4_545 ? N4 C12 N2 N3 1.3(6) . . . . ? C10 C12 N2 N3 176.4(5) . . . . ? N4 C12 N2 Cd1 164.1(4) . . . . ? C10 C12 N2 Cd1 -20.8(9) . . . . ? N2 Cd1 N2 C12 -68.4(5) 7 . . . ? N1 Cd1 N2 C12 -3.9(9) 3_444 . . . ? N1 Cd1 N2 C12 130.7(6) 6_445 . . . ? N6 Cd1 N2 C12 -152.6(5) 6_455 . . . ? N6 Cd1 N2 C12 42.4(6) 3_544 . . . ? N2 Cd1 N2 N3 94.0(4) 7 . . . ? N1 Cd1 N2 N3 158.5(4) 3_444 . . . ? N1 Cd1 N2 N3 -66.9(3) 6_445 . . . ? N6 Cd1 N2 N3 9.8(4) 6_455 . . . ? N6 Cd1 N2 N3 -155.2(4) 3_544 . . . ? N4 C13 N3 N2 0.6(6) . . . . ? C14 C13 N3 N2 178.4(5) . . . . ? C12 N2 N3 C13 -1.2(6) . . . . ? Cd1 N2 N3 C13 -169.1(3) . . . . ? N2 C12 N4 C13 -0.9(6) . . . . ? C10 C12 N4 C13 -176.3(5) . . . . ? N2 C12 N4 N5 175.4(6) . . . . ? C10 C12 N4 N5 0.0(9) . . . . ? N3 C13 N4 C12 0.1(6) . . . . ? C14 C13 N4 C12 -177.5(5) . . . . ? N3 C13 N4 N5 -176.1(6) . . . . ? C14 C13 N4 N5 6.2(9) . . . . ? C24 C23 N6 C22 -1.3(9) . . . . ? C24 C23 N6 Cd1 173.0(5) . . . 4 ? C21 C22 N6 C23 1.6(9) . . . . ? C21 C22 N6 Cd1 -172.0(5) . . . 4 ? O2 Cl1 O2' O2' -25.6(19) 8_665 . . 8_665 ? O2 Cl1 O2' O2' 144(3) . . . 8_665 ? O1 Cl1 O2' O2' 105.4(15) . . . 8_665 ? O1 Cl1 O2' O2' -92.5(18) 8_665 . . 8_665 ? O1' Cl1 O2' O2' 69(3) . . . 8_665 ? O1' Cl1 O2' O2' -147.4(15) 8_665 . . 8_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.238 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.129