# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'A. Amoroso' _publ_contact_author_email AMOROSOAJ@CF.AC.UK _publ_section_title ; The Synthesis and Co-ordination Chemistry of a Novel Tris-8-aminoquinoline Tripod ; loop_ _publ_author_name 'A. Amoroso' 'A.-R. H. Al-Sudani' 'Peter G. Edwards' 'Sian Howard' 'James C. Knight' ; K.M.A.Malik ; 'Li-ling Ooi.' 'Lisa Stratford' # Attachment '01Lisa1.CIF' data_01Lisa1_s92 _database_code_depnum_ccdc_archive 'CCDC 736252' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 N7' _chemical_formula_sum 'C33 H33 N7' _chemical_formula_weight 527.66 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.5530(5) _cell_length_b 8.6310(2) _cell_length_c 16.1819(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.7806(8) _cell_angle_gamma 90.00 _cell_volume 2729.57(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17167 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9768 _exptl_absorpt_correction_T_max 0.9961 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26218 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5358 _reflns_number_gt 3897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0533P)^2^+0.4861P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0144(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5358 _refine_ls_number_parameters 374 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _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 N1 N 0.21089(7) 0.13727(15) 0.02671(7) 0.0262(3) Uani 1 1 d . . . N2 N 0.32211(7) 0.47467(16) -0.01928(8) 0.0319(3) Uani 1 1 d D . . H2 H 0.3430(9) 0.4252(19) -0.0643(8) 0.045(5) Uiso 1 1 d D . . N3 N 0.21103(7) 0.18711(17) 0.20973(8) 0.0334(3) Uani 1 1 d D . . H3 H 0.1760(7) 0.2552(18) 0.1909(11) 0.050(6) Uiso 1 1 d D . . N4 N 0.06903(7) 0.17868(17) 0.02313(8) 0.0321(3) Uani 1 1 d D . . H4 H 0.1004(8) 0.212(2) 0.0653(9) 0.048(5) Uiso 1 1 d D . . N5 N 0.43535(7) 0.57269(17) -0.09579(8) 0.0343(4) Uani 1 1 d . . . N6 N 0.19561(7) 0.49010(17) 0.24810(8) 0.0342(4) Uani 1 1 d . . . N7 N 0.04204(7) 0.33690(16) 0.15995(8) 0.0304(3) Uani 1 1 d . . . C1 C 0.25211(8) 0.24128(19) -0.02249(9) 0.0289(4) Uani 1 1 d . . . H1A H 0.2242 0.2796 -0.0704 0.035 Uiso 1 1 calc R . . H1B H 0.2916 0.1837 -0.0439 0.035 Uiso 1 1 calc R . . C2 C 0.27768(8) 0.37741(19) 0.02854(9) 0.0280(4) Uani 1 1 d . . . H2A H 0.2383 0.4391 0.0469 0.034 Uiso 1 1 calc R . . H2B H 0.3031 0.3391 0.0783 0.034 Uiso 1 1 calc R . . C3 C 0.25210(9) 0.04639(19) 0.08627(10) 0.0306(4) Uani 1 1 d . . . H3A H 0.2978 0.0944 0.0940 0.037 Uiso 1 1 calc R . . H3B H 0.2584 -0.0598 0.0646 0.037 Uiso 1 1 calc R . . C4 C 0.21729(10) 0.0387(2) 0.16897(10) 0.0364(4) Uani 1 1 d . . . H4A H 0.1710 -0.0059 0.1601 0.044 Uiso 1 1 calc R . . H4B H 0.2436 -0.0322 0.2060 0.044 Uiso 1 1 calc R . . C5 C 0.16546(8) 0.03785(19) -0.02392(10) 0.0305(4) Uani 1 1 d . . . H5A H 0.1544 -0.0562 0.0080 0.037 Uiso 1 1 calc R . . H5B H 0.1897 0.0047 -0.0737 0.037 Uiso 1 1 calc R . . C6 C 0.09955(8) 0.1188(2) -0.05039(9) 0.0306(4) Uani 1 1 d . . . H6A H 0.1092 0.2044 -0.0890 0.037 Uiso 1 1 calc R . . H6B H 0.0680 0.0448 -0.0787 0.037 Uiso 1 1 calc R . . C7 C 0.36264(8) 0.58389(18) 0.02024(10) 0.0277(4) Uani 1 1 d . . . C8 C 0.34921(9) 0.64346(19) 0.09717(10) 0.0320(4) Uani 1 1 d . . . H8 H 0.3105 0.6073 0.1256 0.038 Uiso 1 1 calc R . . C9 C 0.39165(9) 0.7564(2) 0.13418(11) 0.0358(4) Uani 1 1 d . . . H9 H 0.3811 0.7957 0.1871 0.043 Uiso 1 1 calc R . . C10 C 0.44798(9) 0.8111(2) 0.09550(11) 0.0363(4) Uani 1 1 d . . . H10 H 0.4757 0.8889 0.1211 0.044 Uiso 1 1 calc R . . C11 C 0.46478(8) 0.75140(19) 0.01730(10) 0.0317(4) Uani 1 1 d . . . C12 C 0.42223(8) 0.63785(19) -0.02096(9) 0.0283(4) Uani 1 1 d . . . C13 C 0.52335(9) 0.7962(2) -0.02585(11) 0.0380(4) Uani 1 1 d . . . H13 H 0.5538 0.8717 -0.0028 0.046 Uiso 1 1 calc R . . C14 C 0.53608(9) 0.7312(2) -0.10035(11) 0.0410(5) Uani 1 1 d . . . H14 H 0.5751 0.7615 -0.1299 0.049 Uiso 1 1 calc R . . C15 C 0.49103(9) 0.6190(2) -0.13304(11) 0.0400(5) Uani 1 1 d . . . H15 H 0.5010 0.5737 -0.1848 0.048 Uiso 1 1 calc R . . C16 C 0.26613(8) 0.2635(2) 0.24559(9) 0.0301(4) Uani 1 1 d . . . C17 C 0.32868(9) 0.1942(2) 0.26501(10) 0.0355(4) Uani 1 1 d . . . H17 H 0.3355 0.0882 0.2519 0.043 Uiso 1 1 calc R . . C18 C 0.38211(9) 0.2790(2) 0.30389(10) 0.0389(5) Uani 1 1 d . . . H18 H 0.4244 0.2288 0.3163 0.047 Uiso 1 1 calc R . . C19 C 0.37479(9) 0.4313(2) 0.32417(10) 0.0374(4) Uani 1 1 d . . . H19 H 0.4119 0.4865 0.3495 0.045 Uiso 1 1 calc R . . C20 C 0.31175(9) 0.5065(2) 0.30730(9) 0.0316(4) Uani 1 1 d . . . C21 C 0.25753(8) 0.4238(2) 0.26709(9) 0.0291(4) Uani 1 1 d . . . C22 C 0.29842(9) 0.6607(2) 0.33033(10) 0.0362(4) Uani 1 1 d . . . H22 H 0.3331 0.7203 0.3578 0.043 Uiso 1 1 calc R . . C23 C 0.23567(9) 0.7243(2) 0.31314(10) 0.0378(4) Uani 1 1 d . . . H23 H 0.2257 0.8273 0.3298 0.045 Uiso 1 1 calc R . . C24 C 0.18620(10) 0.6351(2) 0.27055(10) 0.0370(4) Uani 1 1 d . . . H24 H 0.1433 0.6819 0.2570 0.044 Uiso 1 1 calc R . . C25 C 0.00884(8) 0.25946(18) 0.02282(9) 0.0264(4) Uani 1 1 d . . . C26 C -0.03782(8) 0.2671(2) -0.04320(10) 0.0322(4) Uani 1 1 d . . . H26 H -0.0278 0.2176 -0.0939 0.039 Uiso 1 1 calc R . . C27 C -0.09989(9) 0.3476(2) -0.03581(11) 0.0378(4) Uani 1 1 d . . . H27 H -0.1309 0.3524 -0.0821 0.045 Uiso 1 1 calc R . . C28 C -0.11678(9) 0.4190(2) 0.03576(11) 0.0383(4) Uani 1 1 d . . . H28 H -0.1597 0.4695 0.0397 0.046 Uiso 1 1 calc R . . C29 C -0.06996(8) 0.41765(19) 0.10443(10) 0.0300(4) Uani 1 1 d . . . C30 C -0.00688(8) 0.33928(18) 0.09763(9) 0.0268(4) Uani 1 1 d . . . C31 C -0.08170(9) 0.4932(2) 0.17991(11) 0.0365(4) Uani 1 1 d . . . H31 H -0.1235 0.5467 0.1875 0.044 Uiso 1 1 calc R . . C32 C -0.03307(9) 0.4892(2) 0.24196(11) 0.0366(4) Uani 1 1 d . . . H32 H -0.0406 0.5389 0.2933 0.044 Uiso 1 1 calc R . . C33 C 0.02833(9) 0.4106(2) 0.22883(10) 0.0347(4) Uani 1 1 d . . . H33 H 0.0622 0.4105 0.2722 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0251(7) 0.0281(7) 0.0259(7) 0.0004(6) 0.0052(5) -0.0020(6) N2 0.0315(8) 0.0363(8) 0.0282(7) 0.0015(6) 0.0051(6) -0.0078(7) N3 0.0319(9) 0.0402(9) 0.0284(7) -0.0007(6) 0.0044(6) -0.0023(7) N4 0.0279(8) 0.0428(9) 0.0253(7) -0.0064(6) -0.0006(6) 0.0028(7) N5 0.0307(8) 0.0394(9) 0.0330(7) 0.0055(6) 0.0048(6) -0.0006(7) N6 0.0310(8) 0.0437(9) 0.0278(7) 0.0058(6) 0.0001(6) 0.0011(7) N7 0.0312(8) 0.0344(8) 0.0259(7) 0.0003(6) 0.0020(6) -0.0002(6) C1 0.0280(9) 0.0332(9) 0.0260(8) 0.0015(7) 0.0064(7) -0.0005(7) C2 0.0253(9) 0.0333(9) 0.0257(8) 0.0030(7) 0.0029(6) -0.0024(7) C3 0.0304(9) 0.0283(9) 0.0333(9) 0.0026(7) 0.0029(7) 0.0040(7) C4 0.0417(11) 0.0338(10) 0.0337(9) 0.0060(8) 0.0027(8) -0.0060(8) C5 0.0332(10) 0.0298(9) 0.0291(8) -0.0060(7) 0.0084(7) -0.0050(7) C6 0.0322(10) 0.0347(9) 0.0251(8) -0.0049(7) 0.0042(7) -0.0053(8) C7 0.0263(9) 0.0273(8) 0.0294(8) 0.0049(7) -0.0009(7) -0.0006(7) C8 0.0264(9) 0.0357(10) 0.0338(9) 0.0039(8) 0.0029(7) -0.0024(8) C9 0.0352(10) 0.0386(10) 0.0335(9) -0.0006(8) 0.0015(8) -0.0007(8) C10 0.0309(10) 0.0375(10) 0.0402(10) 0.0020(8) -0.0041(8) -0.0053(8) C11 0.0246(9) 0.0337(9) 0.0367(9) 0.0098(7) -0.0027(7) 0.0011(7) C12 0.0257(9) 0.0305(9) 0.0286(8) 0.0079(7) -0.0011(7) 0.0023(7) C13 0.0266(10) 0.0438(11) 0.0436(10) 0.0095(9) 0.0001(8) -0.0067(8) C14 0.0281(10) 0.0498(12) 0.0454(11) 0.0130(9) 0.0070(8) -0.0042(9) C15 0.0357(11) 0.0487(11) 0.0360(9) 0.0069(8) 0.0084(8) 0.0025(9) C16 0.0299(10) 0.0408(10) 0.0196(7) 0.0048(7) 0.0035(7) -0.0038(8) C17 0.0371(10) 0.0426(11) 0.0272(8) 0.0039(8) 0.0053(7) 0.0038(8) C18 0.0272(10) 0.0596(13) 0.0300(9) 0.0069(9) 0.0020(7) 0.0050(9) C19 0.0278(10) 0.0538(12) 0.0304(9) 0.0042(8) 0.0001(7) -0.0042(8) C20 0.0304(10) 0.0439(11) 0.0206(7) 0.0075(7) 0.0027(7) -0.0053(8) C21 0.0281(9) 0.0406(10) 0.0188(7) 0.0060(7) 0.0038(7) -0.0010(8) C22 0.0418(11) 0.0410(10) 0.0258(8) 0.0047(8) 0.0013(7) -0.0102(9) C23 0.0482(12) 0.0358(10) 0.0296(9) 0.0066(8) 0.0042(8) -0.0009(9) C24 0.0389(11) 0.0412(11) 0.0310(9) 0.0072(8) 0.0006(8) 0.0041(8) C25 0.0228(9) 0.0286(9) 0.0279(8) 0.0020(7) 0.0025(7) -0.0046(7) C26 0.0305(10) 0.0375(10) 0.0286(8) 0.0000(7) -0.0005(7) -0.0068(8) C27 0.0294(10) 0.0470(11) 0.0366(9) 0.0085(8) -0.0062(7) -0.0060(8) C28 0.0276(10) 0.0432(11) 0.0441(10) 0.0077(8) 0.0012(8) 0.0041(8) C29 0.0278(9) 0.0280(9) 0.0345(9) 0.0051(7) 0.0044(7) -0.0018(7) C30 0.0265(9) 0.0270(8) 0.0271(8) 0.0039(7) 0.0031(7) -0.0049(7) C31 0.0355(10) 0.0332(10) 0.0415(10) 0.0037(8) 0.0128(8) 0.0040(8) C32 0.0424(11) 0.0334(10) 0.0347(9) -0.0029(8) 0.0110(8) 0.0010(8) C33 0.0368(10) 0.0409(10) 0.0265(8) -0.0027(8) 0.0024(7) -0.0024(8) _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 N1 C1 1.459(2) . ? N1 C3 1.465(2) . ? N1 C5 1.467(2) . ? N2 C7 1.376(2) . ? N2 C2 1.449(2) . ? N2 H2 0.948(15) . ? N3 C16 1.376(2) . ? N3 C4 1.447(2) . ? N3 H3 0.945(15) . ? N4 C25 1.368(2) . ? N4 C6 1.443(2) . ? N4 H4 0.947(15) . ? N5 C15 1.322(2) . ? N5 C12 1.367(2) . ? N6 C24 1.318(2) . ? N6 C21 1.366(2) . ? N7 C33 1.318(2) . ? N7 C30 1.368(2) . ? C1 C2 1.512(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.380(2) . ? C7 C12 1.438(2) . ? C8 C9 1.402(2) . ? C8 H8 0.9500 . ? C9 C10 1.368(2) . ? C9 H9 0.9500 . ? C10 C11 1.414(2) . ? C10 H10 0.9500 . ? C11 C13 1.414(2) . ? C11 C12 1.416(2) . ? C13 C14 1.360(3) . ? C13 H13 0.9500 . ? C14 C15 1.402(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(2) . ? C16 C21 1.438(2) . ? C17 C18 1.408(2) . ? C17 H17 0.9500 . ? C18 C19 1.363(3) . ? C18 H18 0.9500 . ? C19 C20 1.412(2) . ? C19 H19 0.9500 . ? C20 C22 1.409(2) . ? C20 C21 1.419(2) . ? C22 C23 1.365(2) . ? C22 H22 0.9500 . ? C23 C24 1.401(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.385(2) . ? C25 C30 1.434(2) . ? C26 C27 1.407(2) . ? C26 H26 0.9500 . ? C27 C28 1.362(3) . ? C27 H27 0.9500 . ? C28 C29 1.418(2) . ? C28 H28 0.9500 . ? C29 C31 1.410(2) . ? C29 C30 1.414(2) . ? C31 C32 1.362(3) . ? C31 H31 0.9500 . ? C32 C33 1.401(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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 C1 N1 C3 112.75(13) . . ? C1 N1 C5 112.98(12) . . ? C3 N1 C5 111.44(12) . . ? C7 N2 C2 119.66(13) . . ? C7 N2 H2 114.2(11) . . ? C2 N2 H2 115.4(11) . . ? C16 N3 C4 122.67(15) . . ? C16 N3 H3 112.8(12) . . ? C4 N3 H3 118.2(12) . . ? C25 N4 C6 123.87(13) . . ? C25 N4 H4 112.8(12) . . ? C6 N4 H4 115.2(12) . . ? C15 N5 C12 117.34(15) . . ? C24 N6 C21 117.81(15) . . ? C33 N7 C30 117.38(14) . . ? N1 C1 C2 111.04(12) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 110.62(12) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C4 110.49(13) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 114.13(14) . . ? N3 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? N3 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C6 112.52(13) . . ? N1 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C6 C5 107.57(13) . . ? N4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? N4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? N2 C7 C8 123.48(15) . . ? N2 C7 C12 118.01(14) . . ? C8 C7 C12 118.51(15) . . ? C7 C8 C9 121.18(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 121.25(16) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.76(16) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C13 C11 C10 123.80(16) . . ? C13 C11 C12 116.59(16) . . ? C10 C11 C12 119.59(15) . . ? N5 C12 C11 123.27(15) . . ? N5 C12 C7 117.04(14) . . ? C11 C12 C7 119.68(14) . . ? C14 C13 C11 119.88(17) . . ? C14 C13 H13 120.1 . . ? C11 C13 H13 120.1 . . ? C13 C14 C15 119.33(16) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N5 C15 C14 123.59(17) . . ? N5 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? N3 C16 C17 124.20(16) . . ? N3 C16 C21 117.83(15) . . ? C17 C16 C21 117.93(15) . . ? C16 C17 C18 120.89(17) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 121.80(17) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 119.60(17) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C22 C20 C19 123.41(16) . . ? C22 C20 C21 117.06(16) . . ? C19 C20 C21 119.51(16) . . ? N6 C21 C20 122.45(16) . . ? N6 C21 C16 117.30(15) . . ? C20 C21 C16 120.25(15) . . ? C23 C22 C20 119.92(17) . . ? C23 C22 H22 120.0 . . ? C20 C22 H22 120.0 . . ? C22 C23 C24 118.78(17) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N6 C24 C23 123.90(17) . . ? N6 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? N4 C25 C26 124.97(15) . . ? N4 C25 C30 116.66(13) . . ? C26 C25 C30 118.36(15) . . ? C25 C26 C27 120.48(16) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 121.91(16) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 119.68(16) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C31 C29 C30 117.04(15) . . ? C31 C29 C28 123.83(16) . . ? C30 C29 C28 119.12(15) . . ? N7 C30 C29 122.77(15) . . ? N7 C30 C25 116.84(14) . . ? C29 C30 C25 120.38(14) . . ? C32 C31 C29 119.91(16) . . ? C32 C31 H31 120.0 . . ? C29 C31 H31 120.0 . . ? C31 C32 C33 118.83(16) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? N7 C33 C32 124.05(16) . . ? N7 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.187 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.042 # Attachment '02LISA2_new.cif' data_s92 _database_code_depnum_ccdc_archive 'CCDC 736253' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 Cl2 N7 O8 Zn, 2(Cl O4), 0.38(H2 O)' _chemical_formula_sum 'C33 H33.37 Cl2 N7 O8.19 Zn' _chemical_formula_weight 795.27 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0950(2) _cell_length_b 17.5230(4) _cell_length_c 18.0930(5) _cell_angle_alpha 72.839(1) _cell_angle_beta 80.933(1) _cell_angle_gamma 84.137(2) _cell_volume 3313.22(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6837 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 25.0 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1639 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8450 _exptl_absorpt_correction_T_max 0.9094 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49656 _diffrn_reflns_av_R_equivalents 0.1425 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11630 _reflns_number_gt 6837 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The weak diffraction by the crystal combined with a large assymetric unit resulted in a low data/parameter ratio. The hydrogen on partially occupied water solvate was ignored; other hydrogen atoms were included in calculated positions using a riding model. ; _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^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11630 _refine_ls_number_parameters 1001 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2090 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8803(7) 0.3741(6) 0.4078(5) 0.063(2) Uani 1 1 d . . . H1 H 0.8140 0.3494 0.3987 0.075 Uiso 1 1 calc R . . C2 C 0.9411(7) 0.3342(5) 0.4715(5) 0.065(2) Uani 1 1 d . . . H2 H 0.9135 0.2850 0.5060 0.078 Uiso 1 1 calc R . . C3 C 1.0396(8) 0.3660(7) 0.4838(5) 0.081(3) Uani 1 1 d . . . H3 H 1.0836 0.3384 0.5259 0.097 Uiso 1 1 calc R . . C4 C 1.0761(7) 0.4396(7) 0.4344(5) 0.072(3) Uani 1 1 d . . . C5 C 1.1814(8) 0.4784(9) 0.4400(7) 0.099(4) Uani 1 1 d . . . H5 H 1.2334 0.4515 0.4779 0.118 Uiso 1 1 calc R . . C6 C 1.2082(9) 0.5514(10) 0.3930(8) 0.116(5) Uani 1 1 d . . . H6 H 1.2780 0.5750 0.3991 0.139 Uiso 1 1 calc R . . C7 C 1.1358(7) 0.5940(8) 0.3352(7) 0.100(4) Uani 1 1 d . . . H7 H 1.1549 0.6465 0.3044 0.120 Uiso 1 1 calc R . . C8 C 1.0345(7) 0.5585(6) 0.3231(6) 0.073(3) Uani 1 1 d . . . C9 C 1.0058(6) 0.4800(6) 0.3728(5) 0.062(2) Uani 1 1 d . . . C10 C 0.8771(7) 0.6610(5) 0.2866(7) 0.091(3) Uani 1 1 d . . . H10A H 0.8534 0.7009 0.2389 0.109 Uiso 1 1 calc R . . H10B H 0.9199 0.6887 0.3144 0.109 Uiso 1 1 calc R . . C11 C 0.7634(7) 0.6260(5) 0.3386(6) 0.075(3) Uani 1 1 d . . . H11A H 0.7867 0.5868 0.3868 0.090 Uiso 1 1 calc R . . H11B H 0.7096 0.6692 0.3537 0.090 Uiso 1 1 calc R . . C12 C 0.6045(6) 0.5332(5) 0.3518(5) 0.059(2) Uani 1 1 d . . . H12A H 0.5366 0.5668 0.3709 0.071 Uiso 1 1 calc R . . H12B H 0.6429 0.4997 0.3973 0.071 Uiso 1 1 calc R . . C13 C 0.5535(6) 0.4794(4) 0.3138(4) 0.0466(17) Uani 1 1 d . . . H13A H 0.4929 0.4452 0.3518 0.056 Uiso 1 1 calc R . . H13B H 0.5124 0.5122 0.2691 0.056 Uiso 1 1 calc R . . C14 C 0.6420(5) 0.3913(3) 0.2283(3) 0.0333(14) Uani 1 1 d . . . C15 C 0.5719(5) 0.4232(4) 0.1687(4) 0.0413(16) Uani 1 1 d . . . H15 H 0.5194 0.4697 0.1683 0.050 Uiso 1 1 calc R . . C16 C 0.5782(6) 0.3868(4) 0.1087(4) 0.0445(17) Uani 1 1 d . . . H16 H 0.5335 0.4113 0.0662 0.053 Uiso 1 1 calc R . . C17 C 0.6465(6) 0.3174(4) 0.1093(4) 0.0431(16) Uani 1 1 d . . . H17 H 0.6496 0.2945 0.0675 0.052 Uiso 1 1 calc R . . C18 C 0.7115(5) 0.2803(4) 0.1714(4) 0.0371(15) Uani 1 1 d . . . C19 C 0.7811(6) 0.2072(4) 0.1784(4) 0.0465(17) Uani 1 1 d . . . H19 H 0.7860 0.1808 0.1390 0.056 Uiso 1 1 calc R . . C20 C 0.8411(6) 0.1743(4) 0.2414(4) 0.0470(17) Uani 1 1 d . . . H20 H 0.8871 0.1246 0.2469 0.056 Uiso 1 1 calc R . . C21 C 0.8338(5) 0.2156(4) 0.2988(4) 0.0394(15) Uani 1 1 d . . . H21 H 0.8761 0.1918 0.3425 0.047 Uiso 1 1 calc R . . C22 C 0.7106(5) 0.3167(3) 0.2320(3) 0.0315(14) Uani 1 1 d . . . C23 C 0.6406(7) 0.6465(4) 0.2328(5) 0.068(2) Uani 1 1 d . . . H23A H 0.6782 0.6981 0.2223 0.081 Uiso 1 1 calc R . . H23B H 0.5522 0.6546 0.2502 0.081 Uiso 1 1 calc R . . C24 C 0.6566(6) 0.6217(4) 0.1565(5) 0.058(2) Uani 1 1 d . . . H24A H 0.6011 0.5790 0.1621 0.070 Uiso 1 1 calc R . . H24B H 0.6354 0.6682 0.1129 0.070 Uiso 1 1 calc R . . C25 C 0.8045(6) 0.5466(4) 0.0838(4) 0.0434(17) Uani 1 1 d . . . C26 C 0.7565(6) 0.5685(4) 0.0153(5) 0.056(2) Uani 1 1 d . . . H26 H 0.7071 0.6169 0.0023 0.067 Uiso 1 1 calc R . . C27 C 0.7784(6) 0.5215(5) -0.0364(4) 0.053(2) Uani 1 1 d . . . H27 H 0.7425 0.5378 -0.0834 0.064 Uiso 1 1 calc R . . C28 C 0.8497(6) 0.4533(4) -0.0203(4) 0.0474(18) Uani 1 1 d . . . H28 H 0.8650 0.4223 -0.0562 0.057 Uiso 1 1 calc R . . C29 C 0.9024(5) 0.4274(4) 0.0511(4) 0.0379(15) Uani 1 1 d . . . C30 C 0.9758(5) 0.3567(4) 0.0720(4) 0.0386(15) Uani 1 1 d . . . H30 H 0.9938 0.3237 0.0380 0.046 Uiso 1 1 calc R . . C31 C 1.0217(5) 0.3351(4) 0.1418(4) 0.0359(14) Uani 1 1 d . . . H31 H 1.0740 0.2883 0.1561 0.043 Uiso 1 1 calc R . . C32 C 0.9893(5) 0.3842(4) 0.1917(3) 0.0359(14) Uani 1 1 d . . . H32 H 1.0196 0.3685 0.2406 0.043 Uiso 1 1 calc R . . C33 C 0.8771(5) 0.4746(3) 0.1040(4) 0.0341(14) Uani 1 1 d . . . C34 C 0.4681(6) 0.1338(4) 0.0905(4) 0.0468(17) Uani 1 1 d . . . H34 H 0.3856 0.1508 0.1041 0.056 Uiso 1 1 calc R . . C35 C 0.5342(6) 0.1802(4) 0.0217(4) 0.0480(17) Uani 1 1 d . . . H35 H 0.4954 0.2252 -0.0116 0.058 Uiso 1 1 calc R . . C36 C 0.6537(6) 0.1598(5) 0.0038(4) 0.0516(18) Uani 1 1 d . . . H36 H 0.7002 0.1915 -0.0415 0.062 Uiso 1 1 calc R . . C37 C 0.7078(6) 0.0934(4) 0.0511(4) 0.0448(17) Uani 1 1 d . . . C38 C 0.8329(7) 0.0700(6) 0.0383(5) 0.063(2) Uani 1 1 d . . . H38 H 0.8840 0.1016 -0.0045 0.076 Uiso 1 1 calc R . . C39 C 0.8801(7) 0.0043(6) 0.0853(5) 0.065(2) Uani 1 1 d . . . H39 H 0.9650 -0.0094 0.0756 0.078 Uiso 1 1 calc R . . C40 C 0.8093(7) -0.0453(6) 0.1483(5) 0.069(2) Uani 1 1 d . . . H40 H 0.8452 -0.0926 0.1803 0.083 Uiso 1 1 calc R . . C41 C 0.6854(6) -0.0244(5) 0.1637(4) 0.0547(19) Uani 1 1 d . . . C42 C 0.6345(6) 0.0456(4) 0.1169(4) 0.0430(16) Uani 1 1 d . . . C43 C 0.5675(8) -0.1442(5) 0.2086(5) 0.074(2) Uani 1 1 d . . . H43A H 0.5505 -0.1881 0.2572 0.088 Uiso 1 1 calc R . . H43B H 0.6357 -0.1632 0.1749 0.088 Uiso 1 1 calc R . . C44 C 0.4538(8) -0.1243(5) 0.1667(5) 0.070(2) Uani 1 1 d . . . H44A H 0.4723 -0.0835 0.1159 0.084 Uiso 1 1 calc R . . H44B H 0.4309 -0.1730 0.1563 0.084 Uiso 1 1 calc R . . C45 C 0.2534(8) -0.0497(5) 0.1684(5) 0.064(2) Uani 1 1 d . . . H45A H 0.2085 -0.0884 0.1543 0.077 Uiso 1 1 calc R . . H45B H 0.2918 -0.0132 0.1194 0.077 Uiso 1 1 calc R . . C46 C 0.1635(6) -0.0016(4) 0.2120(4) 0.0518(18) Uani 1 1 d . . . H46A H 0.1002 0.0268 0.1792 0.062 Uiso 1 1 calc R . . H46B H 0.1227 -0.0376 0.2605 0.062 Uiso 1 1 calc R . . C47 C 0.1781(5) 0.0936(3) 0.2898(4) 0.0358(14) Uani 1 1 d . . . C48 C 0.0998(5) 0.0584(4) 0.3556(4) 0.0418(16) Uani 1 1 d . . . H48 H 0.0673 0.0088 0.3603 0.050 Uiso 1 1 calc R . . C49 C 0.0679(5) 0.0947(4) 0.4154(4) 0.0409(15) Uani 1 1 d . . . H49 H 0.0188 0.0673 0.4617 0.049 Uiso 1 1 calc R . . C50 C 0.1047(5) 0.1682(4) 0.4096(4) 0.0418(16) Uani 1 1 d . . . H50 H 0.0816 0.1915 0.4514 0.050 Uiso 1 1 calc R . . C51 C 0.1783(5) 0.2099(3) 0.3404(4) 0.0358(14) Uani 1 1 d . . . C52 C 0.2182(6) 0.2874(4) 0.3277(4) 0.0447(16) Uani 1 1 d . . . H52 H 0.1973 0.3146 0.3667 0.054 Uiso 1 1 calc R . . C53 C 0.2871(6) 0.3228(4) 0.2589(4) 0.0487(18) Uani 1 1 d . . . H53 H 0.3143 0.3749 0.2491 0.058 Uiso 1 1 calc R . . C54 C 0.3166(5) 0.2812(4) 0.2037(4) 0.0435(16) Uani 1 1 d . . . H54 H 0.3640 0.3071 0.1560 0.052 Uiso 1 1 calc R . . C55 C 0.2138(5) 0.1729(3) 0.2807(4) 0.0348(14) Uani 1 1 d . . . C56 C 0.3004(7) -0.1582(4) 0.2831(4) 0.059(2) Uani 1 1 d . . . H56A H 0.3595 -0.2053 0.2897 0.070 Uiso 1 1 calc R . . H56B H 0.2234 -0.1743 0.2724 0.070 Uiso 1 1 calc R . . C57 C 0.2750(7) -0.1353(4) 0.3598(4) 0.0518(18) Uani 1 1 d . . . H57A H 0.2000 -0.0995 0.3601 0.062 Uiso 1 1 calc R . . H57B H 0.2624 -0.1839 0.4044 0.062 Uiso 1 1 calc R . . C58 C 0.3575(5) -0.0495(3) 0.4249(3) 0.0351(14) Uani 1 1 d . . . C59 C 0.2969(6) -0.0779(4) 0.4975(4) 0.0413(15) Uani 1 1 d . . . H59 H 0.2668 -0.1299 0.5130 0.050 Uiso 1 1 calc R . . C60 C 0.2779(5) -0.0312(4) 0.5505(4) 0.0377(15) Uani 1 1 d . . . H60 H 0.2321 -0.0511 0.6005 0.045 Uiso 1 1 calc R . . C61 C 0.3248(5) 0.0423(4) 0.5303(3) 0.0388(15) Uani 1 1 d . . . H61 H 0.3141 0.0726 0.5668 0.047 Uiso 1 1 calc R . . C62 C 0.3891(5) 0.0733(3) 0.4551(3) 0.0332(14) Uani 1 1 d . . . C63 C 0.4389(5) 0.1490(3) 0.4297(3) 0.0346(14) Uani 1 1 d . . . H63 H 0.4307 0.1816 0.4641 0.041 Uiso 1 1 calc R . . C64 C 0.4986(5) 0.1753(4) 0.3560(4) 0.0397(15) Uani 1 1 d . . . H64 H 0.5357 0.2251 0.3395 0.048 Uiso 1 1 calc R . . C65 C 0.5049(5) 0.1288(4) 0.3048(4) 0.0356(14) Uani 1 1 d . . . H65 H 0.5435 0.1492 0.2528 0.043 Uiso 1 1 calc R . . C66 C 0.4039(5) 0.0272(3) 0.4012(3) 0.0318(13) Uani 1 1 d . . . N1 N 0.9101(5) 0.4448(4) 0.3592(4) 0.0558(16) Uani 1 1 d . . . N2 N 0.9611(6) 0.5972(4) 0.2644(5) 0.071(2) Uani 1 1 d . . . H2n H 1.0097 0.6185 0.2173 0.085 Uiso 1 1 calc R . . N3 N 0.6967(5) 0.5860(4) 0.2968(4) 0.0615(17) Uani 1 1 d . . . N4 N 0.6571(4) 0.4288(3) 0.2863(3) 0.0384(12) Uani 1 1 d . . . H4 H 0.6727 0.3873 0.3302 0.046 Uiso 1 1 calc R . . N5 N 0.7729(4) 0.2839(3) 0.2956(3) 0.0369(12) Uani 1 1 d . . . N6 N 0.7856(5) 0.5925(3) 0.1394(4) 0.0533(16) Uani 1 1 d . . . H6n H 0.8350 0.6358 0.1214 0.064 Uiso 1 1 calc R . . N7 N 0.9189(4) 0.4513(3) 0.1744(3) 0.0324(11) Uani 1 1 d . . . N8 N 0.5139(4) 0.0681(3) 0.1370(3) 0.0419(13) Uani 1 1 d . . . N9 N 0.6045(5) -0.0750(4) 0.2279(3) 0.0578(16) Uani 1 1 d . . . H9 H 0.6429 -0.0924 0.2726 0.069 Uiso 1 1 calc R . . N10 N 0.3495(6) -0.0935(3) 0.2147(3) 0.0537(15) Uani 1 1 d . . . N11 N 0.2318(4) 0.0569(3) 0.2312(3) 0.0426(13) Uani 1 1 d . . . H11 H 0.2438 0.0986 0.1855 0.051 Uiso 1 1 calc R . . N12 N 0.2842(4) 0.2088(3) 0.2119(3) 0.0383(12) Uani 1 1 d . . . N13 N 0.3811(5) -0.0938(3) 0.3673(3) 0.0429(13) Uani 1 1 d . . . H13 H 0.4460 -0.1313 0.3794 0.051 Uiso 1 1 calc R . . N14 N 0.4594(4) 0.0572(3) 0.3257(3) 0.0328(11) Uani 1 1 d . . . Zn1 Zn 0.83870(7) 0.51379(5) 0.25145(5) 0.0481(3) Uani 1 1 d . . . Zn2 Zn 0.43393(7) -0.00748(4) 0.25096(4) 0.0412(2) Uani 1 1 d . . . Cl1 Cl 0.31431(15) 0.62893(11) 0.14894(10) 0.0564(5) Uani 1 1 d D . . O1 O 0.1885(5) 0.6538(5) 0.1342(5) 0.062(2) Uani 0.631(4) 1 d PDU A . O2 O 0.3891(12) 0.6386(9) 0.0749(6) 0.082(4) Uani 0.631(4) 1 d PDU A . O3 O 0.3135(8) 0.5460(3) 0.1932(5) 0.061(2) Uani 0.631(4) 1 d PDU A . O4 O 0.3541(11) 0.6785(6) 0.1888(7) 0.073(3) Uani 0.631(4) 1 d PDU A . O1A O 0.2308(12) 0.6965(6) 0.1235(10) 0.096(4) Uani 0.369(4) 1 d PDU A 2 O2A O 0.4015(16) 0.6186(12) 0.0848(8) 0.083(6) Uani 0.369(4) 1 d PDU A 2 O3A O 0.2482(12) 0.5580(6) 0.1841(9) 0.068(4) Uani 0.369(4) 1 d PDU A 2 O4A O 0.3771(17) 0.6436(9) 0.2073(9) 0.071(4) Uani 0.369(4) 1 d PDU A 2 Cl2 Cl 0.46812(15) -0.31337(10) 0.47744(10) 0.0487(4) Uani 1 1 d D . . O5 O 0.3959(5) -0.2853(3) 0.5370(3) 0.0835(19) Uani 1 1 d D . . O6 O 0.5272(6) -0.2471(3) 0.4210(3) 0.098(2) Uani 1 1 d D . . O7 O 0.5624(6) -0.3702(5) 0.5030(4) 0.146(4) Uani 1 1 d D . . O8 O 0.3891(6) -0.3373(6) 0.4358(6) 0.167(4) Uani 1 1 d DU . . Cl3 Cl 0.91050(16) -0.14226(12) 0.34200(11) 0.0592(5) Uani 1 1 d D . . O9 O 0.8832(6) -0.0577(3) 0.3218(4) 0.114(3) Uani 1 1 d D . . O10 O 0.9875(4) -0.1606(3) 0.2769(3) 0.0671(15) Uani 1 1 d D . . O11 O 0.7964(5) -0.1764(4) 0.3554(5) 0.122(3) Uani 1 1 d D . . O12 O 0.9740(7) -0.1588(8) 0.4066(4) 0.189(5) Uani 1 1 d DU . . Cl4 Cl 0.18263(18) 0.18008(15) -0.00606(12) 0.0722(6) Uani 1 1 d D . . O13 O 0.2234(9) 0.2400(5) 0.0242(6) 0.092(2) Uani 0.631(4) 1 d PDU A . O14 O 0.2904(7) 0.1712(8) -0.0564(6) 0.112(3) Uani 0.631(4) 1 d PDU A . O15 O 0.1121(9) 0.2340(6) -0.0645(6) 0.112(3) Uani 0.631(4) 1 d PDU A . O16 O 0.0992(10) 0.1282(7) 0.0433(7) 0.130(3) Uani 0.631(4) 1 d PDU A . O13A O 0.2403(13) 0.2440(7) -0.0621(7) 0.114(3) Uani 0.369(4) 1 d PDU A 2 O14A O 0.2674(9) 0.1072(5) -0.0006(8) 0.076(3) Uani 0.369(4) 1 d PDU A 2 O15A O 0.0735(9) 0.1595(8) -0.0274(9) 0.117(3) Uani 0.369(4) 1 d PDU A 2 O16A O 0.1602(14) 0.1892(9) 0.0710(5) 0.114(3) Uani 0.369(4) 1 d PDU A 2 O17 O -0.0033(12) 0.3044(8) -0.1194(8) 0.069(4) Uani 0.369(4) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(4) 0.085(6) 0.074(6) -0.052(5) -0.017(4) 0.015(4) C2 0.064(5) 0.088(6) 0.059(5) -0.047(5) -0.028(4) 0.030(4) C3 0.066(6) 0.132(9) 0.065(6) -0.071(6) -0.024(5) 0.048(6) C4 0.040(4) 0.136(9) 0.067(6) -0.078(6) -0.010(4) 0.019(5) C5 0.042(5) 0.196(13) 0.101(8) -0.114(9) -0.013(5) 0.015(7) C6 0.044(5) 0.229(16) 0.129(11) -0.138(11) 0.007(7) -0.027(8) C7 0.043(5) 0.174(11) 0.130(9) -0.121(9) 0.019(6) -0.031(6) C8 0.053(5) 0.109(8) 0.085(6) -0.075(6) 0.011(5) -0.016(5) C9 0.038(4) 0.102(7) 0.068(5) -0.066(5) -0.001(4) 0.005(4) C10 0.070(5) 0.082(7) 0.156(10) -0.092(7) 0.000(6) -0.017(5) C11 0.056(5) 0.076(6) 0.120(8) -0.078(6) 0.004(5) 0.000(4) C12 0.051(4) 0.063(5) 0.073(5) -0.043(4) 0.002(4) 0.006(4) C13 0.041(3) 0.045(4) 0.056(4) -0.023(3) 0.002(3) 0.003(3) C14 0.030(3) 0.033(3) 0.037(3) -0.010(3) -0.001(3) -0.011(3) C15 0.035(3) 0.038(4) 0.045(4) -0.001(3) -0.005(3) -0.008(3) C16 0.042(4) 0.050(4) 0.041(4) -0.009(3) -0.005(3) -0.015(3) C17 0.049(4) 0.044(4) 0.040(4) -0.013(3) -0.003(3) -0.022(3) C18 0.036(3) 0.039(4) 0.038(4) -0.011(3) -0.001(3) -0.015(3) C19 0.055(4) 0.038(4) 0.049(4) -0.015(3) 0.000(3) -0.016(3) C20 0.051(4) 0.027(4) 0.062(5) -0.015(3) 0.005(4) -0.008(3) C21 0.038(3) 0.036(4) 0.035(4) 0.003(3) -0.004(3) -0.003(3) C22 0.032(3) 0.027(3) 0.035(3) -0.007(3) 0.000(3) -0.011(3) C23 0.063(5) 0.028(4) 0.106(7) -0.019(4) -0.006(5) 0.011(4) C24 0.055(4) 0.026(4) 0.083(6) -0.004(4) -0.002(4) 0.006(3) C25 0.043(4) 0.030(4) 0.052(4) -0.001(3) -0.003(3) -0.014(3) C26 0.042(4) 0.044(4) 0.066(5) 0.011(4) -0.014(4) -0.004(3) C27 0.049(4) 0.059(5) 0.042(4) 0.011(4) -0.015(3) -0.023(4) C28 0.040(4) 0.058(5) 0.043(4) -0.005(3) -0.006(3) -0.021(4) C29 0.031(3) 0.044(4) 0.039(4) -0.008(3) -0.004(3) -0.015(3) C30 0.038(3) 0.043(4) 0.039(4) -0.017(3) 0.003(3) -0.015(3) C31 0.030(3) 0.033(3) 0.042(4) -0.012(3) 0.002(3) -0.001(3) C32 0.031(3) 0.044(4) 0.033(3) -0.014(3) -0.002(3) -0.002(3) C33 0.031(3) 0.030(3) 0.041(4) -0.007(3) -0.004(3) -0.014(3) C34 0.041(4) 0.052(4) 0.052(4) -0.022(4) -0.012(3) 0.006(3) C35 0.050(4) 0.055(4) 0.041(4) -0.018(3) -0.005(3) -0.005(3) C36 0.052(4) 0.067(5) 0.043(4) -0.028(4) 0.001(3) -0.006(4) C37 0.039(4) 0.071(5) 0.035(4) -0.034(4) -0.001(3) -0.001(4) C38 0.050(4) 0.098(7) 0.051(5) -0.040(5) -0.009(4) 0.009(4) C39 0.044(4) 0.112(7) 0.053(5) -0.052(5) -0.005(4) 0.010(5) C40 0.072(5) 0.102(7) 0.050(5) -0.049(5) -0.035(4) 0.041(5) C41 0.058(4) 0.076(5) 0.041(4) -0.038(4) -0.009(3) 0.015(4) C42 0.044(4) 0.057(4) 0.040(4) -0.033(3) -0.015(3) 0.014(3) C43 0.093(6) 0.044(5) 0.075(6) -0.021(4) 0.001(5) 0.027(4) C44 0.114(7) 0.050(5) 0.057(5) -0.035(4) -0.008(5) -0.002(5) C45 0.098(6) 0.049(5) 0.058(5) -0.025(4) -0.029(5) -0.011(4) C46 0.064(4) 0.045(4) 0.057(4) -0.022(4) -0.025(4) -0.006(4) C47 0.038(3) 0.032(3) 0.041(4) -0.011(3) -0.014(3) -0.002(3) C48 0.040(3) 0.033(4) 0.050(4) -0.003(3) -0.013(3) -0.006(3) C49 0.037(3) 0.042(4) 0.036(4) -0.001(3) -0.004(3) 0.002(3) C50 0.038(3) 0.046(4) 0.039(4) -0.012(3) -0.004(3) 0.007(3) C51 0.031(3) 0.032(3) 0.043(4) -0.009(3) -0.011(3) 0.006(3) C52 0.040(3) 0.039(4) 0.060(4) -0.020(3) -0.014(3) 0.005(3) C53 0.040(4) 0.033(4) 0.070(5) -0.010(4) -0.006(3) -0.002(3) C54 0.037(3) 0.035(4) 0.050(4) 0.001(3) -0.007(3) -0.002(3) C55 0.024(3) 0.030(3) 0.047(4) -0.006(3) -0.008(3) 0.004(3) C56 0.089(5) 0.033(4) 0.061(5) -0.019(4) -0.016(4) -0.009(4) C57 0.071(5) 0.029(4) 0.058(4) -0.013(3) -0.010(4) -0.011(3) C58 0.038(3) 0.029(3) 0.039(4) -0.009(3) -0.011(3) 0.004(3) C59 0.048(4) 0.035(4) 0.038(4) -0.007(3) -0.003(3) -0.004(3) C60 0.039(3) 0.035(4) 0.034(3) -0.004(3) -0.002(3) -0.001(3) C61 0.037(3) 0.050(4) 0.032(3) -0.014(3) -0.011(3) 0.007(3) C62 0.026(3) 0.034(3) 0.040(4) -0.010(3) -0.010(3) 0.004(3) C63 0.034(3) 0.035(4) 0.042(4) -0.018(3) -0.010(3) -0.005(3) C64 0.039(3) 0.040(4) 0.040(4) -0.011(3) -0.001(3) -0.008(3) C65 0.028(3) 0.039(4) 0.038(4) -0.009(3) -0.003(3) -0.002(3) C66 0.030(3) 0.035(3) 0.032(3) -0.010(3) -0.007(3) 0.000(3) N1 0.044(3) 0.076(5) 0.069(4) -0.053(4) -0.016(3) 0.007(3) N2 0.058(4) 0.076(5) 0.105(6) -0.064(4) -0.005(4) -0.013(4) N3 0.058(4) 0.049(4) 0.088(5) -0.043(4) 0.002(4) 0.000(3) N4 0.040(3) 0.030(3) 0.045(3) -0.013(2) -0.004(2) 0.001(2) N5 0.036(3) 0.031(3) 0.043(3) -0.009(2) -0.002(2) -0.007(2) N6 0.043(3) 0.033(3) 0.081(4) -0.013(3) -0.007(3) -0.005(3) N7 0.029(2) 0.032(3) 0.037(3) -0.010(2) -0.002(2) -0.007(2) N8 0.039(3) 0.052(4) 0.039(3) -0.021(3) -0.006(2) 0.008(3) N9 0.067(4) 0.057(4) 0.052(4) -0.026(3) -0.012(3) 0.024(3) N10 0.081(4) 0.039(3) 0.049(4) -0.021(3) -0.018(3) -0.001(3) N11 0.050(3) 0.036(3) 0.046(3) -0.012(3) -0.014(3) -0.007(3) N12 0.035(3) 0.036(3) 0.041(3) -0.005(2) -0.007(2) 0.000(2) N13 0.057(3) 0.032(3) 0.045(3) -0.018(2) -0.010(3) -0.002(3) N14 0.031(2) 0.036(3) 0.034(3) -0.013(2) -0.006(2) 0.003(2) Zn1 0.0470(5) 0.0448(5) 0.0642(6) -0.0332(4) -0.0116(4) 0.0030(4) Zn2 0.0524(5) 0.0356(4) 0.0388(4) -0.0174(3) -0.0068(3) 0.0049(3) Cl1 0.0502(10) 0.0593(12) 0.0511(11) -0.0024(9) -0.0105(9) 0.0023(9) O1 0.047(4) 0.053(5) 0.091(5) -0.021(5) -0.022(4) -0.004(4) O2 0.076(6) 0.081(7) 0.067(6) 0.003(5) 0.011(5) -0.012(5) O3 0.057(6) 0.052(4) 0.057(4) 0.000(4) 0.002(5) 0.012(4) O4 0.065(5) 0.068(8) 0.101(7) -0.050(6) -0.008(4) -0.004(6) O1A 0.075(7) 0.075(7) 0.115(7) 0.005(7) -0.021(6) 0.013(6) O2A 0.083(9) 0.087(11) 0.066(8) -0.006(8) 0.008(8) -0.014(8) O3A 0.069(8) 0.063(6) 0.062(6) -0.004(5) -0.004(7) -0.010(6) O4A 0.061(7) 0.061(9) 0.104(8) -0.049(8) -0.003(6) 0.000(7) Cl2 0.0529(10) 0.0416(10) 0.0567(11) -0.0241(8) -0.0044(8) -0.0008(8) O5 0.094(4) 0.081(4) 0.080(4) -0.049(3) 0.035(3) -0.024(3) O6 0.098(4) 0.072(4) 0.087(4) 0.003(3) 0.034(4) 0.019(3) O7 0.104(5) 0.178(8) 0.088(5) 0.031(5) 0.005(4) 0.065(5) O8 0.104(5) 0.216(9) 0.260(10) -0.182(8) -0.028(6) -0.022(6) Cl3 0.0575(11) 0.0692(13) 0.0517(11) -0.0217(10) 0.0002(9) -0.0057(10) O9 0.127(6) 0.091(5) 0.134(6) -0.073(5) 0.045(5) -0.027(4) O10 0.064(3) 0.072(4) 0.070(3) -0.035(3) 0.009(3) -0.005(3) O11 0.109(5) 0.109(5) 0.162(7) -0.086(5) 0.075(5) -0.070(5) O12 0.130(6) 0.335(13) 0.058(5) -0.012(6) -0.024(4) 0.073(7) Cl4 0.0567(11) 0.1195(19) 0.0527(11) -0.0397(12) -0.0064(9) -0.0180(12) O13 0.091(5) 0.096(5) 0.097(5) -0.028(4) -0.032(4) -0.012(4) O14 0.097(5) 0.132(6) 0.110(5) -0.042(5) -0.012(5) -0.013(5) O15 0.119(5) 0.108(5) 0.113(5) -0.010(5) -0.051(5) -0.041(4) O16 0.118(5) 0.120(6) 0.125(6) 0.010(5) -0.007(5) -0.030(5) O13A 0.105(5) 0.116(5) 0.117(5) -0.019(5) -0.019(5) -0.019(5) O14A 0.071(6) 0.104(7) 0.080(7) -0.055(6) -0.027(6) -0.015(6) O15A 0.109(6) 0.112(6) 0.123(6) -0.004(5) -0.031(5) -0.045(5) O16A 0.109(6) 0.118(6) 0.105(6) -0.014(5) -0.018(5) -0.007(5) O17 0.065(9) 0.051(9) 0.074(10) 0.017(7) -0.015(7) -0.017(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 1.330(10) . ? C1 C2 1.395(11) . ? C2 C3 1.353(12) . ? C3 C4 1.392(13) . ? C4 C9 1.431(12) . ? C4 C5 1.441(13) . ? C5 C6 1.343(16) . ? C6 C7 1.406(17) . ? C7 C8 1.414(11) . ? C8 N2 1.410(12) . ? C8 C9 1.439(12) . ? C9 N1 1.369(9) . ? C10 N2 1.488(10) . ? C10 C11 1.515(11) . ? C11 N3 1.487(9) . ? C12 N3 1.491(9) . ? C12 C13 1.514(9) . ? C13 N4 1.492(8) . ? C14 C15 1.379(8) . ? C14 N4 1.429(7) . ? C14 C22 1.434(8) . ? C15 C16 1.403(9) . ? C16 C17 1.364(9) . ? C17 C18 1.391(9) . ? C18 C19 1.409(9) . ? C18 C22 1.419(8) . ? C19 C20 1.360(10) . ? C20 C21 1.418(9) . ? C21 N5 1.304(8) . ? C22 N5 1.383(8) . ? C23 N3 1.489(10) . ? C23 C24 1.545(11) . ? C24 N6 1.488(8) . ? C25 C26 1.360(10) . ? C25 C33 1.409(9) . ? C25 N6 1.442(9) . ? C26 C27 1.399(11) . ? C27 C28 1.347(10) . ? C28 C29 1.432(9) . ? C29 C30 1.398(9) . ? C29 C33 1.421(9) . ? C30 C31 1.371(9) . ? C31 C32 1.405(8) . ? C32 N7 1.327(7) . ? C33 N7 1.357(7) . ? C34 N8 1.318(8) . ? C34 C35 1.409(9) . ? C35 C36 1.352(9) . ? C36 C37 1.370(10) . ? C37 C38 1.409(9) . ? C37 C42 1.423(9) . ? C38 C39 1.327(11) . ? C39 C40 1.394(11) . ? C40 C41 1.393(10) . ? C41 C42 1.392(10) . ? C41 N9 1.473(9) . ? C42 N8 1.379(8) . ? C43 N9 1.469(10) . ? C43 C44 1.531(12) . ? C44 N10 1.489(10) . ? C45 N10 1.471(10) . ? C45 C46 1.517(10) . ? C46 N11 1.482(8) . ? C47 C48 1.380(8) . ? C47 N11 1.419(8) . ? C47 C55 1.440(8) . ? C48 C49 1.392(9) . ? C49 C50 1.360(9) . ? C50 C51 1.424(8) . ? C51 C55 1.403(9) . ? C51 C52 1.415(8) . ? C52 C53 1.363(9) . ? C53 C54 1.383(9) . ? C54 N12 1.313(8) . ? C55 N12 1.374(7) . ? C56 N10 1.484(9) . ? C56 C57 1.533(10) . ? C57 N13 1.489(8) . ? C58 C59 1.352(8) . ? C58 C66 1.410(8) . ? C58 N13 1.452(8) . ? C59 C60 1.416(9) . ? C60 C61 1.364(8) . ? C61 C62 1.412(8) . ? C62 C63 1.409(8) . ? C62 C66 1.420(8) . ? C63 C64 1.362(8) . ? C64 C65 1.392(8) . ? C65 N14 1.328(7) . ? C66 N14 1.378(7) . ? N1 Zn1 2.188(7) . ? N2 Zn1 2.178(6) . ? N3 Zn1 2.134(6) . ? N4 Zn1 2.517(5) . ? N6 Zn1 2.218(6) . ? N7 Zn1 2.061(5) . ? N8 Zn2 2.201(5) . ? N9 Zn2 2.177(6) . ? N10 Zn2 2.155(5) . ? N11 Zn2 2.435(5) . ? N13 Zn2 2.230(5) . ? N14 Zn2 2.069(5) . ? Cl1 O4 1.421(5) . ? Cl1 O2A 1.432(5) . ? Cl1 O2 1.433(6) . ? Cl1 O3A 1.435(5) . ? Cl1 O1A 1.436(5) . ? Cl1 O3 1.437(5) . ? Cl1 O4A 1.447(6) . ? Cl1 O1 1.460(5) . ? O1 O1A 0.881(14) . ? O1 O3A 1.771(13) . ? O3 O3A 0.763(13) . ? O4 O4A 0.652(18) . ? Cl2 O7 1.403(5) . ? Cl2 O8 1.408(5) . ? Cl2 O5 1.416(4) . ? Cl2 O6 1.437(4) . ? Cl3 O12 1.402(5) . ? Cl3 O11 1.411(4) . ? Cl3 O9 1.430(5) . ? Cl3 O10 1.439(4) . ? Cl4 O16 1.382(6) . ? Cl4 O13A 1.401(5) . ? Cl4 O14 1.410(6) . ? Cl4 O16A 1.429(5) . ? Cl4 O15A 1.436(5) . ? Cl4 O13 1.457(5) . ? Cl4 O15 1.464(6) . ? Cl4 O14A 1.496(5) . ? 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(7) . . ? C3 C2 C1 119.5(9) . . ? C2 C3 C4 119.5(8) . . ? C3 C4 C9 118.4(8) . . ? C3 C4 C5 124.7(10) . . ? C9 C4 C5 116.9(10) . . ? C6 C5 C4 121.8(11) . . ? C5 C6 C7 122.0(10) . . ? C6 C7 C8 119.8(12) . . ? N2 C8 C7 122.4(10) . . ? N2 C8 C9 119.1(7) . . ? C7 C8 C9 118.5(10) . . ? N1 C9 C4 120.9(9) . . ? N1 C9 C8 118.2(8) . . ? C4 C9 C8 120.8(8) . . ? N2 C10 C11 110.8(7) . . ? N3 C11 C10 110.0(7) . . ? N3 C12 C13 112.1(6) . . ? N4 C13 C12 108.2(5) . . ? C15 C14 N4 125.0(6) . . ? C15 C14 C22 118.9(6) . . ? N4 C14 C22 116.0(5) . . ? C14 C15 C16 119.8(6) . . ? C17 C16 C15 122.1(6) . . ? C16 C17 C18 119.6(6) . . ? C17 C18 C19 123.7(6) . . ? C17 C18 C22 119.9(6) . . ? C19 C18 C22 116.4(6) . . ? C20 C19 C18 120.3(6) . . ? C19 C20 C21 118.7(6) . . ? N5 C21 C20 124.4(6) . . ? N5 C22 C18 123.5(5) . . ? N5 C22 C14 117.2(5) . . ? C18 C22 C14 119.4(5) . . ? N3 C23 C24 112.8(6) . . ? N6 C24 C23 109.3(6) . . ? C26 C25 C33 119.8(7) . . ? C26 C25 N6 124.1(7) . . ? C33 C25 N6 116.1(6) . . ? C25 C26 C27 121.5(7) . . ? C28 C27 C26 120.7(7) . . ? C27 C28 C29 120.1(7) . . ? C30 C29 C33 118.1(6) . . ? C30 C29 C28 123.1(6) . . ? C33 C29 C28 118.7(6) . . ? C31 C30 C29 119.9(6) . . ? C30 C31 C32 118.2(6) . . ? N7 C32 C31 123.8(6) . . ? N7 C33 C25 119.2(6) . . ? N7 C33 C29 121.6(6) . . ? C25 C33 C29 119.2(6) . . ? N8 C34 C35 123.8(6) . . ? C36 C35 C34 119.0(7) . . ? C35 C36 C37 119.9(6) . . ? C36 C37 C38 123.4(7) . . ? C36 C37 C42 118.6(6) . . ? C38 C37 C42 118.0(7) . . ? C39 C38 C37 120.9(7) . . ? C38 C39 C40 122.3(7) . . ? C41 C40 C39 119.0(8) . . ? C42 C41 C40 119.9(7) . . ? C42 C41 N9 118.2(6) . . ? C40 C41 N9 121.9(7) . . ? N8 C42 C41 118.6(6) . . ? N8 C42 C37 121.5(6) . . ? C41 C42 C37 119.9(6) . . ? N9 C43 C44 112.4(6) . . ? N10 C44 C43 110.8(6) . . ? N10 C45 C46 112.3(6) . . ? N11 C46 C45 108.4(6) . . ? C48 C47 N11 125.6(5) . . ? C48 C47 C55 117.9(6) . . ? N11 C47 C55 116.4(5) . . ? C47 C48 C49 120.7(6) . . ? C50 C49 C48 122.2(6) . . ? C49 C50 C51 119.4(6) . . ? C55 C51 C52 117.3(5) . . ? C55 C51 C50 118.9(5) . . ? C52 C51 C50 123.8(6) . . ? C53 C52 C51 119.3(6) . . ? C52 C53 C54 118.7(6) . . ? N12 C54 C53 125.2(6) . . ? N12 C55 C51 122.8(5) . . ? N12 C55 C47 116.6(6) . . ? C51 C55 C47 120.6(5) . . ? N10 C56 C57 114.2(5) . . ? N13 C57 C56 109.0(6) . . ? C59 C58 C66 120.3(6) . . ? C59 C58 N13 124.1(5) . . ? C66 C58 N13 115.6(5) . . ? C58 C59 C60 120.8(6) . . ? C61 C60 C59 120.4(5) . . ? C60 C61 C62 120.0(6) . . ? C63 C62 C61 123.2(6) . . ? C63 C62 C66 117.6(5) . . ? C61 C62 C66 119.2(5) . . ? C64 C63 C62 119.9(6) . . ? C63 C64 C65 119.7(5) . . ? N14 C65 C64 122.8(5) . . ? N14 C66 C58 119.6(5) . . ? N14 C66 C62 121.1(5) . . ? C58 C66 C62 119.2(5) . . ? C1 N1 C9 117.8(7) . . ? C1 N1 Zn1 130.1(5) . . ? C9 N1 Zn1 111.9(6) . . ? C8 N2 C10 111.5(7) . . ? C8 N2 Zn1 110.2(5) . . ? C10 N2 Zn1 104.0(4) . . ? C11 N3 C23 110.4(6) . . ? C11 N3 C12 111.2(6) . . ? C23 N3 C12 112.0(6) . . ? C11 N3 Zn1 102.5(4) . . ? C23 N3 Zn1 111.3(5) . . ? C12 N3 Zn1 109.1(4) . . ? C14 N4 C13 119.3(5) . . ? C14 N4 Zn1 114.1(3) . . ? C13 N4 Zn1 105.0(3) . . ? C21 N5 C22 116.7(5) . . ? C25 N6 C24 114.4(6) . . ? C25 N6 Zn1 107.9(4) . . ? C24 N6 Zn1 106.5(4) . . ? C32 N7 C33 118.3(5) . . ? C32 N7 Zn1 125.9(4) . . ? C33 N7 Zn1 114.7(4) . . ? C34 N8 C42 117.0(6) . . ? C34 N8 Zn2 130.0(4) . . ? C42 N8 Zn2 112.7(4) . . ? C43 N9 C41 112.7(6) . . ? C43 N9 Zn2 104.7(5) . . ? C41 N9 Zn2 109.8(4) . . ? C45 N10 C56 112.1(6) . . ? C45 N10 C44 112.5(6) . . ? C56 N10 C44 111.4(6) . . ? C45 N10 Zn2 107.3(4) . . ? C56 N10 Zn2 111.0(4) . . ? C44 N10 Zn2 102.1(4) . . ? C47 N11 C46 119.7(5) . . ? C47 N11 Zn2 114.1(4) . . ? C46 N11 Zn2 105.6(4) . . ? C54 N12 C55 116.6(6) . . ? C58 N13 C57 115.0(5) . . ? C58 N13 Zn2 108.0(3) . . ? C57 N13 Zn2 106.8(4) . . ? C65 N14 C66 118.8(5) . . ? C65 N14 Zn2 126.0(4) . . ? C66 N14 Zn2 114.2(4) . . ? N7 Zn1 N3 154.3(2) . . ? N7 Zn1 N2 112.0(2) . . ? N3 Zn1 N2 85.1(2) . . ? N7 Zn1 N1 101.8(2) . . ? N3 Zn1 N1 100.2(2) . . ? N2 Zn1 N1 78.9(3) . . ? N7 Zn1 N6 78.4(2) . . ? N3 Zn1 N6 81.3(2) . . ? N2 Zn1 N6 94.6(3) . . ? N1 Zn1 N6 173.1(2) . . ? N7 Zn1 N4 90.12(16) . . ? N3 Zn1 N4 76.60(19) . . ? N2 Zn1 N4 156.9(2) . . ? N1 Zn1 N4 90.6(2) . . ? N6 Zn1 N4 96.24(18) . . ? N14 Zn2 N10 155.6(2) . . ? N14 Zn2 N9 108.3(2) . . ? N10 Zn2 N9 85.3(2) . . ? N14 Zn2 N8 102.17(19) . . ? N10 Zn2 N8 100.5(2) . . ? N9 Zn2 N8 77.9(2) . . ? N14 Zn2 N13 78.45(18) . . ? N10 Zn2 N13 80.5(2) . . ? N9 Zn2 N13 93.5(2) . . ? N8 Zn2 N13 171.2(2) . . ? N14 Zn2 N11 92.58(18) . . ? N10 Zn2 N11 77.9(2) . . ? N9 Zn2 N11 158.0(2) . . ? N8 Zn2 N11 91.15(18) . . ? N13 Zn2 N11 97.59(19) . . ? O4 Cl1 O2 109.4(7) . . ? O2A Cl1 O1A 110.6(6) . . ? O3A Cl1 O1A 110.0(6) . . ? O4 Cl1 O3 113.2(6) . . ? O2 Cl1 O3 110.7(7) . . ? O2A Cl1 O4A 109.6(6) . . ? O3A Cl1 O4A 108.4(6) . . ? O1A Cl1 O4A 107.9(6) . . ? O4 Cl1 O1 109.3(6) . . ? O2 Cl1 O1 107.8(7) . . ? O3 Cl1 O1 106.2(5) . . ? O7 Cl2 O8 114.7(6) . . ? O7 Cl2 O5 114.5(5) . . ? O8 Cl2 O5 108.2(4) . . ? O7 Cl2 O6 105.8(4) . . ? O8 Cl2 O6 104.1(6) . . ? O5 Cl2 O6 108.8(3) . . ? O12 Cl3 O11 116.2(6) . . ? O12 Cl3 O9 104.7(6) . . ? O11 Cl3 O9 105.3(4) . . ? O12 Cl3 O10 110.7(4) . . ? O11 Cl3 O10 111.2(4) . . ? O9 Cl3 O10 108.1(4) . . ? O16 Cl4 O14 134.7(8) . . ? O13A Cl4 O16A 114.1(6) . . ? O13A Cl4 O15A 113.9(6) . . ? O16A Cl4 O15A 110.6(6) . . ? O16 Cl4 O13 116.9(8) . . ? O14 Cl4 O13 97.6(6) . . ? O16 Cl4 O15 104.8(7) . . ? O14 Cl4 O15 97.9(7) . . ? O13 Cl4 O15 98.1(6) . . ? O13A Cl4 O14A 107.5(5) . . ? O16A Cl4 O14A 105.5(5) . . ? O15A Cl4 O14A 104.4(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.056 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.090 # Attachment '02LISA4_new.CIF' data_02LISA4 _database_code_depnum_ccdc_archive 'CCDC 736254' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 Cd N7, 2(Cl O4), 2(C2 H3 N)' _chemical_formula_sum 'C37 H39 Cd Cl2 N9 O8' _chemical_formula_weight 921.07 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5127(1) _cell_length_b 12.0043(2) _cell_length_c 15.6429(2) _cell_angle_alpha 85.2158(7) _cell_angle_beta 86.6217(7) _cell_angle_gamma 64.5989(6) _cell_volume 1945.44(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7476 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8941 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38824 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8866 _reflns_number_gt 7476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0453P)^2^+1.9570P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8866 _refine_ls_number_parameters 516 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.327013(18) 0.452946(18) 0.218333(12) 0.01917(7) Uani 1 1 d . . . N1 N 0.1775(2) 0.6194(2) 0.30102(15) 0.0216(5) Uani 1 1 d . . . N2 N 0.1483(2) 0.4093(2) 0.26319(15) 0.0213(5) Uani 1 1 d . . . H2n H 0.1794 0.3286 0.2870 0.026 Uiso 1 1 calc R . . N3 N 0.2709(2) 0.3781(2) 0.09038(15) 0.0239(5) Uani 1 1 d . . . N4 N 0.4974(2) 0.2445(2) 0.19658(15) 0.0232(5) Uani 1 1 d . . . H4 H 0.5684 0.2558 0.1741 0.028 Uiso 1 1 calc R . . N5 N 0.4315(2) 0.3528(2) 0.35326(15) 0.0224(5) Uani 1 1 d . . . N6 N 0.2629(2) 0.6248(2) 0.10303(15) 0.0249(5) Uani 1 1 d . . . H6n H 0.1747 0.6729 0.1073 0.030 Uiso 1 1 calc R . . N7 N 0.4816(2) 0.5379(2) 0.19990(15) 0.0237(5) Uani 1 1 d . . . C1 C 0.1870(3) 0.7226(3) 0.3153(2) 0.0279(7) Uani 1 1 d . . . H1 H 0.2554 0.7369 0.2875 0.033 Uiso 1 1 calc R . . C2 C 0.1017(3) 0.8114(3) 0.3689(2) 0.0329(7) Uani 1 1 d . . . H2 H 0.1120 0.8844 0.3763 0.039 Uiso 1 1 calc R . . C3 C 0.0041(3) 0.7921(3) 0.4101(2) 0.0304(7) Uani 1 1 d . . . H3 H -0.0536 0.8510 0.4474 0.037 Uiso 1 1 calc R . . C4 C -0.0112(3) 0.6840(3) 0.39720(18) 0.0244(6) Uani 1 1 d . . . C5 C -0.1085(3) 0.6565(3) 0.43965(19) 0.0268(6) Uani 1 1 d . . . H5 H -0.1683 0.7127 0.4777 0.032 Uiso 1 1 calc R . . C6 C -0.1165(3) 0.5494(3) 0.42607(19) 0.0285(7) Uani 1 1 d . . . H6 H -0.1812 0.5306 0.4553 0.034 Uiso 1 1 calc R . . C7 C -0.0297(3) 0.4666(3) 0.36917(19) 0.0256(6) Uani 1 1 d . . . H7 H -0.0365 0.3922 0.3606 0.031 Uiso 1 1 calc R . . C8 C 0.0645(3) 0.4908(3) 0.32565(18) 0.0211(6) Uani 1 1 d . . . C9 C 0.0781(3) 0.5998(3) 0.34042(17) 0.0207(6) Uani 1 1 d . . . C10 C 0.0781(3) 0.4183(3) 0.18442(19) 0.0266(6) Uani 1 1 d . . . H10A H 0.0386 0.5051 0.1607 0.032 Uiso 1 1 calc R . . H10B H 0.0084 0.3918 0.1987 0.032 Uiso 1 1 calc R . . C11 C 0.1698(3) 0.3370(3) 0.1182(2) 0.0286(7) Uani 1 1 d . . . H11A H 0.2106 0.2507 0.1429 0.034 Uiso 1 1 calc R . . H11B H 0.1209 0.3387 0.0678 0.034 Uiso 1 1 calc R . . C12 C 0.3879(3) 0.2744(3) 0.05955(19) 0.0286(7) Uani 1 1 d . . . H12A H 0.4445 0.3080 0.0284 0.034 Uiso 1 1 calc R . . H12B H 0.3630 0.2306 0.0184 0.034 Uiso 1 1 calc R . . C13 C 0.4630(3) 0.1823(3) 0.13104(19) 0.0301(7) Uani 1 1 d . . . H13A H 0.4105 0.1413 0.1584 0.036 Uiso 1 1 calc R . . H13B H 0.5423 0.1180 0.1066 0.036 Uiso 1 1 calc R . . C14 C 0.5386(3) 0.1689(3) 0.27523(19) 0.0233(6) Uani 1 1 d . . . C15 C 0.6094(3) 0.0432(3) 0.2765(2) 0.0313(7) Uani 1 1 d . . . H15 H 0.6353 0.0043 0.2238 0.038 Uiso 1 1 calc R . . C16 C 0.6443(3) -0.0293(3) 0.3543(2) 0.0346(8) Uani 1 1 d . . . H16 H 0.6908 -0.1164 0.3534 0.041 Uiso 1 1 calc R . . C17 C 0.6125(3) 0.0237(3) 0.4305(2) 0.0315(7) Uani 1 1 d . . . H17 H 0.6368 -0.0264 0.4825 0.038 Uiso 1 1 calc R . . C18 C 0.5429(3) 0.1539(3) 0.43276(19) 0.0253(6) Uani 1 1 d . . . C19 C 0.5128(3) 0.2152(3) 0.5098(2) 0.0290(7) Uani 1 1 d . . . H19 H 0.5384 0.1694 0.5633 0.035 Uiso 1 1 calc R . . C20 C 0.4468(3) 0.3404(3) 0.5068(2) 0.0312(7) Uani 1 1 d . . . H20 H 0.4281 0.3833 0.5578 0.037 Uiso 1 1 calc R . . C21 C 0.4065(3) 0.4055(3) 0.42691(19) 0.0266(6) Uani 1 1 d . . . H21 H 0.3584 0.4926 0.4260 0.032 Uiso 1 1 calc R . . C22 C 0.5032(3) 0.2272(3) 0.35429(18) 0.0210(6) Uani 1 1 d . . . C23 C 0.2247(3) 0.4789(3) 0.02213(19) 0.0287(7) Uani 1 1 d . . . H23A H 0.1312 0.5291 0.0309 0.034 Uiso 1 1 calc R . . H23B H 0.2383 0.4429 -0.0343 0.034 Uiso 1 1 calc R . . C24 C 0.2937(3) 0.5613(3) 0.02182(19) 0.0294(7) Uani 1 1 d . . . H24A H 0.3877 0.5111 0.0161 0.035 Uiso 1 1 calc R . . H24B H 0.2663 0.6231 -0.0276 0.035 Uiso 1 1 calc R . . C25 C 0.3290(3) 0.7012(3) 0.11001(18) 0.0242(6) Uani 1 1 d . . . C26 C 0.2861(3) 0.8189(3) 0.0724(2) 0.0315(7) Uani 1 1 d . . . H26 H 0.2109 0.8511 0.0392 0.038 Uiso 1 1 calc R . . C27 C 0.3512(3) 0.8932(3) 0.0819(2) 0.0356(8) Uani 1 1 d . . . H27 H 0.3187 0.9749 0.0561 0.043 Uiso 1 1 calc R . . C28 C 0.4604(3) 0.8481(3) 0.1278(2) 0.0339(8) Uani 1 1 d . . . H28 H 0.5039 0.8987 0.1337 0.041 Uiso 1 1 calc R . . C29 C 0.5099(3) 0.7272(3) 0.16688(19) 0.0283(7) Uani 1 1 d . . . C30 C 0.6234(3) 0.6748(3) 0.2148(2) 0.0345(8) Uani 1 1 d . . . H30 H 0.6718 0.7208 0.2210 0.041 Uiso 1 1 calc R . . C31 C 0.6629(3) 0.5591(4) 0.2518(2) 0.0370(8) Uani 1 1 d . . . H31 H 0.7404 0.5222 0.2827 0.044 Uiso 1 1 calc R . . C32 C 0.5878(3) 0.4937(3) 0.2441(2) 0.0304(7) Uani 1 1 d . . . H32 H 0.6152 0.4136 0.2723 0.036 Uiso 1 1 calc R . . C33 C 0.4423(3) 0.6533(3) 0.15894(18) 0.0225(6) Uani 1 1 d . . . N8 N -0.2280(3) 0.2237(3) 0.1647(2) 0.0532(9) Uani 1 1 d . . . C34 C -0.1266(4) 0.1497(4) 0.1554(2) 0.0411(8) Uani 1 1 d . . . C35 C 0.0042(4) 0.0562(4) 0.1424(3) 0.0666(14) Uani 1 1 d . . . H35A H 0.0274 0.0552 0.0810 0.100 Uiso 1 1 calc R . . H35B H 0.0097 -0.0251 0.1634 0.100 Uiso 1 1 calc R . . H35C H 0.0637 0.0755 0.1739 0.100 Uiso 1 1 calc R . . N9 N -0.2696(3) 0.3627(3) 0.4298(2) 0.0449(8) Uani 1 1 d . . . C36 C -0.2167(3) 0.2617(3) 0.4158(2) 0.0312(7) Uani 1 1 d . . . C37 C -0.1492(3) 0.1319(3) 0.3993(2) 0.0385(8) Uani 1 1 d . . . H37A H -0.0592 0.1123 0.3836 0.058 Uiso 1 1 calc R . . H37B H -0.1899 0.1143 0.3520 0.058 Uiso 1 1 calc R . . H37C H -0.1531 0.0814 0.4510 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.21548(7) 0.08624(7) 0.34295(5) 0.02985(17) Uani 1 1 d . . . O1 O 0.1687(2) 0.0443(2) 0.41944(15) 0.0424(6) Uani 1 1 d . . . O2 O 0.3014(4) -0.0177(3) 0.3001(2) 0.0880(12) Uani 1 1 d . . . O3 O 0.1083(3) 0.1619(3) 0.29007(19) 0.0573(8) Uani 1 1 d . . . O4 O 0.2778(3) 0.1601(3) 0.3661(2) 0.0541(8) Uani 1 1 d . . . Cl2 Cl -0.12123(8) 0.80705(8) 0.10410(6) 0.0394(2) Uani 1 1 d . . . O5 O -0.1450(5) 0.7015(5) 0.0915(3) 0.1087(16) Uani 1 1 d . . . O6 O -0.0178(4) 0.7948(5) 0.0509(4) 0.1258(19) Uani 1 1 d . . . O7 O -0.0957(5) 0.8030(4) 0.1913(3) 0.1191(16) Uani 1 1 d U . . O8 O -0.2293(4) 0.9102(4) 0.0837(3) 0.1228(16) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01628(11) 0.01981(12) 0.01993(11) 0.00036(8) -0.00012(7) -0.00662(9) N1 0.0204(12) 0.0204(12) 0.0225(12) -0.0007(10) 0.0011(9) -0.0076(10) N2 0.0184(12) 0.0206(12) 0.0236(12) -0.0023(10) 0.0002(9) -0.0070(10) N3 0.0232(13) 0.0234(13) 0.0228(12) -0.0015(10) 0.0010(10) -0.0078(11) N4 0.0197(12) 0.0226(13) 0.0241(12) -0.0006(10) 0.0006(9) -0.0064(10) N5 0.0155(11) 0.0253(13) 0.0248(12) 0.0004(10) 0.0010(9) -0.0078(10) N6 0.0197(12) 0.0256(13) 0.0254(13) 0.0014(10) -0.0009(10) -0.0063(11) N7 0.0181(12) 0.0260(13) 0.0262(12) 0.0022(10) 0.0010(10) -0.0094(11) C1 0.0324(17) 0.0243(16) 0.0287(16) -0.0006(13) 0.0023(13) -0.0141(14) C2 0.0386(19) 0.0213(16) 0.0372(18) -0.0046(14) 0.0010(14) -0.0110(14) C3 0.0336(17) 0.0217(16) 0.0273(16) -0.0048(13) 0.0007(13) -0.0032(14) C4 0.0216(15) 0.0240(15) 0.0205(14) -0.0004(12) -0.0023(11) -0.0030(12) C5 0.0186(14) 0.0297(17) 0.0237(15) -0.0024(13) 0.0004(11) -0.0023(13) C6 0.0182(15) 0.0392(19) 0.0251(15) 0.0001(13) 0.0016(11) -0.0101(14) C7 0.0200(14) 0.0299(16) 0.0265(15) 0.0001(13) -0.0014(11) -0.0104(13) C8 0.0142(13) 0.0250(15) 0.0214(14) 0.0004(12) -0.0020(10) -0.0058(12) C9 0.0186(14) 0.0225(15) 0.0180(13) 0.0019(11) -0.0014(10) -0.0063(12) C10 0.0216(15) 0.0341(17) 0.0264(15) -0.0054(13) -0.0011(12) -0.0135(14) C11 0.0298(16) 0.0336(18) 0.0271(15) -0.0080(13) 0.0025(12) -0.0175(14) C12 0.0301(16) 0.0292(17) 0.0226(15) -0.0058(13) 0.0018(12) -0.0086(14) C13 0.0335(17) 0.0262(17) 0.0260(15) -0.0077(13) 0.0023(13) -0.0077(14) C14 0.0191(14) 0.0223(15) 0.0273(15) 0.0022(12) -0.0028(11) -0.0080(12) C15 0.0292(17) 0.0250(16) 0.0370(18) -0.0026(14) -0.0068(13) -0.0082(14) C16 0.0333(18) 0.0193(16) 0.048(2) 0.0058(14) -0.0131(15) -0.0084(14) C17 0.0291(17) 0.0280(17) 0.0380(18) 0.0132(14) -0.0127(13) -0.0141(14) C18 0.0185(14) 0.0305(17) 0.0280(15) 0.0077(13) -0.0042(11) -0.0127(13) C19 0.0202(15) 0.0387(19) 0.0253(15) 0.0078(13) -0.0024(12) -0.0114(14) C20 0.0208(15) 0.041(2) 0.0253(15) -0.0029(14) 0.0018(12) -0.0074(14) C21 0.0209(15) 0.0285(16) 0.0253(15) -0.0015(13) 0.0024(12) -0.0061(13) C22 0.0136(13) 0.0229(15) 0.0267(14) 0.0028(12) -0.0014(11) -0.0087(12) C23 0.0308(16) 0.0314(17) 0.0220(14) 0.0028(13) -0.0073(12) -0.0114(14) C24 0.0348(17) 0.0326(18) 0.0197(14) 0.0031(13) -0.0016(12) -0.0141(15) C25 0.0248(15) 0.0248(15) 0.0207(14) 0.0000(12) 0.0029(11) -0.0090(13) C26 0.0328(17) 0.0289(17) 0.0253(15) 0.0003(13) 0.0036(13) -0.0071(14) C27 0.046(2) 0.0202(16) 0.0349(18) -0.0008(14) 0.0084(15) -0.0103(15) C28 0.048(2) 0.0269(17) 0.0325(17) -0.0072(14) 0.0107(15) -0.0222(16) C29 0.0329(17) 0.0306(17) 0.0239(15) -0.0049(13) 0.0101(12) -0.0168(14) C30 0.0372(18) 0.049(2) 0.0308(17) -0.0050(15) 0.0029(14) -0.0309(17) C31 0.0280(17) 0.055(2) 0.0344(17) 0.0045(16) -0.0062(13) -0.0243(17) C32 0.0226(16) 0.0369(18) 0.0299(16) 0.0071(14) -0.0045(12) -0.0123(14) C33 0.0220(14) 0.0240(15) 0.0216(14) -0.0024(12) 0.0041(11) -0.0102(12) N8 0.0352(19) 0.052(2) 0.056(2) 0.0078(17) 0.0092(15) -0.0067(17) C34 0.039(2) 0.045(2) 0.0377(19) -0.0028(17) -0.0019(16) -0.0161(19) C35 0.040(2) 0.060(3) 0.082(3) -0.028(3) -0.013(2) 0.001(2) N9 0.0451(19) 0.0378(19) 0.054(2) 0.0023(15) -0.0082(15) -0.0200(16) C36 0.0258(16) 0.036(2) 0.0352(17) 0.0076(15) -0.0030(13) -0.0180(15) C37 0.0276(17) 0.0326(19) 0.054(2) -0.0002(16) 0.0006(15) -0.0119(15) Cl1 0.0309(4) 0.0288(4) 0.0309(4) 0.0006(3) 0.0026(3) -0.0146(3) O1 0.0511(16) 0.0564(17) 0.0328(13) 0.0031(12) 0.0006(11) -0.0367(14) O2 0.091(3) 0.069(2) 0.082(2) -0.036(2) 0.041(2) -0.013(2) O3 0.070(2) 0.0580(18) 0.0579(17) 0.0258(14) -0.0358(15) -0.0419(16) O4 0.0458(16) 0.0503(17) 0.081(2) 0.0202(15) -0.0210(14) -0.0359(14) Cl2 0.0297(4) 0.0399(5) 0.0404(5) -0.0061(4) -0.0126(3) -0.0050(4) O5 0.164(4) 0.142(4) 0.079(3) -0.017(3) 0.001(3) -0.119(4) O6 0.057(2) 0.134(4) 0.183(5) -0.007(4) 0.038(3) -0.044(3) O7 0.159(3) 0.109(3) 0.078(2) -0.002(2) -0.073(2) -0.038(2) O8 0.091(3) 0.106(3) 0.085(2) 0.001(2) -0.011(2) 0.040(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.385(2) . ? Cd1 N7 2.395(2) . ? Cd1 N1 2.418(2) . ? Cd1 N5 2.446(2) . ? Cd1 N4 2.465(2) . ? Cd1 N3 2.486(2) . ? Cd1 N6 2.507(2) . ? N1 C1 1.327(4) . ? N1 C9 1.366(4) . ? N2 C8 1.443(4) . ? N2 C10 1.485(4) . ? N3 C12 1.477(4) . ? N3 C11 1.478(4) . ? N3 C23 1.479(4) . ? N4 C14 1.441(4) . ? N4 C13 1.481(4) . ? N5 C21 1.318(4) . ? N5 C22 1.373(4) . ? N6 C25 1.434(4) . ? N6 C24 1.482(4) . ? N7 C32 1.318(4) . ? N7 C33 1.372(4) . ? C1 C2 1.399(4) . ? C2 C3 1.359(5) . ? C3 C4 1.414(4) . ? C4 C5 1.413(4) . ? C4 C9 1.421(4) . ? C5 C6 1.363(5) . ? C6 C7 1.403(4) . ? C7 C8 1.370(4) . ? C8 C9 1.422(4) . ? C10 C11 1.515(4) . ? C12 C13 1.519(4) . ? C14 C15 1.373(4) . ? C14 C22 1.423(4) . ? C15 C16 1.408(5) . ? C16 C17 1.353(5) . ? C17 C18 1.420(5) . ? C18 C19 1.412(4) . ? C18 C22 1.425(4) . ? C19 C20 1.361(5) . ? C20 C21 1.407(4) . ? C23 C24 1.511(4) . ? C25 C26 1.373(4) . ? C25 C33 1.421(4) . ? C26 C27 1.409(5) . ? C27 C28 1.359(5) . ? C28 C29 1.410(5) . ? C29 C30 1.414(5) . ? C29 C33 1.425(4) . ? C30 C31 1.352(5) . ? C31 C32 1.410(5) . ? N8 C34 1.133(5) . ? C34 C35 1.457(6) . ? N9 C36 1.133(5) . ? C36 C37 1.451(5) . ? Cl1 O2 1.410(3) . ? Cl1 O1 1.425(2) . ? Cl1 O4 1.436(3) . ? Cl1 O3 1.437(3) . ? Cl2 O8 1.357(4) . ? Cl2 O6 1.373(4) . ? Cl2 O7 1.405(4) . ? Cl2 O5 1.436(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N7 164.86(8) . . ? N2 Cd1 N1 71.20(8) . . ? N7 Cd1 N1 93.96(8) . . ? N2 Cd1 N5 89.44(8) . . ? N7 Cd1 N5 86.81(8) . . ? N1 Cd1 N5 87.32(8) . . ? N2 Cd1 N4 101.83(8) . . ? N7 Cd1 N4 90.51(8) . . ? N1 Cd1 N4 155.64(8) . . ? N5 Cd1 N4 69.01(8) . . ? N2 Cd1 N3 74.52(8) . . ? N7 Cd1 N3 118.10(8) . . ? N1 Cd1 N3 124.90(8) . . ? N5 Cd1 N3 134.10(8) . . ? N4 Cd1 N3 72.68(8) . . ? N2 Cd1 N6 110.49(8) . . ? N7 Cd1 N6 68.70(8) . . ? N1 Cd1 N6 80.96(8) . . ? N5 Cd1 N6 151.83(8) . . ? N4 Cd1 N6 122.76(8) . . ? N3 Cd1 N6 72.32(8) . . ? C1 N1 C9 117.9(2) . . ? C1 N1 Cd1 126.55(19) . . ? C9 N1 Cd1 115.42(18) . . ? C8 N2 C10 111.1(2) . . ? C8 N2 Cd1 113.44(17) . . ? C10 N2 Cd1 106.50(17) . . ? C12 N3 C11 111.1(2) . . ? C12 N3 C23 109.6(2) . . ? C11 N3 C23 111.1(2) . . ? C12 N3 Cd1 108.13(17) . . ? C11 N3 Cd1 107.06(16) . . ? C23 N3 Cd1 109.77(17) . . ? C14 N4 C13 112.8(2) . . ? C14 N4 Cd1 113.42(17) . . ? C13 N4 Cd1 111.88(17) . . ? C21 N5 C22 118.0(3) . . ? C21 N5 Cd1 124.9(2) . . ? C22 N5 Cd1 116.00(18) . . ? C25 N6 C24 113.2(2) . . ? C25 N6 Cd1 111.38(17) . . ? C24 N6 Cd1 104.43(18) . . ? C32 N7 C33 118.3(3) . . ? C32 N7 Cd1 122.3(2) . . ? C33 N7 Cd1 117.25(18) . . ? N1 C1 C2 123.6(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 119.7(3) . . ? C5 C4 C3 122.7(3) . . ? C5 C4 C9 119.9(3) . . ? C3 C4 C9 117.3(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C7 120.4(3) . . ? C8 C7 C6 121.4(3) . . ? C7 C8 C9 119.6(3) . . ? C7 C8 N2 121.2(3) . . ? C9 C8 N2 119.2(2) . . ? N1 C9 C4 122.1(3) . . ? N1 C9 C8 119.2(2) . . ? C4 C9 C8 118.6(3) . . ? N2 C10 C11 110.0(2) . . ? N3 C11 C10 111.8(2) . . ? N3 C12 C13 113.5(2) . . ? N4 C13 C12 111.0(3) . . ? C15 C14 C22 119.1(3) . . ? C15 C14 N4 122.4(3) . . ? C22 C14 N4 118.5(3) . . ? C14 C15 C16 121.3(3) . . ? C17 C16 C15 120.8(3) . . ? C16 C17 C18 120.2(3) . . ? C19 C18 C17 122.8(3) . . ? C19 C18 C22 117.9(3) . . ? C17 C18 C22 119.2(3) . . ? C20 C19 C18 119.4(3) . . ? C19 C20 C21 119.0(3) . . ? N5 C21 C20 124.0(3) . . ? N5 C22 C14 119.3(3) . . ? N5 C22 C18 121.5(3) . . ? C14 C22 C18 119.3(3) . . ? N3 C23 C24 111.7(2) . . ? N6 C24 C23 109.3(2) . . ? C26 C25 C33 118.9(3) . . ? C26 C25 N6 122.7(3) . . ? C33 C25 N6 118.4(3) . . ? C25 C26 C27 121.5(3) . . ? C28 C27 C26 120.2(3) . . ? C27 C28 C29 120.8(3) . . ? C28 C29 C30 123.4(3) . . ? C28 C29 C33 119.0(3) . . ? C30 C29 C33 117.6(3) . . ? C31 C30 C29 119.7(3) . . ? C30 C31 C32 119.3(3) . . ? N7 C32 C31 123.4(3) . . ? N7 C33 C25 118.8(3) . . ? N7 C33 C29 121.5(3) . . ? C25 C33 C29 119.6(3) . . ? N8 C34 C35 178.9(5) . . ? N9 C36 C37 179.2(4) . . ? O2 Cl1 O1 108.5(2) . . ? O2 Cl1 O4 111.5(2) . . ? O1 Cl1 O4 108.44(16) . . ? O2 Cl1 O3 110.8(2) . . ? O1 Cl1 O3 108.83(17) . . ? O4 Cl1 O3 108.78(16) . . ? O8 Cl2 O6 113.1(3) . . ? O8 Cl2 O7 109.7(3) . . ? O6 Cl2 O7 113.0(3) . . ? O8 Cl2 O5 108.0(3) . . ? O6 Cl2 O5 105.2(3) . . ? O7 Cl2 O5 107.6(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.201 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.115 # Attachment 'pge0301.cif' data_pge0301 _database_code_depnum_ccdc_archive 'CCDC 736255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C33 H30 Co N7), 2(C4 H10 O), C4 H10 O' _chemical_formula_sum 'C144 H150 Co4 N28 O3' _chemical_formula_weight 2556.64 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.726(5) _cell_length_b 13.120(5) _cell_length_c 24.291(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 108.174(5) _cell_angle_gamma 90.000(5) _cell_volume 6881(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26904 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2684 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8777 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44726 _diffrn_reflns_av_R_equivalents 0.1517 _diffrn_reflns_av_sigmaI/netI 0.1594 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7810 _reflns_number_gt 3934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1538P)^2^+8.0367P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7810 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1862 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2939 _refine_ls_wR_factor_gt 0.2467 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.5531(2) 0.3964(4) 0.9902(2) 0.0270(12) Uani 1 1 d . . . H1 H 0.5229 0.3459 0.9734 0.032 Uiso 1 1 calc R . . C2 C 0.5497(3) 0.4903(4) 0.9624(3) 0.0312(13) Uani 1 1 d . . . H2 H 0.5177 0.5027 0.9271 0.037 Uiso 1 1 calc R . . C3 C 0.5926(3) 0.5646(4) 0.9862(3) 0.0326(14) Uani 1 1 d . . . H3 H 0.5909 0.6281 0.9669 0.039 Uiso 1 1 calc R . . C4 C 0.6392(2) 0.5470(4) 1.0392(3) 0.0287(13) Uani 1 1 d . . . C5 C 0.6400(2) 0.4497(4) 1.0635(2) 0.0239(12) Uani 1 1 d . . . C6 C 0.6840(3) 0.6197(4) 1.0674(3) 0.0330(14) Uani 1 1 d . . . H6 H 0.6839 0.6863 1.0520 0.040 Uiso 1 1 calc R . . C7 C 0.7290(3) 0.5900(4) 1.1193(3) 0.0335(14) Uani 1 1 d . . . H7 H 0.7593 0.6385 1.1391 0.040 Uiso 1 1 calc R . . C8 C 0.7312(3) 0.4930(4) 1.1431(3) 0.0311(13) Uani 1 1 d . . . H8 H 0.7622 0.4772 1.1785 0.037 Uiso 1 1 calc R . . C9 C 0.6882(2) 0.4187(4) 1.1154(2) 0.0240(12) Uani 1 1 d . . . C10 C 0.7325(3) 0.2812(4) 1.1817(2) 0.0298(13) Uani 1 1 d . . . H10A H 0.7724 0.3141 1.1839 0.036 Uiso 1 1 calc R . . H10B H 0.7373 0.2071 1.1766 0.036 Uiso 1 1 calc R . . C11 C 0.7200(3) 0.2980(5) 1.2391(2) 0.0335(14) Uani 1 1 d . . . H11A H 0.7566 0.2737 1.2705 0.040 Uiso 1 1 calc R . . H11B H 0.7167 0.3723 1.2444 0.040 Uiso 1 1 calc R . . C12 C 0.6105(3) 0.3118(5) 1.2391(3) 0.0352(14) Uani 1 1 d . . . H12A H 0.6202 0.3633 1.2704 0.042 Uiso 1 1 calc R . . H12B H 0.5776 0.2671 1.2445 0.042 Uiso 1 1 calc R . . C13 C 0.5841(3) 0.3677(4) 1.1809(2) 0.0276(13) Uani 1 1 d . . . H13A H 0.5489 0.4106 1.1829 0.033 Uiso 1 1 calc R . . H13B H 0.6164 0.4139 1.1758 0.033 Uiso 1 1 calc R . . C14 C 0.5043(2) 0.2655(4) 1.1154(2) 0.0245(12) Uani 1 1 d . . . C15 C 0.4587(3) 0.2795(4) 1.1430(3) 0.0311(14) Uani 1 1 d . . . H15 H 0.4683 0.3173 1.1780 0.037 Uiso 1 1 calc R . . C16 C 0.3996(3) 0.2380(4) 1.1191(3) 0.0329(14) Uani 1 1 d . . . H16 H 0.3703 0.2475 1.1392 0.040 Uiso 1 1 calc R . . C17 C 0.3815(3) 0.1836(4) 1.0674(3) 0.0319(14) Uani 1 1 d . . . H17 H 0.3402 0.1595 1.0516 0.038 Uiso 1 1 calc R . . C18 C 0.4268(3) 0.1650(4) 1.0386(2) 0.0288(13) Uani 1 1 d . . . C19 C 0.4868(2) 0.2037(4) 1.0633(2) 0.0241(12) Uani 1 1 d . . . C20 C 0.4146(3) 0.1132(4) 0.9860(3) 0.0314(14) Uani 1 1 d . . . H20 H 0.3741 0.0883 0.9669 0.038 Uiso 1 1 calc R . . C21 C 0.4609(3) 0.0985(4) 0.9619(3) 0.0329(14) Uani 1 1 d . . . H21 H 0.4529 0.0629 0.9262 0.039 Uiso 1 1 calc R . . C22 C 0.5202(2) 0.1363(4) 0.9904(2) 0.0269(13) Uani 1 1 d . . . H22 H 0.5525 0.1242 0.9740 0.032 Uiso 1 1 calc R . . C23 C 0.6665(2) 0.2174(4) 0.9902(2) 0.0276(13) Uani 1 1 d . . . H23 H 0.6481 0.2798 0.9736 0.033 Uiso 1 1 calc R . . C24 C 0.7011(3) 0.1613(4) 0.9622(3) 0.0337(14) Uani 1 1 d . . . H24 H 0.7050 0.1853 0.9266 0.040 Uiso 1 1 calc R . . C25 C 0.7293(3) 0.0721(4) 0.9856(2) 0.0312(13) Uani 1 1 d . . . H25 H 0.7527 0.0342 0.9663 0.037 Uiso 1 1 calc R . . C26 C 0.7234(2) 0.0368(4) 1.0387(3) 0.0275(13) Uani 1 1 d . . . C27 C 0.6864(2) 0.0965(4) 1.0639(2) 0.0234(12) Uani 1 1 d . . . C28 C 0.7513(3) -0.0528(4) 1.0669(3) 0.0348(14) Uani 1 1 d . . . H28 H 0.7765 -0.0940 1.0512 0.042 Uiso 1 1 calc R . . C29 C 0.7406(3) -0.0794(4) 1.1193(3) 0.0353(15) Uani 1 1 d . . . H29 H 0.7602 -0.1387 1.1392 0.042 Uiso 1 1 calc R . . C30 C 0.7026(2) -0.0231(4) 1.1435(3) 0.0315(13) Uani 1 1 d . . . H30 H 0.6967 -0.0446 1.1787 0.038 Uiso 1 1 calc R . . C31 C 0.6728(2) 0.0664(4) 1.1154(2) 0.0250(12) Uani 1 1 d . . . C32 C 0.6147(3) 0.1022(4) 1.1811(2) 0.0288(13) Uani 1 1 d . . . H32A H 0.6122 0.0270 1.1834 0.035 Uiso 1 1 calc R . . H32B H 0.5728 0.1297 1.1758 0.035 Uiso 1 1 calc R . . C33 C 0.6584(3) 0.1416(4) 1.2391(2) 0.0326(14) Uani 1 1 d . . . H33A H 0.6434 0.1150 1.2704 0.039 Uiso 1 1 calc R . . H33B H 0.6999 0.1117 1.2447 0.039 Uiso 1 1 calc R . . N1 N 0.5972(2) 0.3756(3) 1.03920(19) 0.0227(10) Uani 1 1 d . . . N2 N 0.68488(19) 0.3199(3) 1.13047(19) 0.0245(10) Uani 1 1 d . . . N3 N 0.6656(2) 0.2499(3) 1.2464(2) 0.0291(10) Uani 1 1 d . . . N4 N 0.5628(2) 0.3024(3) 1.13004(19) 0.0240(10) Uani 1 1 d . . . N5 N 0.53269(19) 0.1882(3) 1.03901(19) 0.0236(10) Uani 1 1 d . . . N6 N 0.65886(19) 0.1860(3) 1.03905(19) 0.0246(10) Uani 1 1 d . . . N7 N 0.6322(2) 0.1277(3) 1.13037(19) 0.0234(10) Uani 1 1 d . . . Co1 Co 0.61171(3) 0.24999(5) 1.08500(3) 0.0215(3) Uani 1 1 d . . . O1 O 0.9021(7) 0.1590(12) 0.2479(8) 0.112(5) Uiso 0.50 1 d P . . O2 O 0.5000 0.9444(17) 0.2500 0.115(7) Uiso 0.50 2 d SP . . C34 C 0.5598(9) 0.9483(15) 0.3448(9) 0.088(6) Uiso 0.50 1 d P . . H34A H 0.5853 0.9959 0.3735 0.132 Uiso 0.50 1 calc PR . . H34B H 0.5853 0.8908 0.3401 0.132 Uiso 0.50 1 calc PR . . H34C H 0.5259 0.9231 0.3581 0.132 Uiso 0.50 1 calc PR . . C35 C 0.8890(10) 0.0987(18) 0.1581(11) 0.109(7) Uiso 0.50 1 d P . . H35A H 0.8606 0.0535 0.1299 0.164 Uiso 0.50 1 calc PR . . H35B H 0.9312 0.0715 0.1681 0.164 Uiso 0.50 1 calc PR . . H35C H 0.8878 0.1668 0.1412 0.164 Uiso 0.50 1 calc PR . . C36 C 0.5402(8) 0.9884(14) 0.3023(8) 0.078(5) Uiso 0.50 1 d P . . H36A H 0.5762 1.0153 0.2923 0.093 Uiso 0.50 1 calc PR . . H36B H 0.5179 1.0486 0.3104 0.093 Uiso 0.50 1 calc PR . . C37 C 0.8749(9) 0.1034(16) 0.1971(9) 0.085(6) Uiso 0.50 1 d P . . H37A H 0.8740 0.0320 0.2100 0.103 Uiso 0.50 1 calc PR . . H37B H 0.8312 0.1260 0.1834 0.103 Uiso 0.50 1 calc PR . . C38 C 0.8891(8) 0.1660(15) 0.3030(9) 0.079(5) Uiso 0.50 1 d P . . H38A H 0.8531 0.2124 0.2953 0.095 Uiso 0.50 1 calc PR . . H38B H 0.8735 0.0977 0.3088 0.095 Uiso 0.50 1 calc PR . . C39 C 0.9197(9) 0.1884(16) 0.3461(10) 0.093(6) Uiso 0.50 1 d P . . H39A H 0.8968 0.1847 0.3742 0.140 Uiso 0.50 1 calc PR . . H39B H 0.9343 0.2583 0.3445 0.140 Uiso 0.50 1 calc PR . . H39C H 0.9553 0.1421 0.3580 0.140 Uiso 0.50 1 calc PR . . 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 0.031(3) 0.023(3) 0.027(3) -0.001(2) 0.008(3) 0.002(2) C2 0.029(3) 0.038(3) 0.025(3) 0.011(3) 0.005(2) 0.005(3) C3 0.041(3) 0.027(3) 0.032(4) 0.008(3) 0.016(3) 0.006(3) C4 0.032(3) 0.027(3) 0.032(3) 0.000(3) 0.016(3) 0.006(2) C5 0.028(3) 0.023(3) 0.021(3) 0.001(2) 0.009(2) 0.002(2) C6 0.038(3) 0.026(3) 0.038(4) 0.002(3) 0.016(3) 0.000(3) C7 0.031(3) 0.034(3) 0.034(4) -0.011(3) 0.009(3) -0.008(3) C8 0.034(3) 0.036(3) 0.025(3) -0.007(3) 0.010(3) -0.008(3) C9 0.026(3) 0.023(3) 0.025(3) -0.004(2) 0.011(2) 0.001(2) C10 0.027(3) 0.035(3) 0.024(3) 0.002(3) 0.002(3) 0.001(2) C11 0.031(3) 0.041(3) 0.023(3) 0.001(3) 0.002(3) 0.000(3) C12 0.042(4) 0.038(3) 0.027(3) -0.007(3) 0.013(3) -0.003(3) C13 0.036(3) 0.025(3) 0.022(3) -0.005(2) 0.010(3) -0.002(2) C14 0.026(3) 0.028(3) 0.019(3) 0.005(2) 0.005(2) 0.002(2) C15 0.035(3) 0.035(3) 0.023(3) 0.004(3) 0.009(3) 0.005(3) C16 0.033(3) 0.039(3) 0.032(3) 0.004(3) 0.016(3) 0.002(3) C17 0.026(3) 0.033(3) 0.035(4) 0.008(3) 0.008(3) 0.000(2) C18 0.033(3) 0.024(3) 0.029(3) 0.009(3) 0.009(3) 0.002(2) C19 0.027(3) 0.027(3) 0.017(3) 0.001(2) 0.004(2) -0.001(2) C20 0.029(3) 0.028(3) 0.032(4) 0.002(3) 0.003(3) -0.003(2) C21 0.040(3) 0.032(3) 0.024(3) -0.007(3) 0.004(3) -0.005(3) C22 0.028(3) 0.027(3) 0.023(3) -0.006(2) 0.006(2) -0.003(2) C23 0.027(3) 0.032(3) 0.027(3) 0.003(3) 0.013(3) 0.002(2) C24 0.036(3) 0.036(3) 0.032(4) -0.004(3) 0.016(3) -0.008(3) C25 0.034(3) 0.038(3) 0.024(3) -0.006(3) 0.012(3) -0.001(3) C26 0.022(3) 0.028(3) 0.031(3) -0.001(3) 0.005(2) -0.002(2) C27 0.022(3) 0.025(3) 0.022(3) 0.000(2) 0.006(2) 0.001(2) C28 0.029(3) 0.035(3) 0.039(4) -0.005(3) 0.009(3) 0.004(3) C29 0.034(3) 0.032(3) 0.031(4) 0.000(3) -0.003(3) 0.005(3) C30 0.030(3) 0.038(3) 0.022(3) 0.002(3) 0.003(2) 0.002(3) C31 0.028(3) 0.025(3) 0.019(3) -0.001(2) 0.004(2) -0.005(2) C32 0.034(3) 0.028(3) 0.022(3) 0.007(3) 0.007(3) 0.000(2) C33 0.040(3) 0.039(3) 0.020(3) 0.005(3) 0.012(3) 0.005(3) N1 0.028(2) 0.022(2) 0.019(3) 0.0005(19) 0.008(2) 0.0031(19) N2 0.025(2) 0.028(2) 0.019(3) 0.000(2) 0.0044(19) -0.0009(19) N3 0.034(3) 0.034(3) 0.020(3) -0.002(2) 0.010(2) 0.000(2) N4 0.030(3) 0.026(2) 0.017(2) -0.003(2) 0.008(2) -0.004(2) N5 0.027(2) 0.024(2) 0.020(3) 0.003(2) 0.008(2) -0.0015(19) N6 0.023(2) 0.029(2) 0.022(3) 0.000(2) 0.0065(19) -0.0014(19) N7 0.027(2) 0.027(2) 0.017(2) 0.000(2) 0.0077(19) -0.0007(19) Co1 0.0239(4) 0.0228(4) 0.0172(4) 0.0001(3) 0.0055(3) 0.0001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.324(7) . ? C1 C2 1.394(7) . ? C1 H1 0.9500 . ? C2 C3 1.374(8) . ? C2 H2 0.9500 . ? C3 C4 1.406(8) . ? C3 H3 0.9500 . ? C4 C5 1.404(7) . ? C4 C6 1.408(8) . ? C5 N1 1.371(7) . ? C5 C9 1.447(7) . ? C6 C7 1.409(8) . ? C6 H6 0.9500 . ? C7 C8 1.392(8) . ? C7 H7 0.9500 . ? C8 C9 1.396(7) . ? C8 H8 0.9500 . ? C9 N2 1.355(7) . ? C10 N2 1.462(7) . ? C10 C11 1.522(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.448(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.457(7) . ? C12 C13 1.538(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N4 1.457(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.353(7) . ? C14 C15 1.409(8) . ? C14 C19 1.452(8) . ? C15 C16 1.397(8) . ? C15 H15 0.9500 . ? C16 C17 1.390(8) . ? C16 H16 0.9500 . ? C17 C18 1.436(8) . ? C17 H17 0.9500 . ? C18 C20 1.397(8) . ? C18 C19 1.401(7) . ? C19 N5 1.364(7) . ? C20 C21 1.369(8) . ? C20 H20 0.9500 . ? C21 C22 1.400(7) . ? C21 H21 0.9500 . ? C22 N5 1.315(7) . ? C22 H22 0.9500 . ? C23 N6 1.317(7) . ? C23 C24 1.398(8) . ? C23 H23 0.9500 . ? C24 C25 1.371(8) . ? C24 H24 0.9500 . ? C25 C26 1.417(8) . ? C25 H25 0.9500 . ? C26 C28 1.407(8) . ? C26 C27 1.421(7) . ? C27 N6 1.378(7) . ? C27 C31 1.433(7) . ? C28 C29 1.414(9) . ? C28 H28 0.9500 . ? C29 C30 1.397(8) . ? C29 H29 0.9500 . ? C30 C31 1.419(8) . ? C30 H30 0.9500 . ? C31 N7 1.357(7) . ? C32 N7 1.446(7) . ? C32 C33 1.538(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N3 1.435(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? N1 Co1 1.958(4) . ? N2 Co1 1.918(4) . ? N4 Co1 1.915(4) . ? N5 Co1 1.969(4) . ? N6 Co1 1.961(4) . ? N7 Co1 1.920(4) . ? O1 C37 1.40(2) . ? O1 C38 1.46(2) . ? O2 C36 1.434(19) . ? O2 C36 1.434(19) 2_655 ? C34 C36 1.12(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.09(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.10(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? 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 122.0(5) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 116.2(5) . . ? C5 C4 C6 119.9(5) . . ? C3 C4 C6 123.8(5) . . ? N1 C5 C4 123.3(5) . . ? N1 C5 C9 114.7(4) . . ? C4 C5 C9 122.0(5) . . ? C4 C6 C7 117.5(5) . . ? C4 C6 H6 121.3 . . ? C7 C6 H6 121.3 . . ? C8 C7 C6 123.1(5) . . ? C8 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? N2 C9 C8 128.8(5) . . ? N2 C9 C5 114.5(5) . . ? C8 C9 C5 116.7(5) . . ? N2 C10 C11 115.4(5) . . ? N2 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? N2 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? N3 C11 C10 117.3(5) . . ? N3 C11 H11A 108.0 . . ? C10 C11 H11A 108.0 . . ? N3 C11 H11B 108.0 . . ? C10 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? N3 C12 C13 116.9(5) . . ? N3 C12 H12A 108.1 . . ? C13 C12 H12A 108.1 . . ? N3 C12 H12B 108.1 . . ? C13 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? N4 C13 C12 115.4(4) . . ? N4 C13 H13A 108.4 . . ? C12 C13 H13A 108.4 . . ? N4 C13 H13B 108.4 . . ? C12 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? N4 C14 C15 129.5(5) . . ? N4 C14 C19 114.1(5) . . ? C15 C14 C19 116.4(5) . . ? C16 C15 C14 120.4(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 123.4(5) . . ? C17 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C16 C17 C18 118.2(5) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C20 C18 C19 117.2(5) . . ? C20 C18 C17 124.1(5) . . ? C19 C18 C17 118.7(5) . . ? N5 C19 C18 122.3(5) . . ? N5 C19 C14 114.9(5) . . ? C18 C19 C14 122.8(5) . . ? C21 C20 C18 120.0(5) . . ? C21 C20 H20 120.0 . . ? C18 C20 H20 120.0 . . ? C20 C21 C22 119.3(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N5 C22 C21 122.2(5) . . ? N5 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? N6 C23 C24 121.7(5) . . ? N6 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.5(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C28 C26 C25 124.1(5) . . ? C28 C26 C27 119.2(5) . . ? C25 C26 C27 116.7(5) . . ? N6 C27 C26 122.0(5) . . ? N6 C27 C31 115.2(5) . . ? C26 C27 C31 122.8(5) . . ? C26 C28 C29 117.8(5) . . ? C26 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? C30 C29 C28 123.4(5) . . ? C30 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C29 C30 C31 120.0(6) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? N7 C31 C30 128.6(5) . . ? N7 C31 C27 114.9(5) . . ? C30 C31 C27 116.6(5) . . ? N7 C32 C33 115.6(4) . . ? N7 C32 H32A 108.4 . . ? C33 C32 H32A 108.4 . . ? N7 C32 H32B 108.4 . . ? C33 C32 H32B 108.4 . . ? H32A C32 H32B 107.4 . . ? N3 C33 C32 117.6(5) . . ? N3 C33 H33A 107.9 . . ? C32 C33 H33A 107.9 . . ? N3 C33 H33B 107.9 . . ? C32 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Co1 129.1(4) . . ? C5 N1 Co1 112.4(3) . . ? C9 N2 C10 118.3(4) . . ? C9 N2 Co1 114.3(3) . . ? C10 N2 Co1 127.0(4) . . ? C33 N3 C11 119.1(5) . . ? C33 N3 C12 118.4(5) . . ? C11 N3 C12 118.5(4) . . ? C14 N4 C13 118.1(4) . . ? C14 N4 Co1 114.8(3) . . ? C13 N4 Co1 126.7(3) . . ? C22 N5 C19 119.0(5) . . ? C22 N5 Co1 128.7(4) . . ? C19 N5 Co1 112.3(3) . . ? C23 N6 C27 119.5(5) . . ? C23 N6 Co1 128.9(4) . . ? C27 N6 Co1 111.7(3) . . ? C31 N7 C32 118.8(4) . . ? C31 N7 Co1 113.9(3) . . ? C32 N7 Co1 126.9(4) . . ? N4 Co1 N2 93.04(18) . . ? N4 Co1 N7 92.98(18) . . ? N2 Co1 N7 93.32(18) . . ? N4 Co1 N1 89.85(18) . . ? N2 Co1 N1 83.50(19) . . ? N7 Co1 N1 175.86(18) . . ? N4 Co1 N6 175.55(18) . . ? N2 Co1 N6 90.18(18) . . ? N7 Co1 N6 83.76(18) . . ? N1 Co1 N6 93.58(18) . . ? N4 Co1 N5 83.25(18) . . ? N2 Co1 N5 175.27(17) . . ? N7 Co1 N5 89.81(18) . . ? N1 Co1 N5 93.53(18) . . ? N6 Co1 N5 93.69(18) . . ? C37 O1 C38 132.9(16) . . ? C36 O2 C36 133(2) . 2_655 ? C36 C34 H34A 109.5 . . ? C36 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C36 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 H35A 109.5 . . ? C37 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C37 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 O2 126(2) . . ? C34 C36 H36A 105.8 . . ? O2 C36 H36A 105.8 . . ? C34 C36 H36B 105.8 . . ? O2 C36 H36B 105.8 . . ? H36A C36 H36B 106.2 . . ? C35 C37 O1 129(2) . . ? C35 C37 H37A 105.1 . . ? O1 C37 H37A 105.1 . . ? C35 C37 H37B 105.1 . . ? O1 C37 H37B 105.1 . . ? H37A C37 H37B 105.9 . . ? C39 C38 O1 130(2) . . ? C39 C38 H38A 104.8 . . ? O1 C38 H38A 104.8 . . ? C39 C38 H38B 104.8 . . ? O1 C38 H38B 104.8 . . ? H38A C38 H38B 105.8 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.547 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.122 # Attachment 'pge0301_trans.cif' data_pge0301t _database_code_depnum_ccdc_archive 'CCDC 741026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 Co N7, 1.5(C4 H10 O)' _chemical_formula_sum 'C39 H45 Co N7 O1.50' _chemical_formula_weight 694.75 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c:h loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 13.1204(9) _cell_length_b 13.1204(9) _cell_length_c 69.238(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10322.1(17) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1621 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4404 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9327 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42510 _diffrn_reflns_av_R_equivalents 0.1583 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -84 _diffrn_reflns_limit_l_max 89 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2633 _reflns_number_gt 1621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1056P)^2^+49.3122P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2633 _refine_ls_number_parameters 166 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.061 _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 0.0533(3) 0.8804(4) 0.32994(6) 0.0270(9) Uani 1 1 d . . . H1 H 0.1022 0.9556 0.3243 0.032 Uiso 1 1 calc R . . C2 C 0.0411(4) 0.7800(4) 0.32062(6) 0.0310(10) Uani 1 1 d . . . H2 H 0.0806 0.7876 0.3087 0.037 Uiso 1 1 calc R . . C3 C -0.0269(4) 0.6718(4) 0.32854(6) 0.0310(9) Uani 1 1 d . . . H3 H -0.0355 0.6038 0.3222 0.037 Uiso 1 1 calc R . . C4 C -0.0851(3) 0.6603(3) 0.34634(6) 0.0271(9) Uani 1 1 d . . . C5 C -0.0714(3) 0.7650(3) 0.35453(5) 0.0228(8) Uani 1 1 d . . . C6 C -0.1579(4) 0.5517(4) 0.35592(6) 0.0318(10) Uani 1 1 d . . . H6 H -0.1690 0.4798 0.3507 0.038 Uiso 1 1 calc R . . C7 C -0.2122(4) 0.5529(4) 0.37297(6) 0.0329(10) Uani 1 1 d . . . H7 H -0.2591 0.4806 0.3795 0.040 Uiso 1 1 calc R . . C8 C -0.2011(4) 0.6564(4) 0.38102(6) 0.0305(10) Uani 1 1 d . . . H8 H -0.2403 0.6525 0.3928 0.037 Uiso 1 1 calc R . . C9 C -0.1328(3) 0.7654(3) 0.37184(5) 0.0234(9) Uani 1 1 d . . . C10 C -0.1770(4) 0.8805(4) 0.39368(5) 0.0279(9) Uani 1 1 d . . . H10A H -0.2556 0.8089 0.3944 0.033 Uiso 1 1 calc R . . H10B H -0.1893 0.9485 0.3920 0.033 Uiso 1 1 calc R . . C11 C -0.1137(4) 0.8949(4) 0.41296(6) 0.0322(10) Uani 1 1 d . . . H11A H -0.1661 0.8928 0.4234 0.039 Uiso 1 1 calc R . . H11B H -0.1033 0.8258 0.4147 0.039 Uiso 1 1 calc R . . N1 N -0.0019(3) 0.8731(3) 0.34638(4) 0.0226(7) Uani 1 1 d . . . N2 N -0.1168(3) 0.8716(3) 0.37677(4) 0.0236(7) Uani 1 1 d . . . N3 N 0.0000 1.0000 0.41550(8) 0.0287(13) Uani 1 3 d S . . Co1 Co 0.0000 1.0000 0.361665(12) 0.0208(3) Uani 1 3 d S . . O1 O 0.5217(9) 0.8550(9) 0.4167 0.244(9) Uani 1 2 d SD . . C12 C 0.5878(17) 0.7964(15) 0.4448(2) 0.105(5) Uani 0.50 1 d PDU . . H12A H 0.6250 0.8238 0.4574 0.157 Uiso 0.50 1 calc PR . . H12B H 0.6347 0.7727 0.4369 0.157 Uiso 0.50 1 calc PR . . H12C H 0.5084 0.7289 0.4465 0.157 Uiso 0.50 1 calc PR . . C13 C 0.580(2) 0.8963(15) 0.43450(19) 0.115(6) Uani 0.50 1 d PDU . . H13A H 0.5367 0.9236 0.4427 0.138 Uiso 0.50 1 calc PR . . H13B H 0.6604 0.9635 0.4323 0.138 Uiso 0.50 1 calc PR . . C14 C 0.542(2) 0.9425(13) 0.40300(15) 0.123(7) Uani 0.50 1 d PDU . . H14A H 0.6258 1.0057 0.4036 0.148 Uiso 0.50 1 calc PR . . H14B H 0.4925 0.9775 0.4059 0.148 Uiso 0.50 1 calc PR . . C15 C 0.5133(18) 0.8872(15) 0.38270(12) 0.099(5) Uani 0.50 1 d PDU . . H15A H 0.5323 0.9488 0.3730 0.149 Uiso 0.50 1 calc PR . . H15B H 0.4293 0.8287 0.3820 0.149 Uiso 0.50 1 calc PR . . H15C H 0.5598 0.8490 0.3802 0.149 Uiso 0.50 1 calc PR . . 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(2) 0.030(2) 0.025(2) -0.0011(17) 0.0013(17) 0.0171(18) C2 0.032(2) 0.037(2) 0.025(2) -0.0050(18) 0.0016(18) 0.018(2) C3 0.034(2) 0.033(2) 0.031(2) -0.0095(19) -0.0045(18) 0.021(2) C4 0.027(2) 0.030(2) 0.028(2) -0.0013(17) -0.0065(17) 0.0162(18) C5 0.026(2) 0.026(2) 0.0185(19) 0.0003(16) -0.0014(16) 0.0142(17) C6 0.035(2) 0.028(2) 0.035(2) -0.0054(19) -0.0077(19) 0.0175(19) C7 0.036(2) 0.026(2) 0.033(2) 0.0070(18) -0.001(2) 0.0123(19) C8 0.031(2) 0.034(2) 0.025(2) 0.0027(18) -0.0019(17) 0.0150(19) C9 0.025(2) 0.026(2) 0.0198(19) 0.0004(16) -0.0025(15) 0.0129(16) C10 0.029(2) 0.029(2) 0.023(2) 0.0062(17) 0.0073(17) 0.0128(18) C11 0.037(2) 0.038(2) 0.021(2) 0.0038(18) 0.0086(18) 0.018(2) N1 0.0262(17) 0.0261(17) 0.0178(16) -0.0004(13) -0.0014(14) 0.0149(14) N2 0.0266(17) 0.0271(18) 0.0177(16) 0.0004(13) 0.0022(13) 0.0139(15) N3 0.033(2) 0.033(2) 0.019(3) 0.000 0.000 0.0167(10) Co1 0.0231(4) 0.0231(4) 0.0162(5) 0.000 0.000 0.01153(18) O1 0.224(9) 0.224(9) 0.138(10) 0.057(7) -0.057(7) 0.004(12) C12 0.128(12) 0.100(11) 0.104(12) 0.023(9) 0.005(10) 0.069(10) C13 0.125(13) 0.116(12) 0.112(13) 0.004(10) 0.014(10) 0.067(10) C14 0.130(12) 0.134(14) 0.119(12) 0.039(11) 0.027(12) 0.076(11) C15 0.114(11) 0.118(12) 0.097(11) 0.032(10) 0.021(11) 0.082(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(5) . ? C1 C2 1.403(6) . ? C1 H1 0.9500 . ? C2 C3 1.359(6) . ? C2 H2 0.9500 . ? C3 C4 1.417(6) . ? C3 H3 0.9500 . ? C4 C5 1.413(5) . ? C4 C6 1.422(6) . ? C5 N1 1.367(5) . ? C5 C9 1.445(5) . ? C6 C7 1.383(6) . ? C6 H6 0.9500 . ? C7 C8 1.406(6) . ? C7 H7 0.9500 . ? C8 C9 1.404(6) . ? C8 H8 0.9500 . ? C9 N2 1.346(5) . ? C10 N2 1.450(5) . ? C10 C11 1.533(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.449(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N1 Co1 1.963(3) . ? N2 Co1 1.923(3) . ? N3 C11 1.449(4) 4_465 ? N3 C11 1.449(4) 2_675 ? Co1 N2 1.923(3) 4_465 ? Co1 N2 1.923(3) 2_675 ? Co1 N1 1.963(3) 4_465 ? Co1 N1 1.963(3) 2_675 ? O1 C14 1.405(9) . ? O1 C13 1.411(9) . ? C12 C13 1.537(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.540(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 121.7(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 116.5(4) . . ? C5 C4 C6 118.8(4) . . ? C3 C4 C6 124.7(4) . . ? N1 C5 C4 122.5(3) . . ? N1 C5 C9 115.0(3) . . ? C4 C5 C9 122.4(3) . . ? C7 C6 C4 118.6(4) . . ? C7 C6 H6 120.7 . . ? C4 C6 H6 120.7 . . ? C6 C7 C8 123.0(4) . . ? C6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N2 C9 C8 129.0(4) . . ? N2 C9 C5 114.6(3) . . ? C8 C9 C5 116.4(4) . . ? N2 C10 C11 115.4(3) . . ? N2 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? N2 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? N3 C11 C10 117.4(4) . . ? N3 C11 H11A 108.0 . . ? C10 C11 H11A 108.0 . . ? N3 C11 H11B 108.0 . . ? C10 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C1 N1 C5 119.1(3) . . ? C1 N1 Co1 128.8(3) . . ? C5 N1 Co1 112.1(2) . . ? C9 N2 C10 118.7(3) . . ? C9 N2 Co1 114.4(2) . . ? C10 N2 Co1 126.6(3) . . ? C11 N3 C11 118.55(12) . 4_465 ? C11 N3 C11 118.55(12) . 2_675 ? C11 N3 C11 118.55(12) 4_465 2_675 ? N2 Co1 N2 93.24(13) 4_465 2_675 ? N2 Co1 N2 93.24(13) 4_465 . ? N2 Co1 N2 93.24(13) 2_675 . ? N2 Co1 N1 175.43(13) 4_465 . ? N2 Co1 N1 89.94(13) 2_675 . ? N2 Co1 N1 83.31(13) . . ? N2 Co1 N1 83.31(13) 4_465 4_465 ? N2 Co1 N1 175.43(13) 2_675 4_465 ? N2 Co1 N1 89.94(13) . 4_465 ? N1 Co1 N1 93.68(12) . 4_465 ? N2 Co1 N1 89.94(13) 4_465 2_675 ? N2 Co1 N1 83.31(13) 2_675 2_675 ? N2 Co1 N1 175.43(13) . 2_675 ? N1 Co1 N1 93.68(12) . 2_675 ? N1 Co1 N1 93.68(12) 4_465 2_675 ? C14 O1 C13 115.5(9) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 C12 109.4(9) . . ? O1 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? O1 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? O1 C14 C15 109.2(9) . . ? O1 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? O1 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.833 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.109