Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global #=============================================================================== _audit_creation_date 15-05-98 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ziessel, Raymond' 'Stroh, Christophe' _publ_contact_author_name 'Prof Raymond Ziessel' _publ_contact_author_address ; Laboratiore de Chimie Moleculaire UMR 7008, ECPM 25 rue Becquerel Strasbourg Cedex 02 FRANCE ; _publ_contact_author_phone '0390242689' _publ_contact_author_fax '0390242689' _publ_contact_author_email ziessel@chimie.u-strasbg.fr _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Copper(II) Complex of a Pentadentate Ligand Featuring Large Ferro-and Antiferromagnetic Interactions ; _publ_requested_category FM #=============================================================================== _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_st203 _database_code_CSD 186271 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H41 Cl4 N7 O13 Zn' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H41 Cl4 N7 O13 Zn' _chemical_formula_weight 890.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Zn ? 0.222 1.431 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall ' P 32' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -y,+x-y,2/3+z -x+y,-x,1/3+z _cell_length_a 15.4545(3) _cell_length_b 15.4545(3) _cell_length_c 13.5594(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2804.7(1) _cell_formula_units_Z 3 _cell_measurement_temperature 173 _cell_measurement_reflns_used 21257 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 26.4 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 21257 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 25. mm. Scan angle = 1.8 deg 1 scans of 50 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 245 frames Friedel pairs were averaged. Internal R = 0.02 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21257 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3739 _reflns_number_gt 3174 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 3174 _refine_ls_number_parameters 438 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.084 _refine_ls_R_factor_gt 0.075 _refine_ls_wR_factor_all 0.129 _refine_ls_wR_factor_ref 0.096 _refine_ls_goodness_of_fit_all 1.784 _refine_ls_goodness_of_fit_ref 1.330 _refine_ls_shift/su_max 0.024 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.870 _refine_diff_density_min -0.743 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol ZN 0.24085(7) 0.85629(7) 0.5378 0.0332(3) 1.000 Uani ? ? Zn O1 0.1201(6) 0.7533(7) 0.6156(6) 0.050(4) 1.000 Uani ? ? O N1 0.3097(6) 0.7690(6) 0.5032(7) 0.048(4) 1.000 Uani ? ? N C1 0.2733(9) 0.6735(7) 0.523(1) 0.062(5) 1.000 Uani ? ? C C2 0.316(1) 0.6181(9) 0.496(1) 0.086(7) 1.000 Uani ? ? C C3 0.403(1) 0.6690(9) 0.439(1) 0.111(7) 1.000 Uani ? ? C C4 0.4429(8) 0.7704(9) 0.417(1) 0.077(5) 1.000 Uani ? ? C C5 0.3957(7) 0.8194(7) 0.4500(8) 0.051(4) 1.000 Uani ? ? C C6 0.4289(6) 0.9259(7) 0.4276(7) 0.041(4) 1.000 Uani ? ? C N2 0.3659(5) 0.9572(5) 0.4584(6) 0.035(3) 1.000 Uani ? ? N C7 0.3867(7) 1.0496(7) 0.4440(7) 0.036(4) 1.000 Uani ? ? C C8 0.4754(8) 1.1197(9) 0.3970(9) 0.049(5) 1.000 Uani ? ? C C9 0.5406(8) 1.088(1) 0.3684(9) 0.053(5) 1.000 Uani ? ? C C10 0.5170(8) 0.991(1) 0.3826(9) 0.055(5) 1.000 Uani ? ? C C11 0.3100(7) 1.0759(7) 0.4757(8) 0.039(4) 1.000 Uani ? ? C N3 0.2272(5) 0.9969(5) 0.5341(6) 0.031(3) 1.000 Uani ? ? N C12 0.1291(6) 0.9696(6) 0.4920(7) 0.033(3) 1.000 Uani ? ? C C13 0.1145(6) 0.9274(6) 0.3906(6) 0.031(3) 1.000 Uani ? ? C N4 0.0853(5) 0.9621(5) 0.3131(6) 0.036(3) 1.000 Uani ? ? N C14 0.0545(7) 0.8928(6) 0.2273(7) 0.039(4) 1.000 Uani ? ? C C15 0.1113(6) 0.8336(6) 0.2532(6) 0.032(3) 1.000 Uani ? ? C N5 0.1235(5) 0.8517(5) 0.3605(6) 0.033(3) 1.000 Uani ? ? N O2 0.0693(5) 1.0349(4) 0.3172(5) 0.046(3) 1.000 Uani ? ? O O3 0.1483(5) 0.7973(4) 0.4156(5) 0.037(3) 1.000 Uani ? ? O C16 -0.0577(8) 0.8287(8) 0.231(1) 0.057(5) 1.000 Uani ? ? C C17 0.0886(9) 0.9505(7) 0.1316(8) 0.052(5) 1.000 Uani ? ? C C18 0.2176(7) 0.8810(8) 0.2100(8) 0.046(4) 1.000 Uani ? ? C C19 0.0506(8) 0.7222(7) 0.2308(8) 0.043(4) 1.000 Uani ? ? C C20 0.2280(6) 1.0292(6) 0.6386(7) 0.034(3) 1.000 Uani ? ? C C21 0.3223(6) 1.0537(6) 0.6887(7) 0.033(4) 1.000 Uani ? ? C N6 0.3877(6) 1.1443(6) 0.7276(7) 0.041(3) 1.000 Uani ? ? N C22 0.4715(9) 1.1433(9) 0.780(1) 0.066(6) 1.000 Uani ? ? C C23 0.4528(7) 1.0393(8) 0.7605(9) 0.063(5) 1.000 Uani ? ? C N7 0.3569(5) 0.9932(5) 0.7043(6) 0.037(3) 1.000 Uani ? ? N O4 0.3761(6) 1.2204(5) 0.7235(7) 0.055(4) 1.000 Uani ? ? O O5 0.3136(5) 0.8984(4) 0.6758(5) 0.043(3) 1.000 Uani ? ? O C24 0.517(2) 1.199(2) 0.856(2) 0.059(6) 0.500 Uiso ? ? C C25 0.565(2) 1.196(2) 0.679(2) 0.059(6) 0.500 Uiso ? ? C C24A 0.422(2) 1.124(2) 0.902(2) 0.052(5) 0.500 Uiso ? ? C C25A 0.558(2) 1.235(2) 0.797(2) 0.058(6) 0.500 Uiso ? ? C C26 0.404(2) 0.988(2) 0.875(2) 0.063(7) 0.500 Uiso ? ? C C27 0.515(2) 0.994(2) 0.728(2) 0.056(6) 0.500 Uiso ? ? C C26A 0.473(2) 0.982(2) 0.821(2) 0.061(6) 0.500 Uiso ? ? C C27A 0.540(2) 1.079(2) 0.663(2) 0.051(5) 0.500 Uiso ? ? C CL1 0.3572(2) 1.2136(2) 0.1890(2) 0.051(1) 1.000 Uani ? ? Cl O6 0.3289(9) 1.1286(9) 0.242(1) 0.092(3) 1.000 Uiso ? ? O O7 0.462(5) 1.240(5) 0.156(5) 0.25(3) 0.500 Uiso ? ? O O8 0.388(2) 1.305(2) 0.250(3) 0.13(1) 0.500 Uiso ? ? O O9 0.284(2) 1.231(2) 0.149(2) 0.099(8) 0.500 Uiso ? ? O O7a 0.449(2) 1.292(2) 0.234(2) 0.083(6) 0.500 Uiso ? ? O O8a 0.278(4) 1.229(4) 0.242(4) 0.19(2) 0.500 Uiso ? ? O O9a 0.388(2) 1.217(2) 0.090(3) 0.12(1) 0.500 Uiso ? ? O CL2 0.2006(2) 1.3059(2) 0.5462(2) 0.045(1) 1.000 Uani ? ? Cl O10 0.112(1) 1.254(1) 0.498(2) 0.146(6) 1.000 Uiso ? ? O O11 0.2737(7) 1.3825(7) 0.4834(8) 0.070(3) 1.000 Uiso ? ? O O12 0.211(2) 1.348(2) 0.639(2) 0.087(7) 0.500 Uiso ? ? O O13 0.206(3) 1.215(3) 0.547(3) 0.14(1) 0.500 Uiso ? ? O O12a 0.242(2) 1.290(2) 0.628(2) 0.089(7) 0.500 Uiso ? ? O O13a 0.164(2) 1.364(2) 0.604(3) 0.12(1) 0.500 Uiso ? ? O C28 0.909(2) 0.523(2) 0.790(2) 0.14(1) 1.000 Uiso ? ? C CL3 0.9972(8) 0.4723(8) 0.7881(9) 0.196(4) 1.000 Uiso ? ? Cl CL4 0.7971(7) 0.4274(7) 0.8061(8) 0.176(3) 1.000 Uiso ? ? Cl H1 0.2125 0.6406 0.5589 0.0784 1.000 Uiso calc C1 H H2 0.2886 0.5501 0.5147 0.1040 1.000 Uiso calc C2 H H3 0.4351 0.6344 0.4144 0.1254 1.000 Uiso calc C3 H H4 0.5025 0.8049 0.3791 0.0876 1.000 Uiso calc C4 H H5 0.4898 1.1862 0.3854 0.0683 1.000 Uiso calc C8 H H6 0.6024 1.1340 0.3386 0.0761 1.000 Uiso calc C9 H H7 0.5614 0.9690 0.3613 0.0733 1.000 Uiso calc C10 H H8 0.2825 1.0883 0.4184 0.0503 1.000 Uiso calc C11 H H9 0.3421 1.1348 0.5147 0.0503 1.000 Uiso calc C11 H H10 0.1229 1.0277 0.4897 0.0425 1.000 Uiso calc C12 H H11 0.0787 0.9212 0.5336 0.0425 1.000 Uiso calc C12 H H12 -0.0801 0.7833 0.1773 0.0708 1.000 Uiso calc C16 H H13 -0.0768 0.7923 0.2914 0.0708 1.000 Uiso calc C16 H H14 -0.0870 0.8699 0.2274 0.0708 1.000 Uiso calc C16 H H15 0.0683 0.9050 0.0779 0.0680 1.000 Uiso calc C17 H H16 0.0597 0.9919 0.1251 0.0680 1.000 Uiso calc C17 H H17 0.1594 0.9908 0.1317 0.0680 1.000 Uiso calc C17 H H18 0.2138 0.8713 0.1406 0.0579 1.000 Uiso calc C18 H H19 0.2529 0.9505 0.2241 0.0579 1.000 Uiso calc C18 H H20 0.2518 0.8504 0.2387 0.0579 1.000 Uiso calc C18 H H21 0.0438 0.7125 0.1614 0.0589 1.000 Uiso calc C19 H H22 0.0839 0.6896 0.2570 0.0589 1.000 Uiso calc C19 H H23 -0.0137 0.6950 0.2599 0.0589 1.000 Uiso calc C19 H H24 0.1739 0.9766 0.6733 0.0430 1.000 Uiso calc C20 H H25 0.2206 1.0867 0.6386 0.0430 1.000 Uiso calc C20 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol ZN 0.0324(3) 0.0323(3) 0.0350(4) 0.0175(2) -0.0007(4) -0.0004(4) Zn O1 0.047(4) 0.058(5) 0.046(4) 0.001(4) -0.001(3) 0.005(4) O N1 0.054(3) 0.047(3) 0.045(4) 0.034(2) -0.017(3) -0.007(3) N C1 0.072(5) 0.042(4) 0.081(8) 0.038(3) -0.024(5) -0.013(5) C C2 0.095(6) 0.067(5) 0.10(1) 0.057(4) -0.037(7) -0.027(6) C C3 0.110(6) 0.100(5) 0.13(1) 0.087(3) -0.066(6) -0.071(6) C C4 0.067(4) 0.093(5) 0.073(8) 0.063(3) -0.019(5) -0.025(5) C C5 0.043(3) 0.057(4) 0.053(5) 0.035(2) -0.016(4) -0.023(4) C C6 0.037(3) 0.057(4) 0.033(5) 0.028(3) -0.009(3) -0.009(4) C N2 0.033(3) 0.041(3) 0.032(4) 0.021(2) 0.001(3) -0.001(3) N C7 0.033(4) 0.048(4) 0.030(4) 0.018(3) 0.000(3) 0.002(4) C C8 0.034(4) 0.064(5) 0.055(6) 0.021(3) 0.008(4) 0.016(5) C C9 0.034(4) 0.086(7) 0.051(6) 0.026(4) 0.012(4) 0.020(5) C C10 0.045(4) 0.094(6) 0.039(5) 0.041(3) 0.002(4) -0.002(5) C C11 0.039(4) 0.033(3) 0.046(5) 0.019(2) 0.005(4) 0.006(4) C N3 0.029(3) 0.033(3) 0.032(3) 0.018(2) -0.001(2) -0.000(3) N C12 0.028(3) 0.043(3) 0.031(4) 0.021(2) -0.001(3) -0.004(3) C C13 0.032(3) 0.033(3) 0.028(4) 0.016(2) 0.000(3) 0.000(3) C N4 0.045(3) 0.035(3) 0.028(3) 0.026(2) -0.003(3) 0.002(3) N C14 0.049(4) 0.038(3) 0.032(4) 0.027(2) -0.003(3) -0.006(3) C C15 0.042(3) 0.033(3) 0.024(4) 0.023(2) 0.004(3) 0.001(3) C N5 0.034(3) 0.034(3) 0.031(3) 0.022(2) -0.000(3) 0.001(3) N O2 0.066(3) 0.040(2) 0.036(3) 0.036(2) -0.005(3) -0.002(2) O O3 0.044(3) 0.035(2) 0.034(3) 0.024(2) -0.003(2) 0.004(2) O C16 0.053(4) 0.058(5) 0.061(7) 0.034(3) -0.013(5) -0.011(5) C C17 0.093(5) 0.050(4) 0.031(5) 0.049(3) 0.007(4) 0.002(3) C C18 0.046(4) 0.050(4) 0.042(5) 0.027(3) 0.010(4) 0.007(4) C C19 0.067(5) 0.038(4) 0.033(5) 0.027(3) -0.005(4) -0.003(3) C C20 0.034(3) 0.037(3) 0.032(4) 0.021(2) -0.004(3) -0.007(3) C C21 0.028(3) 0.031(3) 0.040(4) 0.014(2) -0.002(3) -0.002(3) C N6 0.043(3) 0.033(3) 0.049(4) 0.021(2) -0.011(3) -0.007(3) N C22 0.060(5) 0.038(5) 0.12(1) 0.021(4) -0.051(6) -0.015(6) C C23 0.054(4) 0.070(5) 0.067(6) 0.043(3) -0.040(4) -0.031(4) C N7 0.036(3) 0.038(3) 0.038(4) 0.024(2) -0.014(3) -0.012(3) N O4 0.064(4) 0.035(3) 0.074(5) 0.027(2) -0.022(4) -0.015(3) O O5 0.055(3) 0.036(2) 0.041(3) 0.027(2) -0.015(3) -0.008(2) O CL1 0.056(1) 0.043(1) 0.055(1) 0.0227(8) -0.002(1) 0.008(1) Cl CL2 0.053(1) 0.045(1) 0.038(1) 0.0122(9) -0.008(1) 0.005(1) Cl # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ZN O1 2.040(9) . . ? ZN N1 2.15(1) . . ? ZN N2 2.077(9) . . ? ZN N3 2.286(8) . . ? ZN O3 2.078(7) . . ? ZN O5 2.110(7) . . ? N1 C1 1.32(2) . . ? N1 C5 1.36(2) . . ? C1 C2 1.37(2) . . ? C2 C3 1.41(3) . . ? C3 C4 1.40(3) . . ? C4 C5 1.36(2) . . ? C5 C6 1.49(2) . . ? C6 N2 1.35(1) . . ? C6 C10 1.37(2) . . ? N2 C7 1.31(2) . . ? C7 C8 1.40(2) . . ? C7 C11 1.50(2) . . ? C8 C9 1.38(2) . . ? C9 C10 1.37(2) . . ? C11 N3 1.48(1) . . ? N3 C12 1.47(1) . . ? N3 C20 1.50(1) . . ? C12 C13 1.49(1) . . ? C13 N4 1.36(1) . . ? C13 N5 1.31(1) . . ? N4 C14 1.49(1) . . ? N4 O2 1.27(1) . . ? C14 C15 1.59(1) . . ? C14 C16 1.51(2) . . ? C14 C17 1.51(2) . . ? C15 N5 1.47(1) . . ? C15 C18 1.54(2) . . ? C15 C19 1.52(2) . . ? N5 O3 1.32(1) . . ? C20 C21 1.47(1) . . ? C21 N6 1.36(1) . . ? C21 N7 1.31(1) . . ? N6 C22 1.49(2) . . ? N6 O4 1.28(1) . . ? C22 C23 1.51(2) . . ? C22 C24 1.29(3) . . ? C22 C25 1.86(4) . . ? C22 C24A 1.78(3) . . ? C22 C25A 1.40(3) . . ? C23 N7 1.49(1) . . ? C23 C26 1.73(4) . . ? C23 C27 1.51(3) . . ? C23 C26A 1.35(3) . . ? C23 C27A 1.77(3) . . ? N7 O5 1.33(1) . . ? C24 C24A 1.48(4) . . ? C25 C25A 1.73(4) . . ? C25 C27A 1.67(4) . . ? C26 C26A 1.33(4) . . ? C27 C26A 1.38(4) . . ? C27 C27A 1.46(4) . . ? CL1 O6 1.36(1) . . ? CL1 O7 1.52(9) . . ? CL1 O8 1.50(4) . . ? CL1 O9 1.40(3) . . ? CL1 O7a 1.46(3) . . ? CL1 O8a 1.55(6) . . ? CL1 O9a 1.42(4) . . ? O7 O7a 1.40(8) . . ? O7 O9a 1.35(8) . . ? O8 O9 1.98(5) . . ? O8 O7a 1.09(4) . . ? O8 O8a 1.51(6) . . ? O9 O8a 1.26(6) . . ? O9 O9a 1.91(5) . . ? CL2 O10 1.36(2) . . ? CL2 O11 1.44(1) . . ? CL2 O12 1.38(3) . . ? CL2 O13 1.46(4) . . ? CL2 O12a 1.37(3) . . ? CL2 O13a 1.50(4) . . ? O10 O13 1.96(5) . . ? O12 O12a 1.22(4) . . ? O13 O12a 1.50(5) . . ? C28 CL3 1.89(4) . . ? C28 CL4 1.63(4) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 ZN N1 99.8(5) . . . ? O1 ZN N2 177.7(5) . . . ? O1 ZN N3 105.7(4) . . . ? O1 ZN O3 84.8(3) . . . ? O1 ZN O5 85.5(3) . . . ? N1 ZN N2 77.9(4) . . . ? N1 ZN N3 154.5(4) . . . ? N1 ZN O3 89.9(3) . . . ? N1 ZN O5 91.9(3) . . . ? N2 ZN N3 76.6(3) . . . ? N2 ZN O3 95.4(3) . . . ? N2 ZN O5 94.4(3) . . . ? N3 ZN O3 91.7(3) . . . ? N3 ZN O5 90.8(3) . . . ? O3 ZN O5 170.3(3) . . . ? C1 N1 C5 119(1) . . . ? N1 C1 C2 125(1) . . . ? C1 C2 C3 115(1) . . . ? C2 C3 C4 120(1) . . . ? C3 C4 C5 119(1) . . . ? N1 C5 C4 119(1) . . . ? N1 C5 C6 115.9(9) . . . ? C4 C5 C6 124(1) . . . ? C5 C6 N2 114(1) . . . ? C5 C6 C10 124(1) . . . ? N2 C6 C10 120(1) . . . ? C6 N2 C7 121(1) . . . ? N2 C7 C8 121(1) . . . ? N2 C7 C11 117.1(9) . . . ? C8 C7 C11 121(1) . . . ? C7 C8 C9 117(1) . . . ? C8 C9 C10 120(1) . . . ? C6 C10 C9 119(1) . . . ? C7 C11 N3 113.9(9) . . . ? C11 N3 C12 111.8(8) . . . ? C11 N3 C20 111.7(8) . . . ? C12 N3 C20 107.3(7) . . . ? N3 C12 C13 113.1(8) . . . ? C12 C13 N4 123.4(9) . . . ? C12 C13 N5 128.2(9) . . . ? N4 C13 N5 108.4(8) . . . ? C13 N4 C14 111.8(8) . . . ? C13 N4 O2 124.6(8) . . . ? C14 N4 O2 122.6(8) . . . ? N4 C14 C15 99.9(8) . . . ? N4 C14 C16 107.2(9) . . . ? N4 C14 C17 110.8(9) . . . ? C15 C14 C16 113.4(9) . . . ? C15 C14 C17 113.4(9) . . . ? C16 C14 C17 111(1) . . . ? C14 C15 N5 99.4(7) . . . ? C14 C15 C18 114.0(9) . . . ? C14 C15 C19 113.6(9) . . . ? N5 C15 C18 106.2(9) . . . ? N5 C15 C19 111.1(8) . . . ? C18 C15 C19 111.6(9) . . . ? C13 N5 C15 114.6(8) . . . ? C13 N5 O3 126.0(8) . . . ? C15 N5 O3 119.3(8) . . . ? N3 C20 C21 111.3(9) . . . ? C20 C21 N6 125(1) . . . ? C20 C21 N7 126(1) . . . ? N6 C21 N7 108.3(9) . . . ? C21 N6 C22 112.3(9) . . . ? C21 N6 O4 123.9(9) . . . ? C22 N6 O4 123(1) . . . ? N6 C22 C23 102(1) . . . ? N6 C22 C24 124(1) . . . ? N6 C22 C25 97(1) . . . ? N6 C22 C24A 98(1) . . . ? N6 C22 C25A 117(1) . . . ? C23 C22 C24 126(1) . . . ? C23 C22 C25 91(1) . . . ? C23 C22 C24A 98(1) . . . ? C23 C22 C25A 133(1) . . . ? C24 C22 C25 104(1) . . . ? C24 C22 C24A 54(1) . . . ? C24 C22 C25A 43(1) . . . ? C25 C22 C24A 158(1) . . . ? C25 C22 C25A 62(1) . . . ? C24A C22 C25A 97(1) . . . ? C22 C23 N7 102.4(9) . . . ? C22 C23 C26 97(1) . . . ? C22 C23 C27 135(1) . . . ? C22 C23 C26A 127(1) . . . ? C22 C23 C27A 93(1) . . . ? N7 C23 C26 98(1) . . . ? N7 C23 C27 109(1) . . . ? N7 C23 C26A 119(1) . . . ? N7 C23 C27A 100(1) . . . ? C26 C23 C27 106(1) . . . ? C26 C23 C26A 49(1) . . . ? C26 C23 C27A 155(1) . . . ? C27 C23 C26A 57(1) . . . ? C27 C23 C27A 52(1) . . . ? C26A C23 C27A 106(1) . . . ? C21 N7 C23 113.9(9) . . . ? C21 N7 O5 125.6(8) . . . ? C23 N7 O5 120.5(9) . . . ? C22 C24 C24A 79(2) . . . ? C22 C25 C25A 45(1) . . . ? C22 C25 C27A 85(1) . . . ? C25A C25 C27A 118(2) . . . ? C22 C24A C24 45(1) . . . ? C22 C25A C25 72(1) . . . ? C23 C26 C26A 50(1) . . . ? C23 C27 C26A 55(1) . . . ? C23 C27 C27A 73(1) . . . ? C26A C27 C27A 124(2) . . . ? C23 C26A C26 80(2) . . . ? C23 C26A C27 66(1) . . . ? C26 C26A C27 145(3) . . . ? C23 C27A C25 89(1) . . . ? C23 C27A C27 54(1) . . . ? C25 C27A C27 134(2) . . . ? O6 CL1 O7 101(3) . . . ? O6 CL1 O8 114(1) . . . ? O6 CL1 O9 119(1) . . . ? O6 CL1 O7a 107(1) . . . ? O6 CL1 O8a 90(2) . . . ? O6 CL1 O9a 118(1) . . . ? O7 CL1 O8 96(3) . . . ? O7 CL1 O9 133(3) . . . ? O7 CL1 O7a 55(3) . . . ? O7 CL1 O8a 156(3) . . . ? O7 CL1 O9a 54(3) . . . ? O8 CL1 O9 86(2) . . . ? O8 CL1 O7a 43(1) . . . ? O8 CL1 O8a 59(2) . . . ? O8 CL1 O9a 123(2) . . . ? O9 CL1 O7a 123(1) . . . ? O9 CL1 O8a 50(2) . . . ? O9 CL1 O9a 85(2) . . . ? O7a CL1 O8a 101(2) . . . ? O7a CL1 O9a 101(1) . . . ? O8a CL1 O9a 135(2) . . . ? CL1 O7 O7a 59(3) . . . ? CL1 O7 O9a 58(3) . . . ? O7a O7 O9a 108(6) . . . ? CL1 O8 O9 44(1) . . . ? CL1 O8 O7a 66(2) . . . ? CL1 O8 O8a 61(2) . . . ? O9 O8 O7a 106(3) . . . ? O9 O8 O8a 39(2) . . . ? O7a O8 O8a 126(4) . . . ? CL1 O9 O8 48(1) . . . ? CL1 O9 O8a 70(3) . . . ? CL1 O9 O9a 47(1) . . . ? O8 O9 O8a 49(2) . . . ? O8 O9 O9a 82(2) . . . ? O8a O9 O9a 118(3) . . . ? CL1 O7a O7 64(3) . . . ? CL1 O7a O8 70(2) . . . ? O7 O7a O8 130(4) . . . ? CL1 O8a O8 58(2) . . . ? CL1 O8a O9 58(3) . . . ? O8 O8a O9 90(4) . . . ? CL1 O9a O7 66(4) . . . ? CL1 O9a O9 46(1) . . . ? O7 O9a O9 109(4) . . . ? O10 CL2 O11 110(1) . . . ? O10 CL2 O12 124(1) . . . ? O10 CL2 O13 87(1) . . . ? O10 CL2 O12a 135(1) . . . ? O10 CL2 O13a 91(1) . . . ? O11 CL2 O12 106(1) . . . ? O11 CL2 O13 113(1) . . . ? O11 CL2 O12a 112(1) . . . ? O11 CL2 O13a 101(1) . . . ? O12 CL2 O13 113(2) . . . ? O12 CL2 O12a 52(1) . . . ? O12 CL2 O13a 40(1) . . . ? O13 CL2 O12a 63(1) . . . ? O13 CL2 O13a 143(2) . . . ? O12a CL2 O13a 92(1) . . . ? CL2 O10 O13 48(1) . . . ? CL2 O12 O12a 62(1) . . . ? CL2 O13 O10 44(1) . . . ? CL2 O13 O12a 55(1) . . . ? O10 O13 O12a 93(2) . . . ? CL2 O12a O12 64(1) . . . ? CL2 O12a O13 60(2) . . . ? O12 O12a O13 121(3) . . . ? CL3 C28 CL4 106(1) . . . ? data_st164 _database_code_CSD 186272 _audit_creation_date 15-05-98 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C29 H40 Cl2 Cu N8 O12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H40 Cl2 Cu N8 O12' _chemical_formula_weight 827.13 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 11.8640(4) _cell_length_b 13.2032(4) _cell_length_c 13.2661(5) _cell_angle_alpha 90.539(9) _cell_angle_beta 104.983(9) _cell_angle_gamma 113.252(9) _cell_volume 1829.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 15513 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.3 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.50 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 30 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 25 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15513 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7897 _reflns_number_gt 5601 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5601 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.082 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_all 0.094 _refine_ls_wR_factor_ref 0.078 _refine_ls_goodness_of_fit_all 1.864 _refine_ls_goodness_of_fit_ref 1.556 _refine_ls_shift/su_max 0.012 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.787 _refine_diff_density_min -0.124 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CU 0.51439(3) 0.21159(3) 0.25090(3) 0.0262(2) 1.000 Uani ? ? Cu N1 0.5908(2) 0.1517(2) 0.3738(2) 0.031(1) 1.000 Uani ? ? N C1 0.5911(3) 0.0491(3) 0.3757(3) 0.039(2) 1.000 Uani ? ? C C2 0.6472(4) 0.0177(3) 0.4671(3) 0.051(2) 1.000 Uani ? ? C C3 0.7014(4) 0.0888(3) 0.5576(3) 0.053(2) 1.000 Uani ? ? C C4 0.7028(4) 0.1950(3) 0.5574(3) 0.043(2) 1.000 Uani ? ? C C5 0.6470(3) 0.2246(3) 0.4633(2) 0.033(1) 1.000 Uani ? ? C C6 0.6402(3) 0.3329(3) 0.4505(2) 0.031(1) 1.000 Uani ? ? C C7 0.6874(3) 0.4225(3) 0.5265(3) 0.040(2) 1.000 Uani ? ? C C8 0.6685(3) 0.5170(3) 0.4996(3) 0.045(2) 1.000 Uani ? ? C C9 0.6017(3) 0.5203(3) 0.3975(3) 0.041(2) 1.000 Uani ? ? C C10 0.5544(3) 0.4274(2) 0.3242(3) 0.033(1) 1.000 Uani ? ? C N2 0.5764(2) 0.3380(2) 0.3515(2) 0.029(1) 1.000 Uani ? ? N C11 0.4697(3) 0.4122(2) 0.2132(3) 0.034(1) 1.000 Uani ? ? C N3 0.4544(2) 0.3102(2) 0.1494(2) 0.028(1) 1.000 Uani ? ? N C12 0.5341(3) 0.3412(3) 0.0738(2) 0.032(1) 1.000 Uani ? ? C C13 0.6711(3) 0.4090(2) 0.1274(2) 0.031(1) 1.000 Uani ? ? C N4 0.7336(2) 0.5177(2) 0.1200(2) 0.037(1) 1.000 Uani ? ? N C14 0.8759(3) 0.5571(3) 0.1626(3) 0.035(2) 1.000 Uani ? ? C C15 0.8864(3) 0.4600(2) 0.2268(3) 0.032(1) 1.000 Uani ? ? C N5 0.7518(2) 0.3719(2) 0.1852(2) 0.029(1) 1.000 Uani ? ? N O1 0.6807(2) 0.5787(2) 0.0727(2) 0.054(1) 1.000 Uani ? ? O O2 0.7186(2) 0.2722(2) 0.2120(2) 0.033(1) 1.000 Uani ? ? O C16 0.9257(4) 0.5668(4) 0.0664(3) 0.060(2) 1.000 Uani ? ? C C17 0.9314(5) 0.6697(3) 0.2263(4) 0.056(2) 1.000 Uani ? ? C C18 0.9775(3) 0.4138(3) 0.2044(4) 0.052(2) 1.000 Uani ? ? C C19 0.9109(4) 0.4834(3) 0.3446(3) 0.041(2) 1.000 Uani ? ? C C20 0.3184(3) 0.2485(2) 0.0880(3) 0.032(1) 1.000 Uani ? ? C C21 0.2885(3) 0.1335(3) 0.0417(3) 0.031(1) 1.000 Uani ? ? C N6 0.1836(3) 0.0814(2) -0.0416(2) 0.037(1) 1.000 Uani ? ? N C22 0.1752(4) -0.0309(3) -0.0789(3) 0.044(2) 1.000 Uani ? ? C C23 0.2594(3) -0.0528(3) 0.0197(3) 0.035(2) 1.000 Uani ? ? C N7 0.3425(2) 0.0653(2) 0.0722(2) 0.028(1) 1.000 Uani ? ? N O3 0.1087(2) 0.1236(2) -0.0873(2) 0.051(1) 1.000 Uani ? ? O O4 0.4467(2) 0.0839(2) 0.1484(2) 0.032(1) 1.000 Uani ? ? O C24 0.2306(5) -0.0127(4) -0.1740(4) 0.068(3) 1.000 Uani ? ? C C25 0.0348(4) -0.1139(4) -0.1120(4) 0.059(3) 1.000 Uani ? ? C C26 0.3424(3) -0.1105(3) -0.0006(3) 0.049(2) 1.000 Uani ? ? C C27 0.1894(3) -0.1099(3) 0.0977(3) 0.044(2) 1.000 Uani ? ? C CL1 0.25270(7) 0.17613(6) 0.35278(6) 0.0337(3) 1.000 Uani ? ? Cl O5 0.2239(2) 0.2622(2) 0.3015(2) 0.041(1) 1.000 Uani ? ? O O6 0.3043(2) 0.1274(2) 0.2870(2) 0.042(1) 1.000 Uani ? ? O O7 0.3458(3) 0.2222(2) 0.4533(2) 0.045(1) 1.000 Uani ? ? O O8 0.1394(2) 0.0899(2) 0.3656(2) 0.049(1) 1.000 Uani ? ? O CL2 0.6341(1) 0.32399(8) -0.19641(8) 0.0607(5) 1.000 Uani ? ? Cl O9 0.6145(5) 0.4008(3) -0.2587(4) 0.168(3) 0.900 Uani ? ? O O10 0.7578(4) 0.3354(4) -0.2116(4) 0.124(3) 1.000 Uani ? ? O O11 0.5594(5) 0.2107(3) -0.2354(4) 0.096(3) 0.900 Uani ? ? O O12 0.6646(5) 0.3488(4) -0.0893(3) 0.112(3) 1.000 Uani ? ? O O13 0.498(2) 0.313(1) -0.188(1) 0.09(1) 0.200 Uani ? ? O N8 -0.0008(5) 0.2558(4) -0.5276(5) 0.127(3) 1.000 Uani ? ? N C28 0.0470(6) 0.2060(4) -0.4733(4) 0.156(3) 1.000 Uani ? ? C C29 0.1013(7) 0.1484(5) -0.4097(5) 0.159(4) 1.000 Uani ? ? C H1 0.5521 -0.0018 0.3131 0.0500 1.000 Uiso calc C1 H H2 0.6479 -0.0540 0.4668 0.0633 1.000 Uiso calc C2 H H3 0.7383 0.0664 0.6210 0.0681 1.000 Uiso calc C3 H H4 0.7410 0.2459 0.6200 0.0615 1.000 Uiso calc C4 H H5 0.7322 0.4197 0.5962 0.0561 1.000 Uiso calc C7 H H6 0.7014 0.5799 0.5510 0.0611 1.000 Uiso calc C8 H H7 0.5887 0.5849 0.3785 0.0547 1.000 Uiso calc C9 H H8 0.5070 0.4755 0.1801 0.0436 1.000 Uiso calc C11 H H9 0.3878 0.4051 0.2159 0.0436 1.000 Uiso calc C11 H H10 0.5030 0.3825 0.0245 0.0409 1.000 Uiso calc C12 H H11 0.5263 0.2751 0.0379 0.0409 1.000 Uiso calc C12 H H12 1.0161 0.5916 0.0885 0.0783 1.000 Uiso calc C16 H H13 0.8882 0.4963 0.0251 0.0783 1.000 Uiso calc C16 H H14 0.9036 0.6185 0.0256 0.0783 1.000 Uiso calc C16 H H15 1.0216 0.6945 0.2532 0.0855 1.000 Uiso calc C17 H H16 0.9126 0.7210 0.1828 0.0855 1.000 Uiso calc C17 H H17 0.8951 0.6646 0.2830 0.0855 1.000 Uiso calc C17 H H18 1.0630 0.4682 0.2300 0.0675 1.000 Uiso calc C18 H H19 0.9690 0.3493 0.2385 0.0675 1.000 Uiso calc C18 H H20 0.9575 0.3950 0.1307 0.0675 1.000 Uiso calc C18 H H21 0.9952 0.5388 0.3743 0.0597 1.000 Uiso calc C19 H H22 0.8508 0.5089 0.3575 0.0597 1.000 Uiso calc C19 H H23 0.9023 0.4173 0.3758 0.0597 1.000 Uiso calc C19 H H24 0.2988 0.2891 0.0323 0.0427 1.000 Uiso calc C20 H H25 0.2663 0.2430 0.1332 0.0427 1.000 Uiso calc C20 H H26 0.2277 -0.0809 -0.2010 0.0969 1.000 Uiso calc C24 H H27 0.1813 0.0129 -0.2273 0.0969 1.000 Uiso calc C24 H H28 0.3168 0.0410 -0.1523 0.0969 1.000 Uiso calc C24 H H29 0.0289 -0.1846 -0.1355 0.0932 1.000 Uiso calc C25 H H30 0.0010 -0.1199 -0.0537 0.0932 1.000 Uiso calc C25 H H31 -0.0125 -0.0890 -0.1675 0.0932 1.000 Uiso calc C25 H H32 0.2890 -0.1843 -0.0335 0.0661 1.000 Uiso calc C26 H H33 0.3910 -0.0707 -0.0453 0.0661 1.000 Uiso calc C26 H H34 0.3987 -0.1122 0.0643 0.0661 1.000 Uiso calc C26 H H35 0.1350 -0.1850 0.0696 0.0602 1.000 Uiso calc C27 H H36 0.2497 -0.1077 0.1617 0.0602 1.000 Uiso calc C27 H H37 0.1394 -0.0727 0.1109 0.0602 1.000 Uiso calc C27 H H38 0.1551 0.1298 -0.4413 0.1936 1.000 Uiso calc C29 H H39 0.1508 0.1927 -0.3439 0.1936 1.000 Uiso calc C29 H H40 0.0363 0.0824 -0.3991 0.1936 1.000 Uiso calc C29 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol CU 0.0352(2) 0.0231(1) 0.0222(2) 0.0119(1) 0.0068(1) 0.0033(1) Cu N1 0.033(1) 0.030(1) 0.030(1) 0.0114(8) 0.011(1) 0.007(1) N C1 0.045(2) 0.033(1) 0.040(2) 0.018(1) 0.014(1) 0.009(1) C C2 0.057(2) 0.046(2) 0.051(2) 0.029(1) 0.017(2) 0.025(1) C C3 0.056(2) 0.059(2) 0.045(2) 0.029(1) 0.011(2) 0.024(2) C C4 0.042(2) 0.059(2) 0.031(2) 0.013(1) 0.007(1) 0.005(2) C C5 0.035(1) 0.035(1) 0.028(1) 0.013(1) 0.013(1) 0.009(1) C C6 0.035(1) 0.032(1) 0.026(1) 0.009(1) 0.012(1) 0.001(1) C C7 0.042(2) 0.046(2) 0.033(2) 0.010(1) 0.011(1) -0.008(1) C C8 0.048(2) 0.037(2) 0.052(2) 0.013(1) 0.014(1) -0.013(1) C C9 0.044(2) 0.028(1) 0.054(2) 0.013(1) 0.018(1) -0.001(1) C C10 0.033(1) 0.026(1) 0.040(2) 0.0108(9) 0.018(1) 0.007(1) C N2 0.032(1) 0.027(1) 0.029(1) 0.0092(8) 0.0122(9) 0.005(1) N C11 0.039(1) 0.024(1) 0.043(2) 0.0148(9) 0.017(1) 0.007(1) C N3 0.029(1) 0.025(1) 0.030(1) 0.0088(8) 0.0121(9) 0.005(1) N C12 0.034(1) 0.033(1) 0.029(1) 0.013(1) 0.013(1) 0.012(1) C C13 0.035(1) 0.030(1) 0.029(1) 0.013(1) 0.013(1) 0.009(1) C N4 0.033(1) 0.037(1) 0.041(1) 0.0131(9) 0.016(1) 0.014(1) N C14 0.032(1) 0.031(1) 0.044(2) 0.007(1) 0.011(1) 0.006(1) C C15 0.030(1) 0.030(1) 0.037(2) 0.010(1) 0.010(1) 0.005(1) C N5 0.031(1) 0.028(1) 0.027(1) 0.0101(8) 0.0096(9) 0.005(1) N O1 0.048(1) 0.041(1) 0.081(2) 0.0220(8) 0.021(1) 0.035(1) O O2 0.039(1) 0.0251(9) 0.037(1) 0.0123(7) 0.0130(9) 0.0071(9) O C16 0.044(2) 0.081(2) 0.061(2) 0.022(2) 0.029(2) 0.033(2) C C17 0.072(3) 0.035(2) 0.070(3) 0.015(2) -0.001(2) 0.002(2) C C18 0.039(2) 0.048(2) 0.075(2) 0.018(1) 0.026(2) 0.010(2) C C19 0.046(2) 0.042(2) 0.037(2) 0.009(1) 0.005(2) -0.002(2) C C20 0.030(1) 0.031(1) 0.037(2) 0.011(1) 0.010(1) 0.009(1) C C21 0.029(1) 0.037(1) 0.029(1) 0.010(1) 0.010(1) 0.006(1) C N6 0.030(1) 0.045(1) 0.036(1) 0.009(1) 0.002(1) 0.002(1) N C22 0.040(2) 0.049(2) 0.043(2) 0.014(1) -0.000(2) -0.009(2) C C23 0.030(1) 0.030(1) 0.046(2) 0.007(1) 0.008(1) -0.010(1) C N7 0.029(1) 0.030(1) 0.026(1) 0.0084(8) 0.0086(9) 0.001(1) N O3 0.039(1) 0.055(1) 0.061(2) 0.0187(9) -0.006(1) 0.012(1) O O4 0.0335(9) 0.0317(9) 0.032(1) 0.0164(6) 0.0003(9) -0.0014(9) O C24 0.082(3) 0.098(3) 0.040(2) 0.040(2) 0.006(2) -0.009(2) C C25 0.045(2) 0.053(2) 0.087(3) 0.012(2) -0.018(2) -0.014(2) C C26 0.042(2) 0.048(2) 0.057(2) 0.016(1) 0.010(2) -0.018(2) C C27 0.043(2) 0.033(2) 0.062(2) 0.011(1) 0.019(2) 0.010(2) C CL1 0.0380(3) 0.0311(3) 0.0322(4) 0.0118(2) 0.0129(3) 0.0066(3) Cl O5 0.052(1) 0.034(1) 0.039(1) 0.0224(7) 0.012(1) 0.0080(9) O O6 0.047(1) 0.036(1) 0.045(1) 0.0199(7) 0.0207(9) 0.0079(9) O O7 0.054(1) 0.058(1) 0.029(1) 0.017(1) 0.001(1) 0.002(1) O O8 0.048(1) 0.042(1) 0.060(1) 0.006(1) 0.028(1) 0.010(1) O CL2 0.0906(6) 0.0555(5) 0.0445(5) 0.0351(4) 0.0161(5) 0.0078(4) Cl O9 0.260(3) 0.145(2) 0.127(3) 0.161(2) 0.102(3) 0.074(2) O O10 0.120(2) 0.144(3) 0.110(3) 0.083(2) 0.018(2) 0.007(3) O O11 0.143(4) 0.057(2) 0.110(4) 0.006(3) -0.007(3) -0.019(3) O O12 0.209(4) 0.110(3) 0.061(2) 0.001(3) 0.080(2) -0.016(2) O O13 0.11(1) 0.10(1) 0.07(1) 0.053(7) 0.034(8) 0.023(9) O N8 0.141(3) 0.108(3) 0.134(4) 0.046(2) 0.077(3) 0.005(3) N C28 0.283(3) 0.094(2) 0.142(3) 0.134(2) 0.161(2) 0.079(2) C C29 0.256(4) 0.096(3) 0.163(4) 0.077(3) 0.164(3) 0.030(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU N1 1.983(3) . . ? CU N2 1.895(3) . . ? CU O4 1.914(2) . . ? N1 C1 1.357(4) . . ? N1 C5 1.357(5) . . ? C1 C2 1.376(5) . . ? C2 C3 1.356(6) . . ? C3 C4 1.396(7) . . ? C4 C5 1.392(5) . . ? C5 C6 1.471(5) . . ? C6 C7 1.376(5) . . ? C6 N2 1.353(5) . . ? C7 C8 1.387(6) . . ? C8 C9 1.392(6) . . ? C9 C10 1.384(5) . . ? C10 N2 1.340(4) . . ? C10 C11 1.513(5) . . ? C11 N3 1.507(4) . . ? N3 C12 1.503(4) . . ? N3 C20 1.484(4) . . ? C12 C13 1.480(5) . . ? C13 N4 1.349(4) . . ? C13 N5 1.320(4) . . ? N4 C14 1.500(5) . . ? N4 O1 1.281(4) . . ? C14 C15 1.573(5) . . ? C14 C16 1.525(6) . . ? C14 C17 1.508(6) . . ? C15 N5 1.507(4) . . ? C15 C18 1.521(5) . . ? C15 C19 1.520(5) . . ? N5 O2 1.298(3) . . ? C20 C21 1.501(5) . . ? C21 N6 1.358(5) . . ? C21 N7 1.309(4) . . ? N6 C22 1.515(5) . . ? N6 O3 1.260(4) . . ? C22 C23 1.534(6) . . ? C22 C24 1.547(7) . . ? C22 C25 1.529(6) . . ? C23 N7 1.517(4) . . ? C23 C26 1.533(5) . . ? C23 C27 1.515(6) . . ? N7 O4 1.311(4) . . ? CL1 O5 1.439(3) . . ? CL1 O6 1.458(3) . . ? CL1 O7 1.436(3) . . ? CL1 O8 1.430(3) . . ? CL2 O9 1.367(5) . . ? CL2 O10 1.482(5) . . ? CL2 O11 1.412(4) . . ? CL2 O12 1.375(4) . . ? CL2 O13 1.60(2) . . ? O9 O13 1.89(2) . . ? O11 O13 1.94(2) . . ? O12 O13 1.94(2) . . ? N8 C28 1.17(1) . . ? C28 C29 1.35(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 CU N2 82.1(1) . . . ? N1 CU O4 98.9(1) . . . ? N2 CU O4 178.3(1) . . . ? CU N1 C1 126.9(3) . . . ? CU N1 C5 113.6(2) . . . ? C1 N1 C5 119.5(3) . . . ? N1 C1 C2 121.0(4) . . . ? C1 C2 C3 120.2(4) . . . ? C2 C3 C4 119.8(4) . . . ? C3 C4 C5 118.5(4) . . . ? N1 C5 C4 121.0(3) . . . ? N1 C5 C6 114.1(3) . . . ? C4 C5 C6 124.9(4) . . . ? C5 C6 C7 127.5(4) . . . ? C5 C6 N2 112.6(3) . . . ? C7 C6 N2 119.9(3) . . . ? C6 C7 C8 118.9(4) . . . ? C7 C8 C9 120.3(4) . . . ? C8 C9 C10 118.7(4) . . . ? C9 C10 N2 119.9(4) . . . ? C9 C10 C11 125.9(3) . . . ? N2 C10 C11 114.1(3) . . . ? CU N2 C6 117.6(2) . . . ? CU N2 C10 120.1(3) . . . ? C6 N2 C10 122.3(3) . . . ? C10 C11 N3 111.7(3) . . . ? C11 N3 C12 110.9(3) . . . ? C11 N3 C20 109.7(3) . . . ? C12 N3 C20 108.4(3) . . . ? N3 C12 C13 112.4(3) . . . ? C12 C13 N4 124.6(3) . . . ? C12 C13 N5 125.6(3) . . . ? N4 C13 N5 109.7(3) . . . ? C13 N4 C14 112.1(3) . . . ? C13 N4 O1 124.8(3) . . . ? C14 N4 O1 122.8(3) . . . ? N4 C14 C15 101.4(3) . . . ? N4 C14 C16 105.5(3) . . . ? N4 C14 C17 109.6(4) . . . ? C15 C14 C16 114.4(3) . . . ? C15 C14 C17 115.4(3) . . . ? C16 C14 C17 109.7(4) . . . ? C14 C15 N5 100.8(3) . . . ? C14 C15 C18 115.1(3) . . . ? C14 C15 C19 114.9(3) . . . ? N5 C15 C18 108.2(3) . . . ? N5 C15 C19 106.6(3) . . . ? C18 C15 C19 110.4(3) . . . ? C13 N5 C15 113.4(3) . . . ? C13 N5 O2 124.2(3) . . . ? C15 N5 O2 122.2(3) . . . ? N3 C20 C21 113.2(3) . . . ? C20 C21 N6 119.5(3) . . . ? C20 C21 N7 131.0(3) . . . ? N6 C21 N7 109.3(3) . . . ? C21 N6 C22 110.8(3) . . . ? C21 N6 O3 124.9(4) . . . ? C22 N6 O3 124.1(3) . . . ? N6 C22 C23 100.7(3) . . . ? N6 C22 C24 105.6(4) . . . ? N6 C22 C25 109.1(4) . . . ? C23 C22 C24 114.5(4) . . . ? C23 C22 C25 115.0(4) . . . ? C24 C22 C25 110.8(4) . . . ? C22 C23 N7 100.2(3) . . . ? C22 C23 C26 115.4(4) . . . ? C22 C23 C27 114.7(3) . . . ? N7 C23 C26 110.5(3) . . . ? N7 C23 C27 105.0(3) . . . ? C26 C23 C27 110.1(4) . . . ? C21 N7 C23 112.3(3) . . . ? C21 N7 O4 128.5(3) . . . ? C23 N7 O4 118.6(3) . . . ? CU O4 N7 119.0(2) . . . ? O5 CL1 O6 108.7(2) . . . ? O5 CL1 O7 110.0(2) . . . ? O5 CL1 O8 110.8(2) . . . ? O6 CL1 O7 109.4(2) . . . ? O6 CL1 O8 108.0(2) . . . ? O7 CL1 O8 110.0(2) . . . ? O9 CL2 O10 98.3(4) . . . ? O9 CL2 O11 117.5(4) . . . ? O9 CL2 O12 118.2(4) . . . ? O9 CL2 O13 78.5(8) . . . ? O10 CL2 O11 99.7(4) . . . ? O10 CL2 O12 102.5(4) . . . ? O10 CL2 O13 176.1(7) . . . ? O11 CL2 O12 115.1(3) . . . ? O11 CL2 O13 79.9(8) . . . ? O12 CL2 O13 81.2(8) . . . ? CL2 O9 O13 56.2(7) . . . ? CL2 O11 O13 54.3(7) . . . ? CL2 O12 O13 54.5(6) . . . ? CL2 O13 O9 45.2(6) . . . ? CL2 O13 O11 45.8(6) . . . ? CL2 O13 O12 44.4(6) . . . ? O9 O13 O11 76.8(8) . . . ? O9 O13 O12 75.8(9) . . . ? O11 O13 O12 74.6(8) . . . ? N8 C28 C29 179.2(8) . . . ?