Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_LCu(1) _database_code_depnum_ccdc_archive 'CCDC 253143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H19 N5 Cu +, (ClO4) -' _chemical_formula_sum 'C19 H19 Cl Cu N5 O4' _chemical_formula_weight 480.38 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' Cu Cu 0.3201 1.2651 '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 10.823(5) _cell_length_b 10.882(5) _cell_length_c 11.290(5) _cell_angle_alpha 117.244(5) _cell_angle_beta 90.425(5) _cell_angle_gamma 115.172(5) _cell_volume 1035.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6951 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4924 _reflns_number_gt 4474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, 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^)+(0.0558P)^2^+0.2643P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4924 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 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 Cu Cu 0.65810(2) 0.44048(2) 0.54682(2) 0.01809(8) Uani 1 1 d . . . Cl Cl 1.03946(4) 0.16185(5) 0.86248(4) 0.01747(10) Uani 1 1 d . . . O3 O 1.05953(15) 0.20050(16) 1.00364(13) 0.0263(3) Uani 1 1 d . . . O4 O 0.90157(14) 0.13523(17) 0.81357(13) 0.0255(3) Uani 1 1 d . . . O2 O 1.05067(16) 0.02197(17) 0.77921(15) 0.0335(3) Uani 1 1 d . . . N3 N 0.86664(14) 0.35806(16) 0.66242(14) 0.0151(3) Uani 1 1 d . . . O1 O 1.14480(15) 0.29104(17) 0.85213(15) 0.0328(3) Uani 1 1 d . . . C10 C 0.68212(17) 0.3057(2) 0.78570(16) 0.0163(3) Uani 1 1 d . . . N1 N 0.71470(15) 0.38971(16) 0.36187(14) 0.0159(3) Uani 1 1 d . . . N2 N 0.80307(14) 0.37238(16) 0.56987(13) 0.0151(3) Uani 1 1 d . . . C4 C 0.85093(18) 0.2844(2) 0.22226(17) 0.0192(3) Uani 1 1 d . . . C8 C 0.95862(18) 0.30492(19) 0.61415(18) 0.0174(3) Uani 1 1 d . . . C9 C 0.83514(18) 0.4037(2) 0.79706(17) 0.0173(3) Uani 1 1 d . . . C1 C 0.66597(18) 0.4003(2) 0.25870(18) 0.0198(3) Uani 1 1 d . . . C11 C 0.6202(2) 0.1428(2) 0.7206(2) 0.0236(4) Uani 1 1 d . . . C5 C 0.80679(17) 0.33284(18) 0.34347(16) 0.0151(3) Uani 1 1 d . . . C14 C 0.4602(2) 0.2885(3) 0.83472(19) 0.0266(4) Uani 1 1 d . . . N5 N 0.70100(16) 0.64846(18) 0.69541(15) 0.0216(3) Uani 1 1 d . . . C7 C 0.95447(18) 0.2822(2) 0.48340(18) 0.0184(3) Uani 1 1 d . . . C15 C 0.60087(19) 0.3784(2) 0.84252(17) 0.0204(3) Uani 1 1 d . . . C19 C 0.7191(2) 0.8923(2) 0.9144(2) 0.0269(4) Uani 1 1 d . . . N4 N 0.46069(16) 0.29258(18) 0.51955(15) 0.0199(3) Uani 1 1 d . . . C2 C 0.7056(2) 0.3553(2) 0.13559(18) 0.0225(4) Uani 1 1 d . . . C18 C 0.71114(19) 0.7568(2) 0.79156(18) 0.0206(3) Uani 1 1 d . . . C6 C 0.85646(17) 0.32646(18) 0.46035(16) 0.0148(3) Uani 1 1 d . . . C17 C 0.2042(2) 0.1291(2) 0.5227(2) 0.0244(4) Uani 1 1 d . . . C3 C 0.7997(2) 0.2964(2) 0.11747(18) 0.0221(4) Uani 1 1 d . . . C13 C 0.3997(2) 0.1259(3) 0.7694(2) 0.0290(4) Uani 1 1 d . . . C16 C 0.34780(19) 0.2196(2) 0.51967(16) 0.0186(3) Uani 1 1 d . . . C12 C 0.4793(2) 0.0527(3) 0.7114(2) 0.0300(4) Uani 1 1 d . . . H7 H 1.006(2) 0.245(3) 0.424(2) 0.027(6) Uiso 1 1 d . . . H2 H 0.670(2) 0.368(2) 0.068(2) 0.023(5) Uiso 1 1 d . . . H1 H 0.606(2) 0.442(2) 0.274(2) 0.021(5) Uiso 1 1 d . . . H9B H 0.895(2) 0.391(2) 0.847(2) 0.018(5) Uiso 1 1 d . . . H8 H 1.004(2) 0.290(2) 0.664(2) 0.017(5) Uiso 1 1 d . . . H9A H 0.862(2) 0.513(2) 0.841(2) 0.015(5) Uiso 1 1 d . . . H15 H 0.644(2) 0.488(3) 0.885(2) 0.020(5) Uiso 1 1 d . . . H17B H 0.189(3) 0.184(3) 0.607(3) 0.033(6) Uiso 1 1 d . . . H3 H 0.827(3) 0.263(3) 0.036(2) 0.032(6) Uiso 1 1 d . . . H4 H 0.916(2) 0.246(2) 0.216(2) 0.021(5) Uiso 1 1 d . . . H17C H 0.136(3) 0.101(3) 0.449(3) 0.040(7) Uiso 1 1 d . . . H11 H 0.673(3) 0.098(3) 0.680(2) 0.035(6) Uiso 1 1 d . . . H13 H 0.308(3) 0.067(3) 0.764(2) 0.034(6) Uiso 1 1 d . . . H12 H 0.441(3) -0.052(3) 0.668(3) 0.036(6) Uiso 1 1 d . . . H17A H 0.192(3) 0.034(3) 0.508(3) 0.047(8) Uiso 1 1 d . . . H19C H 0.687(3) 0.942(3) 0.889(3) 0.044(7) Uiso 1 1 d . . . H19A H 0.815(3) 0.959(3) 0.975(2) 0.032(6) Uiso 1 1 d . . . H14 H 0.410(3) 0.339(3) 0.873(2) 0.033(6) Uiso 1 1 d . . . H19B H 0.660(3) 0.861(3) 0.959(3) 0.051(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.01830(12) 0.02135(13) 0.01659(12) 0.00892(9) 0.00687(8) 0.01193(9) Cl 0.01749(19) 0.0192(2) 0.01497(19) 0.00667(15) 0.00418(14) 0.01046(16) O3 0.0342(7) 0.0296(7) 0.0165(6) 0.0110(6) 0.0044(5) 0.0175(6) O4 0.0198(6) 0.0373(8) 0.0250(7) 0.0172(6) 0.0062(5) 0.0167(6) O2 0.0374(8) 0.0290(7) 0.0280(7) 0.0028(6) 0.0056(6) 0.0240(7) N3 0.0142(6) 0.0158(6) 0.0148(6) 0.0080(5) 0.0031(5) 0.0066(5) O1 0.0246(7) 0.0347(8) 0.0343(8) 0.0217(7) 0.0050(6) 0.0058(6) C10 0.0161(8) 0.0212(8) 0.0122(7) 0.0094(6) 0.0031(6) 0.0084(7) N1 0.0146(6) 0.0159(6) 0.0149(6) 0.0074(5) 0.0033(5) 0.0059(5) N2 0.0148(6) 0.0165(6) 0.0138(6) 0.0080(5) 0.0030(5) 0.0071(5) C4 0.0201(8) 0.0175(8) 0.0179(8) 0.0080(7) 0.0082(6) 0.0086(7) C8 0.0168(8) 0.0157(8) 0.0211(8) 0.0096(7) 0.0038(6) 0.0087(6) C9 0.0177(8) 0.0184(8) 0.0126(7) 0.0075(6) 0.0038(6) 0.0067(7) C1 0.0186(8) 0.0220(8) 0.0192(8) 0.0111(7) 0.0049(6) 0.0095(7) C11 0.0209(9) 0.0229(9) 0.0286(9) 0.0124(8) 0.0099(7) 0.0125(7) C5 0.0143(7) 0.0118(7) 0.0145(7) 0.0053(6) 0.0035(6) 0.0040(6) C14 0.0251(9) 0.0463(12) 0.0194(9) 0.0181(9) 0.0106(7) 0.0244(9) N5 0.0236(8) 0.0231(8) 0.0211(7) 0.0119(6) 0.0052(6) 0.0128(6) C7 0.0193(8) 0.0164(8) 0.0207(8) 0.0088(7) 0.0073(6) 0.0103(7) C15 0.0248(9) 0.0249(9) 0.0140(8) 0.0091(7) 0.0050(6) 0.0149(8) C19 0.0313(11) 0.0212(9) 0.0248(9) 0.0085(8) 0.0100(8) 0.0134(8) N4 0.0204(7) 0.0237(7) 0.0184(7) 0.0113(6) 0.0063(6) 0.0121(6) C2 0.0237(9) 0.0259(9) 0.0167(8) 0.0122(7) 0.0037(7) 0.0094(7) C18 0.0214(8) 0.0207(8) 0.0214(8) 0.0121(7) 0.0056(7) 0.0100(7) C6 0.0144(7) 0.0123(7) 0.0143(7) 0.0060(6) 0.0043(6) 0.0046(6) C17 0.0183(9) 0.0271(10) 0.0225(9) 0.0101(8) 0.0051(7) 0.0094(8) C3 0.0250(9) 0.0224(9) 0.0152(8) 0.0089(7) 0.0084(7) 0.0090(7) C13 0.0149(9) 0.0437(12) 0.0277(10) 0.0218(9) 0.0074(7) 0.0096(8) C16 0.0220(9) 0.0216(8) 0.0137(7) 0.0076(7) 0.0037(6) 0.0131(7) C12 0.0224(10) 0.0253(10) 0.0359(11) 0.0152(9) 0.0071(8) 0.0067(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 Cu N5 1.9418(17) . ? Cu N4 1.9651(17) . ? Cu N2 2.0588(15) . ? Cu N1 2.0716(16) . ? Cl O2 1.4367(14) . ? Cl O3 1.4379(15) . ? Cl O1 1.4419(15) . ? Cl O4 1.4456(14) . ? N3 N2 1.3486(19) . ? N3 C8 1.353(2) . ? N3 C9 1.461(2) . ? C10 C11 1.386(3) . ? C10 C15 1.395(2) . ? C10 C9 1.505(2) . ? N1 C1 1.347(2) . ? N1 C5 1.353(2) . ? N2 C6 1.343(2) . ? C4 C3 1.385(3) . ? C4 C5 1.394(2) . ? C8 C7 1.378(2) . ? C1 C2 1.386(2) . ? C11 C12 1.388(3) . ? C5 C6 1.463(2) . ? C14 C13 1.384(3) . ? C14 C15 1.391(3) . ? N5 C18 1.139(2) . ? C7 C6 1.403(2) . ? C19 C18 1.457(3) . ? N4 C16 1.140(2) . ? C2 C3 1.388(3) . ? C17 C16 1.455(3) . ? C13 C12 1.386(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu N4 108.23(7) . . ? N5 Cu N2 113.55(6) . . ? N4 Cu N2 115.54(7) . . ? N5 Cu N1 125.96(6) . . ? N4 Cu N1 111.74(6) . . ? N2 Cu N1 79.60(6) . . ? O2 Cl O3 109.86(9) . . ? O2 Cl O1 109.59(10) . . ? O3 Cl O1 109.66(9) . . ? O2 Cl O4 109.46(9) . . ? O3 Cl O4 109.57(8) . . ? O1 Cl O4 108.69(9) . . ? N2 N3 C8 111.66(14) . . ? N2 N3 C9 119.63(13) . . ? C8 N3 C9 128.67(14) . . ? C11 C10 C15 118.95(16) . . ? C11 C10 C9 120.86(15) . . ? C15 C10 C9 120.18(16) . . ? C1 N1 C5 117.95(14) . . ? C1 N1 Cu 127.65(12) . . ? C5 N1 Cu 114.32(11) . . ? C6 N2 N3 105.35(13) . . ? C6 N2 Cu 113.99(11) . . ? N3 N2 Cu 140.66(11) . . ? C3 C4 C5 118.79(16) . . ? N3 C8 C7 107.29(15) . . ? N3 C9 C10 112.03(13) . . ? N1 C1 C2 122.97(17) . . ? C10 C11 C12 120.79(17) . . ? N1 C5 C4 122.35(15) . . ? N1 C5 C6 114.92(14) . . ? C4 C5 C6 122.73(15) . . ? C13 C14 C15 120.02(17) . . ? C18 N5 Cu 168.46(15) . . ? C8 C7 C6 104.83(14) . . ? C14 C15 C10 120.37(18) . . ? C16 N4 Cu 171.73(14) . . ? C1 C2 C3 118.63(16) . . ? N5 C18 C19 178.0(2) . . ? N2 C6 C7 110.87(14) . . ? N2 C6 C5 117.05(14) . . ? C7 C6 C5 132.08(15) . . ? C4 C3 C2 119.30(16) . . ? C14 C13 C12 119.92(18) . . ? N4 C16 C17 178.80(19) . . ? C13 C12 C11 119.93(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Cu N1 C1 -68.52(17) . . . . ? N4 Cu N1 C1 66.35(16) . . . . ? N2 Cu N1 C1 179.84(15) . . . . ? N5 Cu N1 C5 114.70(12) . . . . ? N4 Cu N1 C5 -110.43(12) . . . . ? N2 Cu N1 C5 3.07(11) . . . . ? C8 N3 N2 C6 0.18(18) . . . . ? C9 N3 N2 C6 178.14(13) . . . . ? C8 N3 N2 Cu -179.38(13) . . . . ? C9 N3 N2 Cu -1.4(2) . . . . ? N5 Cu N2 C6 -126.83(12) . . . . ? N4 Cu N2 C6 107.26(12) . . . . ? N1 Cu N2 C6 -1.99(11) . . . . ? N5 Cu N2 N3 52.70(18) . . . . ? N4 Cu N2 N3 -73.21(18) . . . . ? N1 Cu N2 N3 177.55(18) . . . . ? N2 N3 C8 C7 -0.43(19) . . . . ? C9 N3 C8 C7 -178.16(15) . . . . ? N2 N3 C9 C10 62.03(19) . . . . ? C8 N3 C9 C10 -120.40(18) . . . . ? C11 C10 C9 N3 57.4(2) . . . . ? C15 C10 C9 N3 -123.41(16) . . . . ? C5 N1 C1 C2 0.2(3) . . . . ? Cu N1 C1 C2 -176.48(13) . . . . ? C15 C10 C11 C12 0.2(3) . . . . ? C9 C10 C11 C12 179.39(17) . . . . ? C1 N1 C5 C4 -0.6(2) . . . . ? Cu N1 C5 C4 176.55(12) . . . . ? C1 N1 C5 C6 179.32(14) . . . . ? Cu N1 C5 C6 -3.57(17) . . . . ? C3 C4 C5 N1 0.6(2) . . . . ? C3 C4 C5 C6 -179.24(16) . . . . ? N4 Cu N5 C18 34.6(8) . . . . ? N2 Cu N5 C18 -95.1(8) . . . . ? N1 Cu N5 C18 170.7(7) . . . . ? N3 C8 C7 C6 0.49(18) . . . . ? C13 C14 C15 C10 -0.5(3) . . . . ? C11 C10 C15 C14 0.5(2) . . . . ? C9 C10 C15 C14 -178.68(15) . . . . ? N5 Cu N4 C16 -22.3(10) . . . . ? N2 Cu N4 C16 106.3(10) . . . . ? N1 Cu N4 C16 -165.2(10) . . . . ? N1 C1 C2 C3 0.1(3) . . . . ? Cu N5 C18 C19 -35(6) . . . . ? N3 N2 C6 C7 0.15(18) . . . . ? Cu N2 C6 C7 179.84(11) . . . . ? N3 N2 C6 C5 -178.99(13) . . . . ? Cu N2 C6 C5 0.71(18) . . . . ? C8 C7 C6 N2 -0.40(19) . . . . ? C8 C7 C6 C5 178.56(17) . . . . ? N1 C5 C6 N2 1.9(2) . . . . ? C4 C5 C6 N2 -178.19(15) . . . . ? N1 C5 C6 C7 -176.97(17) . . . . ? C4 C5 C6 C7 2.9(3) . . . . ? C5 C4 C3 C2 -0.3(3) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C15 C14 C13 C12 -0.2(3) . . . . ? Cu N4 C16 C17 4(10) . . . . ? C14 C13 C12 C11 0.9(3) . . . . ? C10 C11 C12 C13 -0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.452 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.073 data_PYPZCuOAc _database_code_depnum_ccdc_archive 'CCDC 253144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Cu2 N6 O4' _chemical_formula_sum 'C20 H18 Cu2 N6 O4' _chemical_formula_weight 533.48 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M ' Pcab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 17.217(5) _cell_length_b 6.420(5) _cell_length_c 17.644(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 1950.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Dark Blue' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 2.225 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11553 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.80 _reflns_number_total 2358 _reflns_number_gt 2101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, 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^)+(0.0506P)^2^+1.9931P] 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 none _refine_ls_extinction_coef 0.0001(2) _refine_ls_number_reflns 2358 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.047961(16) 0.22438(4) 0.489413(16) 0.01217(11) Uani 1 1 d . . . O2 O 0.13048(10) 0.0773(3) 0.35399(10) 0.0215(4) Uani 1 1 d . . . O1 O 0.03778(9) -0.0344(2) 0.43107(9) 0.0145(3) Uani 1 1 d . . . N1 N 0.14045(11) 0.1116(3) 0.54814(10) 0.0145(4) Uani 1 1 d . . . N3 N -0.02801(11) 0.3606(3) 0.42214(11) 0.0142(4) Uani 1 1 d . . . N2 N 0.06619(11) 0.4623(3) 0.55912(11) 0.0137(4) Uani 1 1 d . . . C8 C -0.05651(14) 0.2906(3) 0.35427(14) 0.0171(5) Uani 1 1 d . . . H8 H -0.0395 0.1715 0.3293 0.021 Uiso 1 1 calc R . . C6 C 0.11778(12) 0.4257(3) 0.61479(13) 0.0141(4) Uani 1 1 d . . . C4 C 0.22680(14) 0.1911(4) 0.65136(14) 0.0193(5) Uani 1 1 d . . . H4 H 0.2429 0.2809 0.6896 0.023 Uiso 1 1 calc R . . C9 C 0.08113(13) -0.0501(3) 0.37011(13) 0.0158(4) Uani 1 1 d . . . C7 C -0.11370(14) 0.4209(4) 0.32834(13) 0.0180(5) Uani 1 1 d . . . H7 H -0.1427 0.4106 0.2840 0.022 Uiso 1 1 calc R . . C5 C 0.16408(13) 0.2384(3) 0.60592(14) 0.0156(4) Uani 1 1 d . . . C10 C 0.06479(15) -0.2355(4) 0.31946(16) 0.0233(5) Uani 1 1 d . . . H10A H 0.0242 -0.3184 0.3414 0.035 Uiso 1 1 calc R . . H10B H 0.1110 -0.3182 0.3146 0.035 Uiso 1 1 calc R . . H10C H 0.0489 -0.1875 0.2703 0.035 Uiso 1 1 calc R . . C2 C 0.24010(14) -0.1256(4) 0.57947(14) 0.0208(5) Uani 1 1 d . . . H2 H 0.2653 -0.2512 0.5704 0.025 Uiso 1 1 calc R . . C3 C 0.26487(14) 0.0051(4) 0.63792(15) 0.0221(5) Uani 1 1 d . . . H3 H 0.3070 -0.0331 0.6678 0.027 Uiso 1 1 calc R . . C1 C 0.17808(13) -0.0667(4) 0.53543(14) 0.0180(5) Uani 1 1 d . . . H1 H 0.1620 -0.1527 0.4960 0.022 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 Cu1 0.01280(16) 0.00941(16) 0.01431(18) -0.00095(9) -0.00085(10) 0.00057(9) O2 0.0183(8) 0.0245(9) 0.0217(9) 0.0029(7) -0.0009(7) -0.0046(7) O1 0.0167(8) 0.0118(7) 0.0151(8) -0.0026(6) 0.0016(6) 0.0004(6) N1 0.0134(8) 0.0144(9) 0.0158(9) 0.0022(7) 0.0008(7) 0.0007(7) N3 0.0170(9) 0.0100(9) 0.0157(9) -0.0005(7) -0.0006(7) 0.0018(7) N2 0.0132(8) 0.0103(8) 0.0174(9) -0.0022(7) 0.0010(7) 0.0004(7) C8 0.0224(11) 0.0116(11) 0.0173(12) -0.0032(8) -0.0012(9) 0.0002(8) C6 0.0127(10) 0.0140(10) 0.0154(10) 0.0021(8) -0.0010(8) -0.0013(8) C4 0.0150(10) 0.0228(12) 0.0202(12) 0.0010(9) -0.0018(9) -0.0006(9) C9 0.0148(10) 0.0162(11) 0.0163(11) 0.0007(8) -0.0030(9) 0.0026(8) C7 0.0198(11) 0.0178(11) 0.0163(11) -0.0004(9) -0.0042(9) -0.0013(9) C5 0.0143(10) 0.0147(10) 0.0178(11) 0.0031(8) 0.0020(9) -0.0020(8) C10 0.0188(11) 0.0262(13) 0.0250(13) -0.0105(10) 0.0027(10) -0.0016(10) C2 0.0176(11) 0.0195(11) 0.0251(13) 0.0030(9) 0.0042(9) 0.0065(9) C3 0.0140(10) 0.0268(13) 0.0256(13) 0.0060(10) 0.0006(9) 0.0028(9) C1 0.0173(11) 0.0182(11) 0.0186(11) 0.0009(9) 0.0026(9) 0.0021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9625(19) . ? Cu1 N3 1.9709(19) . ? Cu1 N2 1.986(2) . ? Cu1 N1 2.0332(19) . ? Cu1 O1 2.3737(17) 5_556 ? O2 C9 1.213(3) . ? O1 C9 1.313(3) . ? O1 Cu1 2.3737(17) 5_556 ? N1 C1 1.334(3) . ? N1 C5 1.367(3) . ? N3 N2 1.354(3) 5_566 ? N3 C8 1.370(3) . ? N2 C6 1.345(3) . ? N2 N3 1.354(3) 5_566 ? C8 C7 1.371(3) . ? C6 C7 1.408(3) 5_566 ? C6 C5 1.451(3) . ? C4 C5 1.379(3) . ? C4 C3 1.383(3) . ? C9 C10 1.515(3) . ? C7 C6 1.408(3) 5_566 ? C2 C1 1.374(3) . ? C2 C3 1.396(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 O1 Cu1 N3 90.03(8) . . ? O1 Cu1 N2 171.95(7) . . ? N3 Cu1 N2 97.85(9) . . ? O1 Cu1 N1 92.04(8) . . ? N3 Cu1 N1 169.98(8) . . ? N2 Cu1 N1 80.48(8) . . ? O1 Cu1 O1 79.60(7) . 5_556 ? N3 Cu1 O1 99.85(7) . 5_556 ? N2 Cu1 O1 97.32(8) . 5_556 ? N1 Cu1 O1 90.16(7) . 5_556 ? C9 O1 Cu1 116.35(14) . . ? C9 O1 Cu1 142.96(15) . 5_556 ? Cu1 O1 Cu1 100.40(7) . 5_556 ? C1 N1 C5 119.5(2) . . ? C1 N1 Cu1 126.89(16) . . ? C5 N1 Cu1 113.65(15) . . ? N2 N3 C8 108.36(18) 5_566 . ? N2 N3 Cu1 123.20(15) 5_566 . ? C8 N3 Cu1 128.21(16) . . ? C6 N2 N3 106.80(18) . 5_566 ? C6 N2 Cu1 114.97(15) . . ? N3 N2 Cu1 136.07(15) 5_566 . ? N3 C8 C7 110.4(2) . . ? N2 C6 C7 111.4(2) . 5_566 ? N2 C6 C5 115.4(2) . . ? C7 C6 C5 133.1(2) 5_566 . ? C5 C4 C3 117.5(2) . . ? O2 C9 O1 122.6(2) . . ? O2 C9 C10 121.4(2) . . ? O1 C9 C10 116.0(2) . . ? C8 C7 C6 103.0(2) . 5_566 ? N1 C5 C4 122.4(2) . . ? N1 C5 C6 114.2(2) . . ? C4 C5 C6 123.4(2) . . ? C1 C2 C3 119.3(2) . . ? C4 C3 C2 120.0(2) . . ? N1 C1 C2 121.2(2) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.728 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.097 data_LCuOH _database_code_depnum_ccdc_archive 'CCDC 253145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Cl2 Cu2 N6 O10' _chemical_formula_weight 832.58 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' Cc ' 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' _cell_length_a 7.571(5) _cell_length_b 18.245(5) _cell_length_c 23.845(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 95.334(5) _cell_angle_gamma 90.000(5) _cell_volume 3280(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour ' Dark Blue ' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.527 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10814 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5357 _reflns_number_gt 5026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, 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^)+(0.0326P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(8) _refine_ls_number_reflns 5357 _refine_ls_number_parameters 451 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 Cu2 Cu 0.70583(4) 0.01817(2) 0.30750(2) 0.01364(10) Uani 1 1 d . . . Cu1 Cu 0.71572(4) 0.17111(2) 0.28423(2) 0.01338(10) Uani 1 1 d . . . Cl2 Cl 0.33396(10) 0.07452(5) 0.20453(4) 0.01616(18) Uani 1 1 d . . . Cl1 Cl 1.11308(10) 0.09846(5) 0.37816(4) 0.01748(18) Uani 1 1 d . . . O7 O 0.4543(3) 0.13614(13) 0.20395(13) 0.0269(6) Uani 1 1 d . . . O5 O 0.9894(3) 0.03754(13) 0.37524(12) 0.0240(6) Uani 1 1 d . . . O9 O 0.3999(3) 0.02269(13) 0.24667(12) 0.0196(6) Uani 1 1 d . . . O8 O 0.3207(4) 0.03950(15) 0.15017(12) 0.0266(6) Uani 1 1 d . . . O3 O 1.0311(4) 0.15960(14) 0.34817(14) 0.0312(7) Uani 1 1 d . . . O10 O 0.1617(3) 0.10084(15) 0.21589(12) 0.0287(7) Uani 1 1 d . . . O1 O 0.6261(3) 0.10791(12) 0.33910(11) 0.0134(5) Uani 1 1 d . . . O6 O 1.2669(4) 0.07493(19) 0.35308(15) 0.0425(8) Uani 1 1 d . . . O4 O 1.1598(4) 0.11732(16) 0.43564(12) 0.0298(7) Uani 1 1 d . . . N5 N 0.6280(4) -0.05523(15) 0.36353(13) 0.0132(6) Uani 1 1 d . . . C26 C 0.6994(4) -0.13721(18) 0.29160(17) 0.0152(8) Uani 1 1 d . . . C11 C 0.6241(5) 0.31403(19) 0.50316(17) 0.0215(8) Uani 1 1 d . . . H11 H 0.5246 0.3438 0.4966 0.026 Uiso 1 1 calc R . . O2 O 0.8036(3) 0.08180(12) 0.25343(10) 0.0145(5) Uani 1 1 d . . . N2 N 0.6603(4) 0.26963(15) 0.31743(13) 0.0152(6) Uani 1 1 d . . . N1 N 0.7855(4) 0.23616(15) 0.22255(14) 0.0144(6) Uani 1 1 d . . . N3 N 0.6032(4) 0.29840(15) 0.36430(13) 0.0159(6) Uani 1 1 d . . . C27 C 0.7109(5) -0.20495(19) 0.26562(17) 0.0189(8) Uani 1 1 d . . . H27 H 0.6797 -0.2476 0.2837 0.023 Uiso 1 1 calc R . . N6 N 0.7461(4) -0.07441(16) 0.26631(14) 0.0142(6) Uani 1 1 d . . . C21 C 0.6733(5) 0.00044(18) 0.50313(17) 0.0186(8) Uani 1 1 d . . . N4 N 0.5639(4) -0.05574(15) 0.41377(14) 0.0181(7) Uani 1 1 d . . . C10 C 0.6585(5) 0.26088(18) 0.46394(16) 0.0177(7) Uani 1 1 d . . . C20 C 0.6041(5) -0.02332(19) 0.55189(16) 0.0185(8) Uani 1 1 d . . . H20 H 0.4821 -0.0288 0.5523 0.022 Uiso 1 1 calc R . . C3 C 0.8505(5) 0.3368(2) 0.14000(18) 0.0239(8) Uani 1 1 d . . . H3 H 0.8726 0.3702 0.1121 0.029 Uiso 1 1 calc R . . C8 C 0.6095(5) 0.37240(18) 0.36214(18) 0.0195(8) Uani 1 1 d . . . H8 H 0.5771 0.4043 0.3899 0.023 Uiso 1 1 calc R . . C22 C 0.5572(5) 0.01033(19) 0.44945(16) 0.0207(8) Uani 1 1 d . . . H22A H 0.4360 0.0190 0.4578 0.025 Uiso 1 1 calc R . . H22B H 0.5966 0.0526 0.4293 0.025 Uiso 1 1 calc R . . C1 C 0.8367(5) 0.2145(2) 0.17307(17) 0.0197(8) Uani 1 1 d . . . H1 H 0.8502 0.1646 0.1670 0.024 Uiso 1 1 calc R . . C23 C 0.5301(5) -0.12576(19) 0.42944(17) 0.0201(8) Uani 1 1 d . . . H23 H 0.4861 -0.1401 0.4629 0.024 Uiso 1 1 calc R . . C19 C 0.7156(5) -0.03902(19) 0.60015(16) 0.0220(8) Uani 1 1 d . . . H19 H 0.6684 -0.0561 0.6323 0.026 Uiso 1 1 calc R . . C5 C 0.7647(4) 0.30916(19) 0.23113(17) 0.0153(7) Uani 1 1 d . . . C16 C 0.8557(5) 0.01200(18) 0.50412(17) 0.0215(8) Uani 1 1 d . . . H16 H 0.9038 0.0300 0.4723 0.026 Uiso 1 1 calc R . . C9 C 0.5421(5) 0.25253(18) 0.40953(16) 0.0183(8) Uani 1 1 d . . . H9A H 0.5416 0.2016 0.3979 0.022 Uiso 1 1 calc R . . H9B H 0.4215 0.2660 0.4156 0.022 Uiso 1 1 calc R . . C2 C 0.8703(5) 0.2619(2) 0.13086(17) 0.0237(8) Uani 1 1 d . . . H2 H 0.9055 0.2446 0.0969 0.028 Uiso 1 1 calc R . . C17 C 0.9647(5) -0.0033(2) 0.55229(18) 0.0237(9) Uani 1 1 d . . . H17 H 1.0864 0.0040 0.5526 0.028 Uiso 1 1 calc R . . C14 C 0.9184(5) 0.2253(2) 0.52339(18) 0.0278(9) Uani 1 1 d . . . H14 H 1.0179 0.1955 0.5301 0.033 Uiso 1 1 calc R . . C29 C 0.8136(5) -0.1439(2) 0.18619(18) 0.0217(8) Uani 1 1 d . . . H29 H 0.8505 -0.1449 0.1501 0.026 Uiso 1 1 calc R . . C15 C 0.8069(5) 0.21637(19) 0.47481(18) 0.0241(8) Uani 1 1 d . . . H15 H 0.8310 0.1803 0.4491 0.029 Uiso 1 1 calc R . . C25 C 0.6334(4) -0.12492(18) 0.34661(16) 0.0149(8) Uani 1 1 d . . . C24 C 0.5726(5) -0.17127(19) 0.38702(17) 0.0195(8) Uani 1 1 d . . . H24 H 0.5629 -0.2221 0.3855 0.023 Uiso 1 1 calc R . . C4 C 0.7982(5) 0.3608(2) 0.19034(17) 0.0198(8) Uani 1 1 d . . . H4 H 0.7852 0.4106 0.1972 0.024 Uiso 1 1 calc R . . C30 C 0.8018(5) -0.0782(2) 0.21464(17) 0.0190(8) Uani 1 1 d . . . H30 H 0.8336 -0.0352 0.1973 0.023 Uiso 1 1 calc R . . C18 C 0.8951(5) -0.0293(2) 0.60008(18) 0.0241(8) Uani 1 1 d . . . H18 H 0.9700 -0.0401 0.6321 0.029 Uiso 1 1 calc R . . C12 C 0.7363(5) 0.3231(2) 0.55184(17) 0.0262(9) Uani 1 1 d . . . H12 H 0.7134 0.3593 0.5776 0.031 Uiso 1 1 calc R . . C28 C 0.7696(5) -0.20791(19) 0.21243(18) 0.0216(8) Uani 1 1 d . . . H28 H 0.7793 -0.2528 0.1945 0.026 Uiso 1 1 calc R . . C6 C 0.7023(5) 0.32721(17) 0.2857(2) 0.0164(7) Uani 1 1 d . . . C7 C 0.6719(4) 0.39258(18) 0.31215(17) 0.0180(8) Uani 1 1 d . . . H7 H 0.6896 0.4398 0.2991 0.022 Uiso 1 1 calc R . . C13 C 0.8833(5) 0.2780(2) 0.56198(18) 0.0286(9) Uani 1 1 d . . . H13 H 0.9580 0.2833 0.5949 0.034 Uiso 1 1 calc R . . H31 H 0.5297 0.1045 0.3344 0.050 Uiso 1 1 d . . . H32 H 0.8931 0.0866 0.2482 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.0167(2) 0.0099(2) 0.0144(2) 0.00081(19) 0.00261(17) -0.00011(17) Cu1 0.0150(2) 0.00962(19) 0.0156(2) -0.00020(18) 0.00189(17) -0.00112(16) Cl2 0.0123(4) 0.0169(4) 0.0190(5) 0.0013(4) 0.0001(3) -0.0003(3) Cl1 0.0137(4) 0.0224(4) 0.0165(4) -0.0010(4) 0.0020(3) -0.0011(3) O7 0.0180(13) 0.0175(13) 0.0439(19) 0.0076(13) -0.0045(12) -0.0034(10) O5 0.0254(14) 0.0167(12) 0.0288(16) 0.0034(12) -0.0029(13) -0.0021(10) O9 0.0192(13) 0.0185(13) 0.0201(15) 0.0029(11) -0.0047(12) -0.0015(10) O8 0.0299(15) 0.0308(15) 0.0191(15) 0.0000(13) 0.0028(12) 0.0037(12) O3 0.0400(17) 0.0141(13) 0.0369(19) 0.0057(13) -0.0106(15) -0.0093(12) O10 0.0157(13) 0.0386(16) 0.0323(17) 0.0017(14) 0.0049(12) 0.0060(11) O1 0.0145(12) 0.0102(11) 0.0155(13) -0.0006(11) 0.0014(10) -0.0028(9) O6 0.0221(15) 0.067(2) 0.040(2) -0.0071(18) 0.0133(15) -0.0027(14) O4 0.0303(15) 0.0367(16) 0.0215(15) -0.0054(14) -0.0015(13) 0.0024(12) N5 0.0135(14) 0.0137(14) 0.0123(16) -0.0013(12) 0.0008(13) -0.0008(11) C26 0.0087(16) 0.0147(16) 0.022(2) -0.0005(15) -0.0029(15) 0.0009(13) C11 0.0227(19) 0.0224(18) 0.020(2) -0.0010(16) 0.0053(16) -0.0019(14) O2 0.0148(12) 0.0139(12) 0.0151(13) -0.0003(11) 0.0036(10) -0.0002(9) N2 0.0156(15) 0.0133(14) 0.0168(17) -0.0033(12) 0.0015(12) 0.0004(11) N1 0.0146(14) 0.0119(14) 0.0165(17) 0.0000(13) 0.0000(13) -0.0032(11) N3 0.0192(15) 0.0166(14) 0.0119(16) 0.0013(13) 0.0017(13) 0.0006(12) C27 0.0155(17) 0.0133(17) 0.027(2) -0.0003(16) -0.0010(16) 0.0011(14) N6 0.0139(15) 0.0123(14) 0.0163(16) 0.0006(12) 0.0009(12) -0.0008(11) C21 0.0234(18) 0.0122(16) 0.021(2) -0.0026(15) 0.0041(16) 0.0022(13) N4 0.0240(16) 0.0138(14) 0.0166(17) 0.0025(13) 0.0021(13) 0.0017(12) C10 0.0191(17) 0.0149(16) 0.0199(19) 0.0033(15) 0.0065(15) -0.0016(13) C20 0.0166(17) 0.0202(17) 0.019(2) -0.0010(15) 0.0031(15) 0.0000(13) C3 0.0234(19) 0.0227(19) 0.026(2) 0.0083(17) 0.0023(17) 0.0005(15) C8 0.0238(18) 0.0112(17) 0.023(2) -0.0036(15) 0.0000(17) 0.0036(14) C22 0.033(2) 0.0149(17) 0.015(2) 0.0010(15) 0.0055(17) 0.0050(15) C1 0.0165(17) 0.0186(18) 0.024(2) 0.0007(17) 0.0003(16) 0.0019(14) C23 0.0204(18) 0.0178(18) 0.023(2) 0.0103(16) 0.0040(16) -0.0035(14) C19 0.028(2) 0.0258(18) 0.0135(19) 0.0036(16) 0.0055(16) 0.0024(15) C5 0.0100(16) 0.0170(17) 0.0182(19) -0.0024(15) -0.0024(14) -0.0008(12) C16 0.029(2) 0.0167(17) 0.021(2) 0.0002(16) 0.0126(17) -0.0004(15) C9 0.0217(19) 0.0174(17) 0.016(2) -0.0020(15) 0.0051(16) -0.0024(14) C2 0.028(2) 0.027(2) 0.016(2) -0.0006(17) 0.0063(17) -0.0002(16) C17 0.0158(18) 0.028(2) 0.028(2) -0.0075(17) 0.0053(17) -0.0015(14) C14 0.025(2) 0.029(2) 0.029(2) 0.0093(19) -0.0006(18) 0.0039(16) C29 0.023(2) 0.0227(19) 0.019(2) -0.0032(17) 0.0024(16) 0.0024(15) C15 0.0272(19) 0.0176(17) 0.029(2) 0.0020(17) 0.0095(17) 0.0003(14) C25 0.0091(16) 0.0121(16) 0.022(2) 0.0022(15) -0.0043(15) -0.0013(12) C24 0.0196(18) 0.0160(17) 0.023(2) 0.0028(16) 0.0013(16) -0.0003(14) C4 0.0221(19) 0.0137(17) 0.024(2) 0.0028(16) 0.0042(16) 0.0015(14) C30 0.0165(18) 0.0192(18) 0.021(2) 0.0048(16) -0.0019(16) 0.0010(14) C18 0.023(2) 0.028(2) 0.021(2) -0.0025(17) -0.0031(17) 0.0053(16) C12 0.034(2) 0.028(2) 0.017(2) 0.0000(17) 0.0043(17) -0.0089(17) C28 0.0232(19) 0.0127(17) 0.028(2) -0.0052(16) -0.0037(17) 0.0036(14) C6 0.0132(16) 0.0107(15) 0.0245(18) 0.0007(16) -0.0024(14) -0.0026(13) C7 0.0150(18) 0.0108(15) 0.027(2) 0.0011(16) -0.0060(16) 0.0029(12) C13 0.028(2) 0.037(2) 0.020(2) 0.0059(19) -0.0018(18) -0.0089(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 O1 1.923(2) . ? Cu2 O2 1.933(2) . ? Cu2 N6 1.992(3) . ? Cu2 N5 2.018(3) . ? Cu2 Cu1 2.8474(9) . ? Cu1 O1 1.915(2) . ? Cu1 O2 1.931(2) . ? Cu1 N1 1.999(3) . ? Cu1 N2 2.024(3) . ? Cl2 O9 1.435(3) . ? Cl2 O10 1.439(3) . ? Cl2 O8 1.440(3) . ? Cl2 O7 1.448(3) . ? Cl1 O6 1.424(3) . ? Cl1 O4 1.426(3) . ? Cl1 O3 1.435(3) . ? Cl1 O5 1.451(3) . ? N5 N4 1.334(4) . ? N5 C25 1.336(4) . ? C26 N6 1.357(4) . ? C26 C27 1.389(5) . ? C26 C25 1.464(5) . ? C11 C12 1.383(6) . ? C11 C10 1.389(5) . ? N2 N3 1.342(4) . ? N2 C6 1.350(5) . ? N1 C1 1.335(5) . ? N1 C5 1.359(4) . ? N3 C8 1.352(4) . ? N3 C9 1.473(4) . ? C27 C28 1.383(6) . ? N6 C30 1.340(5) . ? C21 C20 1.388(5) . ? C21 C16 1.395(5) . ? C21 C22 1.495(5) . ? N4 C23 1.362(4) . ? N4 C22 1.479(4) . ? C10 C15 1.391(5) . ? C10 C9 1.507(5) . ? C20 C19 1.392(5) . ? C3 C4 1.371(6) . ? C3 C2 1.394(5) . ? C8 C7 1.372(5) . ? C1 C2 1.369(5) . ? C23 C24 1.370(5) . ? C19 C18 1.371(5) . ? C5 C4 1.394(5) . ? C5 C6 1.462(6) . ? C16 C17 1.379(6) . ? C17 C18 1.383(6) . ? C14 C13 1.373(5) . ? C14 C15 1.378(6) . ? C29 C28 1.380(5) . ? C29 C30 1.385(5) . ? C25 C24 1.392(5) . ? C12 C13 1.388(6) . ? C6 C7 1.379(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 O1 Cu2 O2 84.47(10) . . ? O1 Cu2 N6 169.56(12) . . ? O2 Cu2 N6 95.44(11) . . ? O1 Cu2 N5 100.60(10) . . ? O2 Cu2 N5 173.62(11) . . ? N6 Cu2 N5 80.28(13) . . ? O1 Cu2 Cu1 42.00(7) . . ? O2 Cu2 Cu1 42.50(7) . . ? N6 Cu2 Cu1 136.64(9) . . ? N5 Cu2 Cu1 142.56(8) . . ? O1 Cu1 O2 84.73(10) . . ? O1 Cu1 N1 174.24(12) . . ? O2 Cu1 N1 95.58(11) . . ? O1 Cu1 N2 99.67(11) . . ? O2 Cu1 N2 171.77(11) . . ? N1 Cu1 N2 80.75(12) . . ? O1 Cu1 Cu2 42.21(7) . . ? O2 Cu1 Cu2 42.55(7) . . ? N1 Cu1 Cu2 137.63(9) . . ? N2 Cu1 Cu2 141.63(9) . . ? O9 Cl2 O10 110.51(16) . . ? O9 Cl2 O8 109.17(16) . . ? O10 Cl2 O8 109.21(17) . . ? O9 Cl2 O7 109.87(16) . . ? O10 Cl2 O7 108.96(16) . . ? O8 Cl2 O7 109.10(17) . . ? O6 Cl1 O4 109.70(19) . . ? O6 Cl1 O3 111.0(2) . . ? O4 Cl1 O3 110.41(18) . . ? O6 Cl1 O5 107.35(19) . . ? O4 Cl1 O5 109.42(17) . . ? O3 Cl1 O5 108.92(17) . . ? Cu1 O1 Cu2 95.78(11) . . ? N4 N5 C25 106.8(3) . . ? N4 N5 Cu2 138.8(2) . . ? C25 N5 Cu2 114.4(2) . . ? N6 C26 C27 121.6(3) . . ? N6 C26 C25 113.2(3) . . ? C27 C26 C25 125.2(3) . . ? C12 C11 C10 120.7(4) . . ? Cu1 O2 Cu2 94.95(10) . . ? N3 N2 C6 105.9(3) . . ? N3 N2 Cu1 140.2(2) . . ? C6 N2 Cu1 113.8(2) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Cu1 126.3(2) . . ? C5 N1 Cu1 115.4(3) . . ? N2 N3 C8 110.1(3) . . ? N2 N3 C9 122.3(3) . . ? C8 N3 C9 127.6(3) . . ? C28 C27 C26 118.9(3) . . ? C30 N6 C26 118.8(3) . . ? C30 N6 Cu2 124.9(2) . . ? C26 N6 Cu2 116.0(2) . . ? C20 C21 C16 118.9(4) . . ? C20 C21 C22 121.2(3) . . ? C16 C21 C22 119.9(3) . . ? N5 N4 C23 110.3(3) . . ? N5 N4 C22 123.1(3) . . ? C23 N4 C22 126.1(3) . . ? C11 C10 C15 118.8(4) . . ? C11 C10 C9 121.3(3) . . ? C15 C10 C9 119.9(3) . . ? C21 C20 C19 120.6(3) . . ? C4 C3 C2 119.7(4) . . ? N3 C8 C7 108.5(3) . . ? N4 C22 C21 110.2(3) . . ? N1 C1 C2 123.5(3) . . ? N4 C23 C24 107.6(3) . . ? C18 C19 C20 119.8(3) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 114.0(3) . . ? C4 C5 C6 124.3(3) . . ? C17 C16 C21 119.9(4) . . ? N3 C9 C10 112.0(3) . . ? C1 C2 C3 118.3(4) . . ? C16 C17 C18 120.7(4) . . ? C13 C14 C15 120.3(4) . . ? C28 C29 C30 118.8(4) . . ? C14 C15 C10 120.6(4) . . ? N5 C25 C24 110.4(3) . . ? N5 C25 C26 116.0(3) . . ? C24 C25 C26 133.6(3) . . ? C23 C24 C25 105.0(3) . . ? C3 C4 C5 118.7(3) . . ? N6 C30 C29 122.4(3) . . ? C19 C18 C17 120.0(4) . . ? C11 C12 C13 119.7(4) . . ? C29 C28 C27 119.6(3) . . ? N2 C6 C7 111.0(4) . . ? N2 C6 C5 115.8(3) . . ? C7 C6 C5 133.1(3) . . ? C8 C7 C6 104.5(3) . . ? C14 C13 C12 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.614 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.077 data_LCuOAc _database_code_depnum_ccdc_archive 'CCDC 253146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C40 H46 N8 O6 Cu2 2+, 2 (Cl O4) 2-, (C3 H7 N O), 0.5 (C2 H4 O2) ' _chemical_formula_sum 'C44 H52 Cl2 Cu2 N9 O16' _chemical_formula_weight 1160.93 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.234(5) _cell_length_b 23.253(5) _cell_length_c 19.581(5) _cell_angle_alpha 90.000 _cell_angle_beta 98.723(5) _cell_angle_gamma 90.000 _cell_volume 5056(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour ' Bluish green ' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26671 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.1276 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12404 _reflns_number_gt 7788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, 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^)+(0.0900P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 12404 _refine_ls_number_parameters 1277 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _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 Cu1 Cu 0.42912(12) 0.21756(6) 0.42163(6) 0.0322(3) Uani 1 1 d . . . Cu2 Cu 0.69274(11) 0.26116(6) 0.44479(6) 0.0328(3) Uani 1 1 d . . . N1 N 0.4038(7) 0.2100(4) 0.5221(4) 0.028(2) Uani 1 1 d . . . C1 C 0.3762(9) 0.2521(5) 0.5633(5) 0.033(3) Uani 1 1 d . . . H1 H 0.3651 0.2890 0.5451 0.039 Uiso 1 1 calc R . . C2 C 0.3633(12) 0.2437(6) 0.6311(6) 0.050(3) Uani 1 1 d . . . H2 H 0.3465 0.2743 0.6587 0.060 Uiso 1 1 calc R . . C3 C 0.3757(10) 0.1887(6) 0.6573(6) 0.045(3) Uani 1 1 d . . . H3 H 0.3661 0.1812 0.7028 0.054 Uiso 1 1 calc R . . C4 C 0.4025(10) 0.1455(6) 0.6151(6) 0.042(3) Uani 1 1 d . . . H4 H 0.4117 0.1080 0.6318 0.050 Uiso 1 1 calc R . . C5 C 0.4160(10) 0.1569(5) 0.5482(6) 0.042(3) Uani 1 1 d . . . C6 C 0.4482(11) 0.1136(6) 0.4978(6) 0.047(3) Uani 1 1 d . . . C7 C 0.4697(12) 0.0560(5) 0.5043(7) 0.053(4) Uani 1 1 d . . . H7 H 0.4706 0.0333 0.5435 0.064 Uiso 1 1 calc R . . C8 C 0.4895(12) 0.0393(6) 0.4404(6) 0.050(3) Uani 1 1 d . . . H8 H 0.5058 0.0019 0.4276 0.060 Uiso 1 1 calc R . . N2 N 0.4537(9) 0.1316(5) 0.4348(5) 0.042(3) Uani 1 1 d . . . N3 N 0.4820(9) 0.0847(5) 0.3994(5) 0.044(3) Uani 1 1 d . . . C9 C 0.4819(11) 0.0855(6) 0.3254(6) 0.051(3) Uani 1 1 d . . . H9A H 0.5222 0.0514 0.3120 0.061 Uiso 1 1 calc R . . H9B H 0.5266 0.1188 0.3134 0.061 Uiso 1 1 calc R . . C10 C 0.3561(13) 0.0877(6) 0.2859(7) 0.054(4) Uani 1 1 d . . . C11 C 0.2551(14) 0.0752(7) 0.3118(9) 0.074(4) Uani 1 1 d . . . H11 H 0.2615 0.0636 0.3577 0.089 Uiso 1 1 calc R . . C12 C 0.1422(16) 0.0789(7) 0.2729(10) 0.086(5) Uani 1 1 d . . . H12 H 0.0735 0.0722 0.2929 0.104 Uiso 1 1 calc R . . C13 C 0.1336(19) 0.0920(9) 0.2068(12) 0.104(7) Uani 1 1 d . . . H13 H 0.0582 0.0907 0.1796 0.125 Uiso 1 1 calc R . . C14 C 0.2329(19) 0.1080(9) 0.1759(8) 0.094(6) Uani 1 1 d . . . H14 H 0.2252 0.1203 0.1303 0.112 Uiso 1 1 calc R . . C15 C 0.3463(15) 0.1042(7) 0.2190(8) 0.072(5) Uani 1 1 d . . . H15 H 0.4158 0.1132 0.2008 0.087 Uiso 1 1 calc R . . N4 N 0.7479(8) 0.1794(5) 0.4358(5) 0.043(3) Uani 1 1 d . . . C16 C 0.7690(9) 0.1546(5) 0.3793(5) 0.035(3) Uani 1 1 d . . . H16 H 0.7637 0.1767 0.3394 0.042 Uiso 1 1 calc R . . C17 C 0.7989(11) 0.0969(6) 0.3754(6) 0.047(3) Uani 1 1 d . . . H17 H 0.8138 0.0804 0.3343 0.057 Uiso 1 1 calc R . . C18 C 0.8054(12) 0.0656(6) 0.4346(6) 0.057(4) Uani 1 1 d . . . H18 H 0.8266 0.0269 0.4345 0.068 Uiso 1 1 calc R . . C19 C 0.7811(11) 0.0904(6) 0.4942(6) 0.046(3) Uani 1 1 d . . . H19 H 0.7845 0.0688 0.5344 0.056 Uiso 1 1 calc R . . C20 C 0.7516(11) 0.1474(6) 0.4937(5) 0.041(3) Uani 1 1 d . . . C21 C 0.7252(9) 0.1784(5) 0.5544(5) 0.033(3) Uani 1 1 d . . . C22 C 0.7192(11) 0.1626(7) 0.6207(6) 0.049(3) Uani 1 1 d . . . H22 H 0.7325 0.1261 0.6399 0.059 Uiso 1 1 calc R . . C23 C 0.6898(10) 0.2112(7) 0.6527(5) 0.050(4) Uani 1 1 d . . . H23 H 0.6784 0.2140 0.6986 0.059 Uiso 1 1 calc R . . N5 N 0.7022(7) 0.2348(4) 0.5432(4) 0.030(2) Uani 1 1 d . . . N6 N 0.6798(9) 0.2550(5) 0.6060(4) 0.047(3) Uani 1 1 d . . . C24 C 0.6629(11) 0.3142(6) 0.6200(6) 0.044(3) Uani 1 1 d . . . H24A H 0.6274 0.3176 0.6620 0.052 Uiso 1 1 calc R . . H24B H 0.6069 0.3307 0.5825 0.052 Uiso 1 1 calc R . . C25 C 0.7808(12) 0.3485(6) 0.6283(6) 0.050(3) Uani 1 1 d . . . C26 C 0.8930(11) 0.3245(7) 0.6484(6) 0.054(4) Uani 1 1 d . . . H26 H 0.8980 0.2850 0.6556 0.065 Uiso 1 1 calc R . . C27 C 0.9938(12) 0.3549(7) 0.6577(7) 0.064(4) Uani 1 1 d . . . H27 H 1.0677 0.3373 0.6722 0.077 Uiso 1 1 calc R . . C28 C 0.9860(15) 0.4151(8) 0.6450(7) 0.067(4) Uani 1 1 d . . . H28 H 1.0546 0.4379 0.6537 0.080 Uiso 1 1 calc R . . C29 C 0.8806(15) 0.4385(7) 0.6209(7) 0.071(4) Uani 1 1 d . . . H29 H 0.8765 0.4772 0.6086 0.085 Uiso 1 1 calc R . . C30 C 0.7789(13) 0.4066(7) 0.6140(6) 0.061(4) Uani 1 1 d . . . H30 H 0.7054 0.4243 0.5992 0.073 Uiso 1 1 calc R . . O1 O 0.2412(7) 0.2139(3) 0.3729(4) 0.044(2) Uani 1 1 d . . . N7 N 0.1026(8) 0.2306(5) 0.2785(5) 0.049(3) Uani 1 1 d . . . C31 C 0.2141(11) 0.2242(5) 0.3106(5) 0.041(3) Uani 1 1 d . . . H31 H 0.2763 0.2277 0.2845 0.050 Uiso 1 1 calc . . . C32 C 0.0751(13) 0.2430(7) 0.2040(6) 0.073(5) Uani 1 1 d . . . H32A H -0.0105 0.2461 0.1907 0.110 Uiso 1 1 calc R . . H32B H 0.1053 0.2125 0.1784 0.110 Uiso 1 1 calc R . . H32C H 0.1125 0.2786 0.1943 0.110 Uiso 1 1 calc R . . C33 C 0.0024(14) 0.2168(9) 0.3128(7) 0.090(6) Uani 1 1 d . . . H33A H -0.0713 0.2242 0.2824 0.135 Uiso 1 1 calc R . . H33B H 0.0055 0.2400 0.3536 0.135 Uiso 1 1 calc R . . H33C H 0.0059 0.1768 0.3255 0.135 Uiso 1 1 calc R . . O4 O 0.8655(7) 0.3001(4) 0.4475(4) 0.043(2) Uani 1 1 d . . . N8 N 0.9947(10) 0.3752(5) 0.4577(5) 0.057(3) Uani 1 1 d . . . C34 C 0.8923(12) 0.3492(7) 0.4587(5) 0.052(4) Uani 1 1 d . . . H34 H 0.8307 0.3724 0.4698 0.063 Uiso 1 1 calc . . . C35 C 1.0956(17) 0.3463(9) 0.4433(11) 0.112(7) Uani 1 1 d . . . H35D H 1.1617 0.3727 0.4453 0.168 Uiso 1 1 calc R . . H35E H 1.0790 0.3298 0.3979 0.168 Uiso 1 1 calc R . . H35F H 1.1162 0.3163 0.4767 0.168 Uiso 1 1 calc R . . C36 C 1.0076(18) 0.4381(9) 0.4734(8) 0.112(8) Uani 1 1 d . . . H36D H 1.0885 0.4500 0.4705 0.167 Uiso 1 1 calc R . . H36E H 0.9904 0.4452 0.5192 0.167 Uiso 1 1 calc R . . H36F H 0.9523 0.4593 0.4407 0.167 Uiso 1 1 calc R . . O2 O 0.4788(7) 0.2199(3) 0.3311(3) 0.0366(18) Uani 1 1 d . . . O3 O 0.6528(7) 0.2709(3) 0.3434(3) 0.0401(19) Uani 1 1 d . . . C37 C 0.5483(12) 0.2532(5) 0.2305(5) 0.048(3) Uani 1 1 d . . . H37A H 0.4764 0.2340 0.2094 0.072 Uiso 1 1 calc R . . H37B H 0.6170 0.2362 0.2148 0.072 Uiso 1 1 calc R . . H37C H 0.5439 0.2932 0.2181 0.072 Uiso 1 1 calc R . . C38 C 0.5606(11) 0.2473(5) 0.3101(5) 0.035(3) Uani 1 1 d . . . O5 O 0.6105(7) 0.3329(3) 0.4573(3) 0.0367(19) Uani 1 1 d . . . O6 O 0.4217(6) 0.3011(3) 0.4256(3) 0.0314(18) Uani 1 1 d . . . C39 C 0.4512(11) 0.4002(5) 0.4476(5) 0.039(3) Uani 1 1 d . . . H39A H 0.5182 0.4255 0.4611 0.059 Uiso 1 1 calc R . . H39B H 0.3978 0.4016 0.4815 0.059 Uiso 1 1 calc R . . H39C H 0.4087 0.4121 0.4036 0.059 Uiso 1 1 calc R . . C40 C 0.4957(12) 0.3405(5) 0.4423(5) 0.036(3) Uani 1 1 d . . . Cu1A Cu 0.21299(14) 0.36471(9) 0.03952(7) 0.0608(5) Uani 1 1 d . . . Cu2A Cu 0.47361(13) 0.40719(6) 0.08019(7) 0.0417(4) Uani 1 1 d . . . N1A N 0.1561(11) 0.4462(8) 0.0410(8) 0.093(6) Uani 1 1 d . . . C1A C 0.1351(18) 0.4750(11) -0.0191(13) 0.112(8) Uani 1 1 d . . . C2A C 0.098(2) 0.5351(10) -0.0163(15) 0.125(9) Uani 1 1 d . . . H2A H 0.0856 0.5561 -0.0571 0.150 Uiso 1 1 calc R . . C3A C 0.083(3) 0.5606(15) 0.0412(18) 0.173(14) Uani 1 1 d . . . H3A H 0.0617 0.5993 0.0420 0.208 Uiso 1 1 calc R . . C4A C 0.097(2) 0.5308(12) 0.0949(18) 0.140(9) Uani 1 1 d . . . H4A H 0.0797 0.5478 0.1353 0.168 Uiso 1 1 calc R . . C5A C 0.137(2) 0.4718(11) 0.0989(16) 0.132(9) Uani 1 1 d . . . H5A H 0.1500 0.4524 0.1408 0.158 Uiso 1 1 calc R . . C6A C 0.1513(19) 0.4432(18) -0.0733(11) 0.137(12) Uani 1 1 d . . . C7A C 0.150(2) 0.4595(14) -0.1431(11) 0.147(11) Uani 1 1 d . . . H7A H 0.1302 0.4948 -0.1641 0.176 Uiso 1 1 calc R . . C8A C 0.1842(15) 0.4104(14) -0.1712(8) 0.109(9) Uani 1 1 d . . . H8A H 0.1900 0.4059 -0.2178 0.131 Uiso 1 1 calc R . . N2A N 0.1954(12) 0.3875(11) -0.0640(7) 0.102(7) Uani 1 1 d . . . N3A N 0.2082(11) 0.3706(9) -0.1253(9) 0.092(5) Uani 1 1 d . . . C9A C 0.2393(14) 0.3104(10) -0.1307(9) 0.098(7) Uani 1 1 d . . . H9A1 H 0.2713 0.2972 -0.0846 0.118 Uiso 1 1 calc R . . H9A2 H 0.3047 0.3085 -0.1578 0.118 Uiso 1 1 calc R . . C10A C 0.1401(12) 0.2650(10) -0.1628(8) 0.165(13) Uani 1 1 d G . . C11A C 0.0318(16) 0.2700(10) -0.1371(8) 0.29(3) Uani 1 1 d G . . H11A H 0.0240 0.2969 -0.1030 0.353 Uiso 1 1 calc R . . C12A C -0.0647(13) 0.2346(12) -0.1623(9) 0.21(2) Uani 1 1 d G . . H12A H -0.1371 0.2380 -0.1451 0.253 Uiso 1 1 calc R . . C13A C -0.0530(17) 0.1943(8) -0.2133(10) 0.175(13) Uani 1 1 d G . . H13A H -0.1175 0.1707 -0.2302 0.210 Uiso 1 1 calc R . . C14A C 0.055(2) 0.1893(9) -0.2390(10) 0.27(3) Uani 1 1 d G . . H14A H 0.0631 0.1624 -0.2731 0.321 Uiso 1 1 calc R . . C15A C 0.1518(14) 0.2247(11) -0.2138(10) 0.27(2) Uani 1 1 d G . . H15A H 0.2242 0.2213 -0.2310 0.319 Uiso 1 1 calc R . . N4A N 0.4873(9) 0.4249(5) -0.0188(5) 0.043(3) Uani 1 1 d . . . C16A C 0.5097(12) 0.3861(7) -0.0663(6) 0.058(4) Uani 1 1 d . . . H16A H 0.5245 0.3482 -0.0527 0.070 Uiso 1 1 calc R . . C17A C 0.5113(12) 0.4006(7) -0.1340(6) 0.058(4) Uani 1 1 d . . . H17A H 0.5278 0.3731 -0.1657 0.070 Uiso 1 1 calc R . . C18A C 0.4875(15) 0.4582(7) -0.1544(7) 0.071(5) Uani 1 1 d . . . H18A H 0.4915 0.4702 -0.1993 0.085 Uiso 1 1 calc R . . C19A C 0.4588(15) 0.4951(7) -0.1065(7) 0.077(5) Uani 1 1 d . . . H19A H 0.4361 0.5325 -0.1193 0.092 Uiso 1 1 calc R . . C20A C 0.4627(14) 0.4785(7) -0.0397(7) 0.068(4) Uani 1 1 d . . . C21A C 0.4379(14) 0.5167(7) 0.0168(9) 0.073(4) Uani 1 1 d . . . C22A C 0.4189(17) 0.5751(7) 0.0192(10) 0.090(6) Uani 1 1 d . . . H22A H 0.4135 0.6013 -0.0171 0.108 Uiso 1 1 calc R . . C23A C 0.4095(16) 0.5862(8) 0.0874(12) 0.100(6) Uani 1 1 d . . . H23A H 0.3978 0.6223 0.1057 0.121 Uiso 1 1 calc R . . N5A N 0.4427(10) 0.4927(5) 0.0793(5) 0.048(3) Uani 1 1 d . . . N6A N 0.4203(11) 0.5362(5) 0.1237(6) 0.062(3) Uani 1 1 d . . . C24A C 0.4235(15) 0.5278(8) 0.1951(7) 0.077(5) Uani 1 1 d . . . H24C H 0.3769 0.4938 0.2018 0.093 Uiso 1 1 calc R . . H24D H 0.3843 0.5603 0.2134 0.093 Uiso 1 1 calc R . . C25A C 0.5466(13) 0.5212(7) 0.2363(8) 0.066(4) Uani 1 1 d . . . C26A C 0.6501(19) 0.5457(9) 0.2164(10) 0.105(7) Uani 1 1 d . . . H26A H 0.6453 0.5666 0.1756 0.126 Uiso 1 1 calc R . . C27A C 0.7599(19) 0.5385(10) 0.2587(12) 0.113(8) Uani 1 1 d . . . H27A H 0.8299 0.5536 0.2460 0.135 Uiso 1 1 calc R . . C28A C 0.764(2) 0.5091(10) 0.3193(10) 0.105(7) Uani 1 1 d . . . H28A H 0.8382 0.5066 0.3475 0.126 Uiso 1 1 calc R . . C29A C 0.6698(16) 0.4832(11) 0.3418(10) 0.108(8) Uani 1 1 d . . . H29A H 0.6770 0.4620 0.3824 0.129 Uiso 1 1 calc R . . C30A C 0.5601(15) 0.4914(7) 0.2984(7) 0.066(4) Uani 1 1 d . . . H30A H 0.4913 0.4758 0.3122 0.079 Uiso 1 1 calc R . . O1A O 0.019(2) 0.3271(9) 0.0396(8) 0.160(9) Uani 1 1 d . . . N7A N -0.1147(15) 0.2698(8) 0.0318(6) 0.085(5) Uani 1 1 d . . . C31A C 0.036(2) 0.2914(10) 0.0288(10) 0.094(8) Uani 1 1 d . . . H31A H 0.1050 0.2726 0.0195 0.113 Uiso 1 1 calc . . . C32A C -0.122(2) 0.2103(11) 0.0215(12) 0.132(9) Uani 1 1 d . . . H32D H -0.0463 0.1964 0.0107 0.197 Uiso 1 1 calc R . . H32E H -0.1846 0.2018 -0.0161 0.197 Uiso 1 1 calc R . . H32F H -0.1390 0.1920 0.0627 0.197 Uiso 1 1 calc R . . C33A C -0.220(2) 0.2945(10) 0.0484(10) 0.124(8) Uani 1 1 d . . . H33D H -0.2063 0.3346 0.0579 0.186 Uiso 1 1 calc R . . H33E H -0.2413 0.2758 0.0884 0.186 Uiso 1 1 calc R . . H33F H -0.2835 0.2899 0.0102 0.186 Uiso 1 1 calc R . . O4A O 0.6622(8) 0.4160(5) 0.1248(4) 0.060(3) Uani 1 1 d . . . N8A N 0.8161(11) 0.3935(6) 0.2090(5) 0.063(3) Uani 1 1 d . . . C34A C 0.6999(11) 0.3955(6) 0.1824(8) 0.056(4) Uani 1 1 d . . . H34A H 0.6442 0.3807 0.2084 0.067 Uiso 1 1 calc . . . C35A C 0.9049(14) 0.4185(8) 0.1727(7) 0.084(5) Uani 1 1 d . . . H35A H 0.9834 0.4133 0.1990 0.126 Uiso 1 1 calc R . . H35B H 0.8890 0.4588 0.1661 0.126 Uiso 1 1 calc R . . H35C H 0.9017 0.4001 0.1285 0.126 Uiso 1 1 calc R . . C36A C 0.8574(16) 0.3710(8) 0.2798(7) 0.087(5) Uani 1 1 d . . . H36A H 0.9436 0.3733 0.2898 0.131 Uiso 1 1 calc R . . H36B H 0.8326 0.3317 0.2824 0.131 Uiso 1 1 calc R . . H36C H 0.8225 0.3936 0.3128 0.131 Uiso 1 1 calc R . . O2A O 0.3036(10) 0.2957(5) 0.0318(5) 0.080(3) Uani 1 1 d . . . O3A O 0.4901(8) 0.3253(4) 0.0676(4) 0.046(2) Uani 1 1 d . . . C37A C 0.4621(15) 0.2266(6) 0.0428(7) 0.070(5) Uani 1 1 d . . . H37D H 0.3951 0.2015 0.0286 0.105 Uiso 1 1 calc R . . H37E H 0.5048 0.2139 0.0864 0.105 Uiso 1 1 calc R . . H37F H 0.5152 0.2260 0.0087 0.105 Uiso 1 1 calc R . . C38A C 0.4166(13) 0.2873(6) 0.0500(6) 0.048(3) Uani 1 1 d . . . O5A O 0.4221(9) 0.3940(4) 0.1694(4) 0.056(2) Uani 1 1 d . . . O6A O 0.2393(8) 0.3596(4) 0.1406(4) 0.060(3) Uani 1 1 d . . . C39A C 0.3165(16) 0.3635(7) 0.2597(6) 0.085(5) Uani 1 1 d . . . H39D H 0.2391 0.3474 0.2635 0.128 Uiso 1 1 calc R . . H39E H 0.3256 0.3996 0.2838 0.128 Uiso 1 1 calc R . . H39F H 0.3785 0.3375 0.2797 0.128 Uiso 1 1 calc R . . C40A C 0.3264(14) 0.3730(6) 0.1845(7) 0.054(4) Uani 1 1 d . . . N9 N 0.8080(13) 0.4265(8) 0.8683(8) 0.100(5) Uani 1 1 d . . . O15 O 0.8067(13) 0.4560(10) 0.9792(7) 0.174(9) Uani 1 1 d . . . C41 C 0.7984(17) 0.4663(10) 0.9148(7) 0.094(7) Uani 1 1 d . . . C42 C 0.8389(19) 0.3735(12) 0.8912(16) 0.197(16) Uani 1 1 d . . . H42D H 0.8419 0.3484 0.8526 0.295 Uiso 1 1 calc R . . H42E H 0.7804 0.3594 0.9181 0.295 Uiso 1 1 calc R . . H42F H 0.9166 0.3747 0.9194 0.295 Uiso 1 1 calc R . . C43 C 0.779(2) 0.4371(9) 0.7941(8) 0.127(9) Uani 1 1 d . . . H43D H 0.7912 0.4026 0.7693 0.191 Uiso 1 1 calc R . . H43E H 0.8302 0.4670 0.7811 0.191 Uiso 1 1 calc R . . H43F H 0.6963 0.4489 0.7831 0.191 Uiso 1 1 calc R . . O15A O 0.8614(14) 0.5606(8) 0.5188(12) 0.171(8) Uani 1 1 d . . . N9A N 0.9101(12) 0.6420(8) 0.4770(9) 0.088(4) Uani 1 1 d . . . C41A C 0.8729(17) 0.6093(10) 0.5242(13) 0.099(7) Uani 1 1 d . . . C42A C 0.9297(19) 0.7044(10) 0.4771(14) 0.156(11) Uani 1 1 d . . . H42A H 0.9566 0.7156 0.4348 0.234 Uiso 1 1 calc R . . H42B H 0.9896 0.7146 0.5155 0.234 Uiso 1 1 calc R . . H42C H 0.8556 0.7238 0.4810 0.234 Uiso 1 1 calc R . . C43A C 0.934(2) 0.6207(13) 0.4155(11) 0.158(11) Uani 1 1 d . . . H43A H 0.9590 0.6514 0.3881 0.237 Uiso 1 1 calc R . . H43B H 0.8631 0.6029 0.3911 0.237 Uiso 1 1 calc R . . H43C H 0.9976 0.5927 0.4240 0.237 Uiso 1 1 calc R . . O16 O 0.7713(16) 0.5326(9) 0.0593(9) 0.062(5) Uiso 0.50 1 d P . . H16B H 0.7719 0.5105 0.0267 0.092 Uiso 0.50 1 calc PR . . O17 O 0.741(4) 0.586(2) -0.016(2) 0.203(17) Uiso 0.50 1 d P . . C44 C 0.768(3) 0.5833(17) 0.0379(18) 0.078(9) Uiso 0.50 1 d P . . C45 C 0.758(3) 0.6314(15) 0.0786(16) 0.082(9) Uiso 0.50 1 d P . . H45A H 0.7717 0.6205 0.1265 0.124 Uiso 0.50 1 calc PR . . H45B H 0.6787 0.6475 0.0673 0.124 Uiso 0.50 1 calc PR . . H45C H 0.8167 0.6595 0.0703 0.124 Uiso 0.50 1 calc PR . . Cl1 Cl 0.5623(3) 0.23312(15) 0.82775(14) 0.0551(9) Uani 1 1 d D . . O7 O 0.4458(11) 0.2135(9) 0.8300(7) 0.169(8) Uani 1 1 d D . . O8 O 0.6300(11) 0.1879(5) 0.8079(5) 0.097(4) Uani 1 1 d D . . O9 O 0.6141(13) 0.2499(6) 0.8947(4) 0.118(5) Uani 1 1 d D . . O10 O 0.5650(15) 0.2769(4) 0.7805(5) 0.124(6) Uani 1 1 d D . . Cl2 Cl 0.2491(3) 0.62877(18) 0.82294(15) 0.0592(10) Uani 1 1 d D . . O11 O 0.1576(10) 0.5936(6) 0.7914(7) 0.153(6) Uani 1 1 d D . . O12 O 0.2614(15) 0.6169(6) 0.8920(5) 0.193(9) Uani 1 1 d D . . O13 O 0.3526(9) 0.6159(5) 0.7968(7) 0.128(5) Uani 1 1 d D . . O14 O 0.2141(9) 0.6847(5) 0.8088(6) 0.112(5) Uani 1 1 d D . . Cl1A Cl 0.3570(3) 0.41415(14) 0.65732(13) 0.0441(7) Uani 1 1 d D . . O7A O 0.3074(11) 0.3984(6) 0.5888(4) 0.107(4) Uani 1 1 d D . . O8A O 0.3329(9) 0.3704(4) 0.7051(4) 0.069(3) Uani 1 1 d D . . O9A O 0.3057(9) 0.4673(4) 0.6745(5) 0.071(3) Uani 1 1 d D . . O10A O 0.4827(8) 0.4222(5) 0.6609(6) 0.095(4) Uani 1 1 d D . . Cl2A Cl 0.1641(4) 0.50876(18) 0.31313(19) 0.0695(10) Uiso 1 1 d D . . O11A O 0.1653(17) 0.5168(10) 0.2404(7) 0.142(9) Uiso 0.60 1 d PD A . O12A O 0.0815(14) 0.5470(7) 0.3360(8) 0.086(6) Uiso 0.60 1 d PD A . O13A O 0.1216(16) 0.4510(6) 0.3199(10) 0.109(7) Uiso 0.60 1 d PD A . O14A O 0.2807(11) 0.5163(7) 0.3473(7) 0.067(4) Uiso 0.60 1 d PD A . O11B O 0.234(2) 0.4960(12) 0.3781(9) 0.088(8) Uiso 0.40 1 d PD A 1 O12B O 0.163(3) 0.4606(11) 0.2683(12) 0.107(10) Uiso 0.40 1 d PD A 1 O13B O 0.160(3) 0.5603(19) 0.2734(19) 0.134(13) Uiso 0.40 1 d P A 1 O14B O 0.056(5) 0.512(3) 0.328(3) 0.18(2) Uiso 0.40 1 d P A 1 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 Cu1 0.0413(8) 0.0217(8) 0.0317(7) -0.0017(6) -0.0004(6) -0.0031(7) Cu2 0.0362(7) 0.0332(8) 0.0288(6) -0.0040(7) 0.0047(5) -0.0043(7) N1 0.031(5) 0.022(5) 0.028(4) 0.005(4) -0.001(3) 0.001(4) C1 0.026(5) 0.022(7) 0.050(6) -0.007(6) 0.006(5) -0.008(5) C2 0.065(9) 0.040(9) 0.047(7) -0.013(6) 0.017(6) -0.012(7) C3 0.043(7) 0.045(9) 0.047(7) -0.013(7) 0.006(6) -0.011(6) C4 0.053(8) 0.032(8) 0.040(7) 0.017(6) 0.007(5) 0.009(6) C5 0.038(7) 0.028(7) 0.056(8) 0.001(6) -0.006(6) 0.011(6) C6 0.055(8) 0.040(9) 0.048(7) 0.017(7) 0.009(6) -0.005(7) C7 0.082(10) 0.023(7) 0.062(8) 0.005(7) 0.036(7) -0.001(7) C8 0.076(9) 0.026(8) 0.047(7) -0.014(6) 0.012(6) 0.011(7) N2 0.054(6) 0.037(7) 0.037(5) 0.003(5) 0.010(5) 0.013(5) N3 0.061(7) 0.032(6) 0.040(6) -0.003(5) 0.014(5) 0.002(5) C9 0.066(9) 0.032(8) 0.052(8) -0.019(7) 0.004(6) -0.005(7) C10 0.075(10) 0.037(8) 0.044(8) -0.027(7) -0.008(7) -0.020(7) C11 0.066(11) 0.052(10) 0.101(12) -0.008(9) 0.004(9) 0.001(8) C12 0.082(13) 0.059(12) 0.113(15) -0.032(11) -0.001(11) -0.007(10) C13 0.108(16) 0.082(15) 0.108(16) -0.016(13) -0.032(13) -0.041(13) C14 0.120(16) 0.096(16) 0.057(10) -0.007(10) -0.012(10) -0.005(13) C15 0.074(11) 0.053(10) 0.083(11) -0.020(9) -0.010(9) -0.002(8) N4 0.039(6) 0.056(8) 0.035(5) -0.004(5) 0.008(4) 0.004(5) C16 0.037(7) 0.027(7) 0.037(6) -0.008(6) -0.002(5) 0.008(5) C17 0.056(8) 0.050(9) 0.035(7) -0.012(6) 0.003(5) 0.019(7) C18 0.080(10) 0.044(9) 0.041(7) -0.015(7) -0.010(6) 0.006(8) C19 0.053(8) 0.044(8) 0.041(7) 0.011(7) 0.001(6) 0.006(7) C20 0.055(8) 0.038(8) 0.026(6) -0.007(6) -0.004(5) 0.007(6) C21 0.027(6) 0.028(7) 0.042(6) 0.005(6) -0.002(5) -0.009(5) C22 0.053(8) 0.064(10) 0.031(6) 0.014(7) 0.008(6) -0.003(7) C23 0.042(7) 0.084(11) 0.020(5) 0.002(7) -0.003(5) 0.021(8) N5 0.025(5) 0.035(6) 0.030(5) -0.008(4) 0.001(4) 0.002(4) N6 0.059(6) 0.051(7) 0.031(5) -0.009(6) 0.008(4) -0.006(6) C24 0.056(8) 0.048(9) 0.029(6) -0.003(6) 0.015(6) 0.006(7) C25 0.060(9) 0.041(9) 0.050(7) -0.011(7) 0.013(6) 0.010(7) C26 0.034(8) 0.070(11) 0.054(8) -0.002(7) -0.003(6) 0.005(7) C27 0.034(8) 0.071(12) 0.084(10) -0.002(9) 0.001(6) -0.003(8) C28 0.078(11) 0.069(12) 0.055(8) -0.036(9) 0.013(7) -0.035(10) C29 0.073(11) 0.063(11) 0.081(10) 0.002(9) 0.029(9) 0.002(10) C30 0.068(10) 0.066(11) 0.053(8) -0.006(8) 0.023(7) -0.007(9) O1 0.044(5) 0.024(4) 0.058(5) -0.011(4) -0.009(4) 0.000(4) N7 0.034(6) 0.069(9) 0.041(5) 0.008(5) -0.004(4) -0.008(5) C31 0.055(8) 0.035(8) 0.028(6) 0.014(6) -0.012(5) -0.014(6) C32 0.084(11) 0.063(11) 0.062(9) 0.011(8) -0.020(7) -0.009(9) C33 0.079(12) 0.112(16) 0.069(9) 0.012(11) -0.025(8) 0.016(11) O4 0.049(5) 0.030(5) 0.051(5) -0.003(4) 0.011(4) -0.019(4) N8 0.057(7) 0.052(8) 0.064(7) 0.001(6) 0.016(5) -0.022(7) C34 0.064(9) 0.069(11) 0.022(6) -0.002(7) -0.002(5) -0.023(8) C35 0.085(14) 0.094(16) 0.158(18) 0.017(14) 0.020(13) -0.021(12) C36 0.158(19) 0.103(16) 0.079(11) -0.017(11) 0.035(11) -0.090(15) O2 0.047(5) 0.030(5) 0.035(4) -0.004(4) 0.010(3) -0.008(4) O3 0.060(5) 0.028(5) 0.034(4) 0.003(4) 0.015(4) 0.004(4) C37 0.093(10) 0.028(7) 0.026(5) 0.015(5) 0.018(6) 0.020(7) C38 0.052(7) 0.025(7) 0.023(5) -0.009(5) -0.011(5) 0.009(6) O5 0.045(5) 0.028(5) 0.038(4) -0.009(4) 0.009(4) -0.005(4) O6 0.033(4) 0.018(4) 0.041(4) 0.001(4) -0.002(3) -0.009(4) C39 0.061(8) 0.023(7) 0.038(6) -0.007(6) 0.019(5) 0.001(6) C40 0.064(9) 0.033(7) 0.014(5) 0.014(5) 0.012(5) 0.005(7) Cu1A 0.0510(10) 0.0939(16) 0.0403(8) -0.0087(10) 0.0154(7) -0.0101(10) Cu2A 0.0528(9) 0.0328(9) 0.0374(7) -0.0024(7) 0.0003(6) -0.0037(7) N1A 0.042(8) 0.150(17) 0.096(10) 0.049(12) 0.036(7) -0.009(9) C1A 0.097(15) 0.12(2) 0.128(18) 0.047(17) 0.058(14) -0.009(14) C2A 0.16(2) 0.074(17) 0.15(2) 0.057(16) 0.042(18) 0.036(15) C3A 0.23(4) 0.12(3) 0.19(3) 0.04(3) 0.10(3) 0.03(3) C4A 0.113(19) 0.09(2) 0.22(3) 0.01(2) 0.036(19) -0.034(16) C5A 0.104(18) 0.083(18) 0.22(3) 0.026(19) 0.060(18) -0.033(14) C6A 0.058(13) 0.28(4) 0.082(15) 0.02(2) 0.041(11) -0.022(18) C7A 0.15(2) 0.22(3) 0.088(15) 0.075(18) 0.076(15) 0.02(2) C8A 0.052(10) 0.25(3) 0.035(8) 0.002(15) 0.021(7) -0.009(14) N2A 0.035(8) 0.22(2) 0.060(9) -0.015(12) 0.022(6) 0.009(10) N3A 0.049(8) 0.135(16) 0.087(11) 0.015(12) -0.006(7) -0.001(9) C9A 0.059(11) 0.125(18) 0.102(13) -0.076(13) -0.017(9) 0.007(12) C10A 0.059(12) 0.34(4) 0.096(14) -0.10(2) 0.017(10) -0.017(18) C11A 0.101(19) 0.68(9) 0.107(17) -0.14(3) 0.029(15) -0.09(4) C12A 0.15(3) 0.40(6) 0.092(16) -0.05(3) 0.046(16) -0.08(3) C13A 0.17(3) 0.21(3) 0.111(18) 0.03(2) -0.073(18) 0.04(2) C14A 0.14(3) 0.31(5) 0.32(4) -0.19(4) -0.09(3) 0.13(3) C15A 0.13(2) 0.39(6) 0.24(3) -0.20(4) -0.10(2) 0.06(3) N4A 0.047(6) 0.034(7) 0.048(6) -0.004(5) 0.002(5) -0.016(5) C16A 0.075(10) 0.060(11) 0.041(7) 0.000(7) 0.015(6) -0.006(8) C17A 0.084(10) 0.061(11) 0.028(6) -0.003(7) 0.003(6) -0.012(8) C18A 0.105(13) 0.054(11) 0.050(8) -0.004(8) -0.005(8) -0.023(9) C19A 0.115(14) 0.050(10) 0.059(9) 0.009(9) -0.004(9) -0.007(10) C20A 0.095(12) 0.047(11) 0.053(9) 0.005(8) -0.011(8) -0.002(9) C21A 0.075(11) 0.039(10) 0.099(13) -0.008(10) -0.006(9) -0.002(8) C22A 0.138(16) 0.033(10) 0.091(13) 0.006(10) -0.007(11) -0.008(10) C23A 0.105(15) 0.049(12) 0.148(19) -0.040(13) 0.019(13) 0.022(10) N5A 0.068(7) 0.025(6) 0.047(6) -0.011(5) -0.004(5) -0.006(5) N6A 0.070(8) 0.041(8) 0.072(8) -0.021(7) -0.003(6) 0.002(6) C24A 0.103(13) 0.080(12) 0.047(8) -0.028(8) 0.005(8) 0.028(10) C25A 0.063(10) 0.062(11) 0.075(10) -0.032(9) 0.014(8) -0.014(8) C26A 0.117(18) 0.090(16) 0.108(15) -0.003(12) 0.016(13) -0.044(13) C27A 0.080(14) 0.13(2) 0.130(18) -0.078(17) 0.010(13) -0.022(13) C28A 0.099(16) 0.13(2) 0.076(12) -0.037(13) -0.023(12) 0.026(14) C29A 0.051(11) 0.16(2) 0.109(14) -0.052(14) 0.016(10) 0.010(13) C30A 0.083(12) 0.055(10) 0.066(9) -0.014(8) 0.032(8) 0.006(8) O1A 0.26(2) 0.142(17) 0.070(9) -0.008(10) -0.008(11) 0.089(16) N7A 0.103(12) 0.083(12) 0.060(8) 0.022(8) -0.016(7) -0.052(10) C31A 0.102(14) 0.12(2) 0.070(11) 0.015(13) 0.054(10) 0.088(15) C32A 0.121(18) 0.12(2) 0.17(2) 0.061(18) 0.072(15) 0.035(16) C33A 0.18(2) 0.091(17) 0.088(14) -0.008(12) -0.026(14) 0.014(17) O4A 0.061(6) 0.087(8) 0.028(4) 0.010(5) -0.011(4) -0.009(6) N8A 0.066(8) 0.073(10) 0.048(6) -0.001(6) -0.003(6) -0.013(7) C34A 0.031(7) 0.043(9) 0.095(11) -0.029(8) 0.016(7) -0.005(6) C35A 0.079(11) 0.108(16) 0.068(9) -0.006(10) 0.019(8) -0.029(11) C36A 0.125(14) 0.070(12) 0.062(9) 0.021(9) -0.004(9) -0.029(11) O2A 0.075(8) 0.080(8) 0.087(7) -0.030(6) 0.021(6) -0.036(6) O3A 0.066(6) 0.033(5) 0.038(5) -0.001(4) 0.003(4) -0.008(5) C37A 0.125(14) 0.030(9) 0.064(9) -0.002(7) 0.044(9) -0.009(9) C38A 0.052(9) 0.060(10) 0.034(7) -0.010(7) 0.015(6) -0.016(8) O5A 0.075(7) 0.052(6) 0.037(5) -0.009(4) 0.000(4) 0.008(5) O6A 0.079(6) 0.068(7) 0.034(4) 0.000(5) 0.010(4) -0.028(6) C39A 0.155(16) 0.071(12) 0.032(7) 0.012(8) 0.020(8) -0.016(12) C40A 0.071(10) 0.044(9) 0.052(8) 0.002(7) 0.023(8) 0.017(8) N9 0.088(11) 0.108(15) 0.103(12) 0.038(11) 0.012(9) 0.007(10) O15 0.116(12) 0.31(3) 0.092(10) 0.046(13) 0.000(8) -0.042(14) C41 0.120(15) 0.136(19) 0.028(7) -0.003(10) 0.022(8) -0.031(13) C42 0.080(15) 0.15(2) 0.35(4) 0.16(3) -0.007(19) -0.004(15) C43 0.23(3) 0.092(16) 0.073(11) -0.003(11) 0.083(14) 0.007(16) O15A 0.105(12) 0.079(12) 0.33(3) 0.021(15) 0.040(13) 0.008(10) N9A 0.060(9) 0.087(12) 0.111(12) -0.022(11) -0.010(8) -0.002(8) C41A 0.077(13) 0.057(13) 0.17(2) 0.023(14) 0.026(13) 0.012(11) C42A 0.093(15) 0.086(17) 0.26(3) -0.075(19) -0.052(16) 0.002(13) C43A 0.122(19) 0.23(3) 0.113(17) -0.07(2) -0.004(14) -0.027(19) Cl1 0.081(2) 0.055(2) 0.0304(15) -0.0012(15) 0.0138(15) 0.0064(19) O7 0.076(9) 0.29(2) 0.147(12) -0.065(14) 0.043(8) -0.059(12) O8 0.142(11) 0.081(9) 0.087(7) 0.033(7) 0.078(7) 0.054(8) O9 0.220(14) 0.106(11) 0.024(5) -0.001(6) 0.011(6) -0.016(10) O10 0.282(18) 0.050(7) 0.047(6) 0.016(5) 0.046(8) 0.051(9) Cl2 0.066(2) 0.075(3) 0.0381(17) 0.0166(18) 0.0132(15) 0.007(2) O11 0.090(10) 0.166(17) 0.204(16) -0.037(13) 0.030(10) -0.042(11) O12 0.34(3) 0.178(18) 0.077(9) 0.062(10) 0.083(12) 0.122(17) O13 0.088(9) 0.120(12) 0.190(14) 0.042(10) 0.065(9) 0.044(8) O14 0.062(7) 0.107(11) 0.172(12) 0.052(9) 0.033(7) 0.045(7) Cl1A 0.0542(19) 0.042(2) 0.0389(15) 0.0071(15) 0.0157(13) -0.0011(16) O7A 0.150(11) 0.131(12) 0.042(5) -0.006(7) 0.025(6) -0.023(9) O8A 0.112(8) 0.046(6) 0.056(5) 0.017(5) 0.032(5) -0.003(6) O9A 0.081(7) 0.043(6) 0.088(7) 0.018(5) 0.010(5) 0.023(5) O10A 0.066(7) 0.074(9) 0.150(10) 0.038(8) 0.039(7) 0.020(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.939(7) . ? Cu1 O6 1.946(8) . ? Cu1 N2 2.028(11) . ? Cu1 N1 2.037(8) . ? Cu1 O1 2.183(7) . ? Cu2 O5 1.941(8) . ? Cu2 O3 1.980(7) . ? Cu2 N5 2.010(8) . ? Cu2 N4 2.017(11) . ? Cu2 O4 2.135(8) . ? N1 C1 1.335(13) . ? N1 C5 1.336(14) . ? C1 C2 1.373(15) . ? C2 C3 1.376(17) . ? C3 C4 1.364(16) . ? C4 C5 1.366(15) . ? C5 C6 1.492(17) . ? C6 N2 1.313(14) . ? C6 C7 1.365(17) . ? C7 C8 1.362(16) . ? C8 N3 1.322(15) . ? N2 N3 1.356(13) . ? N3 C9 1.450(14) . ? C9 C10 1.505(17) . ? C10 C11 1.343(19) . ? C10 C15 1.353(19) . ? C11 C12 1.38(2) . ? C12 C13 1.32(2) . ? C13 C14 1.40(3) . ? C14 C15 1.42(2) . ? N4 C16 1.300(13) . ? N4 C20 1.351(14) . ? C16 C17 1.389(17) . ? C17 C18 1.362(16) . ? C18 C19 1.365(16) . ? C19 C20 1.365(17) . ? C20 C21 1.459(15) . ? C21 N5 1.348(14) . ? C21 C22 1.360(14) . ? C22 C23 1.358(19) . ? C23 N6 1.364(16) . ? N5 N6 1.374(11) . ? N6 C24 1.422(16) . ? C24 C25 1.533(18) . ? C25 C30 1.378(19) . ? C25 C26 1.380(17) . ? C26 C27 1.324(18) . ? C27 C28 1.42(2) . ? C28 C29 1.32(2) . ? C29 C30 1.353(19) . ? O1 C31 1.235(11) . ? N7 C31 1.322(14) . ? N7 C33 1.433(18) . ? N7 C32 1.473(14) . ? O4 C34 1.192(15) . ? N8 C34 1.302(16) . ? N8 C35 1.38(2) . ? N8 C36 1.50(2) . ? O2 C38 1.240(13) . ? O3 C38 1.262(13) . ? C37 C38 1.548(13) . ? O5 C40 1.291(14) . ? O6 C40 1.246(14) . ? C39 C40 1.485(16) . ? Cu1A O2A 1.919(12) . ? Cu1A O6A 1.960(8) . ? Cu1A N1A 2.001(19) . ? Cu1A N2A 2.075(16) . ? Cu1A O1A 2.34(3) . ? Cu2A O3A 1.932(9) . ? Cu2A O5A 1.946(9) . ? Cu2A N4A 2.010(10) . ? Cu2A N5A 2.018(11) . ? Cu2A O4A 2.176(8) . ? N1A C5A 1.32(3) . ? N1A C1A 1.34(2) . ? C1A C6A 1.33(3) . ? C1A C2A 1.46(3) . ? C2A C3A 1.31(3) . ? C3A C4A 1.25(3) . ? C4A C5A 1.44(3) . ? C6A N2A 1.39(4) . ? C6A C7A 1.42(3) . ? C7A C8A 1.35(3) . ? C8A N3A 1.29(3) . ? N2A N3A 1.29(2) . ? N3A C9A 1.45(2) . ? C9A C10A 1.59(2) . ? C10A C11A 1.3900 . ? C10A C15A 1.3900 . ? C11A C12A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? N4A C20A 1.326(17) . ? N4A C16A 1.348(15) . ? C16A C17A 1.369(16) . ? C17A C18A 1.41(2) . ? C18A C19A 1.35(2) . ? C19A C20A 1.359(18) . ? C20A C21A 1.48(2) . ? C21A N5A 1.339(18) . ? C21A C22A 1.38(2) . ? C22A C23A 1.38(2) . ? C23A N6A 1.36(2) . ? N5A N6A 1.381(14) . ? N6A C24A 1.407(17) . ? C24A C25A 1.50(2) . ? C25A C30A 1.39(2) . ? C25A C26A 1.40(2) . ? C26A C27A 1.39(3) . ? C27A C28A 1.36(3) . ? C28A C29A 1.35(3) . ? C29A C30A 1.40(2) . ? O1A C31A 0.89(2) . ? N7A C33A 1.39(2) . ? N7A C32A 1.40(3) . ? N7A C31A 1.78(3) . ? O4A C34A 1.239(16) . ? N8A C34A 1.330(16) . ? N8A C35A 1.434(17) . ? N8A C36A 1.487(16) . ? O2A C38A 1.280(16) . ? O3A C38A 1.224(15) . ? C37A C38A 1.514(19) . ? O5A C40A 1.256(16) . ? O6A C40A 1.240(16) . ? C39A C40A 1.510(16) . ? N9 C41 1.31(2) . ? N9 C42 1.34(3) . ? N9 C43 1.46(2) . ? O15 C41 1.274(17) . ? O15A C41A 1.14(2) . ? N9A C41A 1.31(2) . ? N9A C43A 1.37(2) . ? N9A C42A 1.47(3) . ? O16 C44 1.25(4) . ? O17 C44 1.05(4) . ? C44 C45 1.39(4) . ? Cl1 O10 1.378(9) . ? Cl1 O8 1.388(9) . ? Cl1 O7 1.393(11) . ? Cl1 O9 1.405(9) . ? Cl2 O12 1.366(9) . ? Cl2 O13 1.373(9) . ? Cl2 O14 1.374(9) . ? Cl2 O11 1.384(10) . ? Cl1A O10A 1.416(9) . ? Cl1A O7A 1.420(9) . ? Cl1A O9A 1.426(8) . ? Cl1A O8A 1.436(8) . ? Cl2A O14B 1.29(5) . ? Cl2A O14A 1.389(11) . ? Cl2A O12A 1.406(13) . ? Cl2A O11B 1.419(15) . ? Cl2A O12B 1.423(15) . ? Cl2A O13B 1.42(4) . ? Cl2A O13A 1.438(14) . ? Cl2A O11A 1.438(14) . ? O11A O13B 1.21(4) . ? O11A O12B 1.42(3) . ? O12A O14B 0.86(6) . ? O12A O13B 1.64(4) . ? O13A O12B 1.19(3) . ? O13A O14B 1.62(6) . ? O14A O11B 0.98(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O6 91.6(3) . . ? O2 Cu1 N2 95.2(4) . . ? O6 Cu1 N2 169.7(3) . . ? O2 Cu1 N1 170.8(3) . . ? O6 Cu1 N1 92.0(3) . . ? N2 Cu1 N1 80.1(4) . . ? O2 Cu1 O1 89.7(3) . . ? O6 Cu1 O1 90.7(3) . . ? N2 Cu1 O1 96.9(4) . . ? N1 Cu1 O1 98.7(3) . . ? O5 Cu2 O3 89.3(3) . . ? O5 Cu2 N5 95.7(3) . . ? O3 Cu2 N5 165.2(4) . . ? O5 Cu2 N4 168.7(4) . . ? O3 Cu2 N4 92.6(3) . . ? N5 Cu2 N4 79.9(4) . . ? O5 Cu2 O4 94.6(3) . . ? O3 Cu2 O4 92.5(3) . . ? N5 Cu2 O4 100.9(3) . . ? N4 Cu2 O4 96.4(4) . . ? C1 N1 C5 117.8(9) . . ? C1 N1 Cu1 126.9(7) . . ? C5 N1 Cu1 115.4(8) . . ? N1 C1 C2 123.3(11) . . ? C1 C2 C3 118.2(12) . . ? C4 C3 C2 118.6(11) . . ? C3 C4 C5 120.2(12) . . ? N1 C5 C4 121.8(11) . . ? N1 C5 C6 113.0(10) . . ? C4 C5 C6 125.2(11) . . ? N2 C6 C7 111.7(12) . . ? N2 C6 C5 117.2(11) . . ? C7 C6 C5 131.1(11) . . ? C8 C7 C6 104.1(11) . . ? N3 C8 C7 109.1(11) . . ? C6 N2 N3 105.8(10) . . ? C6 N2 Cu1 114.1(8) . . ? N3 N2 Cu1 139.9(7) . . ? C8 N3 N2 109.3(9) . . ? C8 N3 C9 127.4(11) . . ? N2 N3 C9 122.4(10) . . ? N3 C9 C10 111.8(11) . . ? C11 C10 C15 118.5(14) . . ? C11 C10 C9 125.5(13) . . ? C15 C10 C9 116.0(13) . . ? C10 C11 C12 122.5(17) . . ? C13 C12 C11 118.7(19) . . ? C12 C13 C14 122.8(18) . . ? C13 C14 C15 115.5(17) . . ? C10 C15 C14 121.7(17) . . ? C16 N4 C20 118.9(11) . . ? C16 N4 Cu2 126.2(8) . . ? C20 N4 Cu2 114.6(7) . . ? N4 C16 C17 123.5(11) . . ? C18 C17 C16 116.9(11) . . ? C17 C18 C19 120.6(13) . . ? C18 C19 C20 119.0(12) . . ? N4 C20 C19 121.1(10) . . ? N4 C20 C21 115.3(10) . . ? C19 C20 C21 123.6(11) . . ? N5 C21 C22 112.4(11) . . ? N5 C21 C20 114.0(9) . . ? C22 C21 C20 133.6(12) . . ? C23 C22 C21 105.4(12) . . ? C22 C23 N6 108.3(10) . . ? C21 N5 N6 104.2(9) . . ? C21 N5 Cu2 115.6(7) . . ? N6 N5 Cu2 139.7(8) . . ? C23 N6 N5 109.7(10) . . ? C23 N6 C24 126.5(10) . . ? N5 N6 C24 123.5(10) . . ? N6 C24 C25 112.7(10) . . ? C30 C25 C26 116.1(14) . . ? C30 C25 C24 120.1(12) . . ? C26 C25 C24 123.8(12) . . ? C27 C26 C25 123.2(15) . . ? C26 C27 C28 118.2(14) . . ? C29 C28 C27 119.8(15) . . ? C28 C29 C30 120.3(17) . . ? C29 C30 C25 122.1(15) . . ? C31 O1 Cu1 120.1(7) . . ? C31 N7 C33 120.4(10) . . ? C31 N7 C32 122.3(10) . . ? C33 N7 C32 116.6(10) . . ? O1 C31 N7 124.4(11) . . ? C34 O4 Cu2 127.9(9) . . ? C34 N8 C35 122.0(14) . . ? C34 N8 C36 120.7(14) . . ? C35 N8 C36 117.3(14) . . ? O4 C34 N8 129.9(14) . . ? C38 O2 Cu1 130.5(7) . . ? C38 O3 Cu2 120.8(7) . . ? O2 C38 O3 130.0(9) . . ? O2 C38 C37 115.0(10) . . ? O3 C38 C37 115.0(11) . . ? C40 O5 Cu2 124.5(7) . . ? C40 O6 Cu1 135.5(8) . . ? O6 C40 O5 124.3(11) . . ? O6 C40 C39 119.2(11) . . ? O5 C40 C39 116.5(11) . . ? O2A Cu1A O6A 91.6(4) . . ? O2A Cu1A N1A 165.4(4) . . ? O6A Cu1A N1A 92.4(5) . . ? O2A Cu1A N2A 96.3(7) . . ? O6A Cu1A N2A 168.3(7) . . ? N1A Cu1A N2A 77.8(8) . . ? O2A Cu1A O1A 101.0(5) . . ? O6A Cu1A O1A 88.5(4) . . ? N1A Cu1A O1A 93.1(6) . . ? N2A Cu1A O1A 98.4(5) . . ? O3A Cu2A O5A 90.4(4) . . ? O3A Cu2A N4A 93.3(4) . . ? O5A Cu2A N4A 167.0(4) . . ? O3A Cu2A N5A 171.7(4) . . ? O5A Cu2A N5A 95.1(4) . . ? N4A Cu2A N5A 80.1(4) . . ? O3A Cu2A O4A 92.2(4) . . ? O5A Cu2A O4A 93.4(3) . . ? N4A Cu2A O4A 99.0(3) . . ? N5A Cu2A O4A 93.8(4) . . ? C5A N1A C1A 120(2) . . ? C5A N1A Cu1A 122.1(15) . . ? C1A N1A Cu1A 118.2(16) . . ? C6A C1A N1A 113(2) . . ? C6A C1A C2A 129(3) . . ? N1A C1A C2A 117(2) . . ? C3A C2A C1A 123(3) . . ? C4A C3A C2A 117(3) . . ? C3A C4A C5A 125(3) . . ? N1A C5A C4A 118(3) . . ? C1A C6A N2A 120(2) . . ? C1A C6A C7A 130(4) . . ? N2A C6A C7A 109(3) . . ? C8A C7A C6A 102(3) . . ? N3A C8A C7A 111.5(17) . . ? N3A N2A C6A 104(2) . . ? N3A N2A Cu1A 145.2(19) . . ? C6A N2A Cu1A 110.3(14) . . ? C8A N3A N2A 113(2) . . ? C8A N3A C9A 132(2) . . ? N2A N3A C9A 115.1(19) . . ? N3A C9A C10A 120.4(15) . . ? C11A C10A C15A 120.0 . . ? C11A C10A C9A 113.6(14) . . ? C15A C10A C9A 126.4(14) . . ? C10A C11A C12A 120.0 . . ? C11A C12A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C13A C14A C15A 120.0 . . ? C14A C15A C10A 120.0 . . ? C20A N4A C16A 117.9(11) . . ? C20A N4A Cu2A 116.6(9) . . ? C16A N4A Cu2A 125.3(9) . . ? N4A C16A C17A 122.3(14) . . ? C16A C17A C18A 118.5(14) . . ? C19A C18A C17A 117.6(13) . . ? C18A C19A C20A 120.9(16) . . ? N4A C20A C19A 122.6(15) . . ? N4A C20A C21A 112.8(12) . . ? C19A C20A C21A 124.5(15) . . ? N5A C21A C22A 111.4(15) . . ? N5A C21A C20A 116.5(13) . . ? C22A C21A C20A 131.9(17) . . ? C21A C22A C23A 104.6(16) . . ? N6A C23A C22A 109.4(15) . . ? C21A N5A N6A 106.5(11) . . ? C21A N5A Cu2A 113.7(9) . . ? N6A N5A Cu2A 139.8(9) . . ? C23A N6A N5A 108.0(13) . . ? C23A N6A C24A 128.6(14) . . ? N5A N6A C24A 123.0(12) . . ? N6A C24A C25A 115.6(13) . . ? C30A C25A C26A 117.4(16) . . ? C30A C25A C24A 119.5(14) . . ? C26A C25A C24A 123.0(17) . . ? C27A C26A C25A 119.0(19) . . ? C28A C27A C26A 119(2) . . ? C29A C28A C27A 126(2) . . ? C28A C29A C30A 114(2) . . ? C25A C30A C29A 124.7(16) . . ? C31A O1A Cu1A 97(3) . . ? C33A N7A C32A 114.1(16) . . ? C33A N7A C31A 137.5(17) . . ? C32A N7A C31A 107.9(17) . . ? O1A C31A N7A 91(2) . . ? C34A O4A Cu2A 120.4(8) . . ? C34A N8A C35A 120.4(12) . . ? C34A N8A C36A 121.8(13) . . ? C35A N8A C36A 117.6(12) . . ? O4A C34A N8A 123.4(12) . . ? C38A O2A Cu1A 128.4(9) . . ? C38A O3A Cu2A 132.4(10) . . ? O3A C38A O2A 124.5(14) . . ? O3A C38A C37A 118.5(14) . . ? O2A C38A C37A 116.8(14) . . ? C40A O5A Cu2A 130.8(8) . . ? C40A O6A Cu1A 131.8(8) . . ? O6A C40A O5A 123.2(11) . . ? O6A C40A C39A 118.2(13) . . ? O5A C40A C39A 118.6(14) . . ? C41 N9 C42 117(2) . . ? C41 N9 C43 122.6(17) . . ? C42 N9 C43 120(2) . . ? O15 C41 N9 123(2) . . ? C41A N9A C43A 122(2) . . ? C41A N9A C42A 129(2) . . ? C43A N9A C42A 108(2) . . ? O15A C41A N9A 123(3) . . ? O17 C44 O16 113(5) . . ? O17 C44 C45 119(5) . . ? O16 C44 C45 125(3) . . ? O10 Cl1 O8 107.6(6) . . ? O10 Cl1 O7 112.3(11) . . ? O8 Cl1 O7 108.5(10) . . ? O10 Cl1 O9 111.9(8) . . ? O8 Cl1 O9 107.7(9) . . ? O7 Cl1 O9 108.6(8) . . ? O12 Cl2 O13 111.1(8) . . ? O12 Cl2 O14 111.9(8) . . ? O13 Cl2 O14 111.4(6) . . ? O12 Cl2 O11 106.2(8) . . ? O13 Cl2 O11 108.5(8) . . ? O14 Cl2 O11 107.4(7) . . ? O10A Cl1A O7A 109.0(7) . . ? O10A Cl1A O9A 108.0(7) . . ? O7A Cl1A O9A 109.4(7) . . ? O10A Cl1A O8A 110.2(6) . . ? O7A Cl1A O8A 110.3(7) . . ? O9A Cl1A O8A 109.8(6) . . ? O14B Cl2A O14A 137(2) . . ? O14B Cl2A O12A 37(3) . . ? O14A Cl2A O12A 112.7(8) . . ? O14B Cl2A O11B 103(3) . . ? O14A Cl2A O11B 40.9(11) . . ? O12A Cl2A O11B 98.4(12) . . ? O14B Cl2A O12B 105(3) . . ? O14A Cl2A O12B 108.5(14) . . ? O12A Cl2A O12B 138.6(14) . . ? O11B Cl2A O12B 109.9(13) . . ? O14B Cl2A O13B 97(3) . . ? O14A Cl2A O13B 96.1(17) . . ? O12A Cl2A O13B 71.0(16) . . ? O11B Cl2A O13B 129(2) . . ? O12B Cl2A O13B 109.2(19) . . ? O14B Cl2A O13A 73(3) . . ? O14A Cl2A O13A 112.1(8) . . ? O12A Cl2A O13A 108.5(9) . . ? O11B Cl2A O13A 82.4(13) . . ? O12B Cl2A O13A 49.4(12) . . ? O13B Cl2A O13A 148.4(17) . . ? O14B Cl2A O11A 111(2) . . ? O14A Cl2A O11A 108.2(8) . . ? O12A Cl2A O11A 109.8(9) . . ? O11B Cl2A O11A 145.9(13) . . ? O12B Cl2A O11A 59.4(13) . . ? O13B Cl2A O11A 49.8(15) . . ? O13A Cl2A O11A 105.4(9) . . ? O13B O11A O12B 124(2) . . ? O13B O11A Cl2A 64(2) . . ? O12B O11A Cl2A 59.7(8) . . ? O14B O12A Cl2A 64(4) . . ? O14B O12A O13B 104(4) . . ? Cl2A O12A O13B 55.0(15) . . ? O12B O13A Cl2A 64.7(10) . . ? O12B O13A O14B 99(2) . . ? Cl2A O13A O14B 50(2) . . ? O11B O14A Cl2A 71.2(11) . . ? O14A O11B Cl2A 67.9(10) . . ? O13A O12B O11A 121.9(17) . . ? O13A O12B Cl2A 66.0(9) . . ? O11A O12B Cl2A 60.8(10) . . ? O11A O13B Cl2A 66(2) . . ? O11A O13B O12A 109(3) . . ? Cl2A O13B O12A 54.0(14) . . ? O12A O14B Cl2A 79(4) . . ? O12A O14B O13A 134(5) . . ? Cl2A O14B O13A 58(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.827 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.094 #=END