# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_email LINDOY@GMAIL.COM _publ_section_title ; Interaction of an extended series of N-substituted di(2-picolyl)amine derivatives with copper(II). Synthetic, structural, magnetic and solution studies ; loop_ _publ_author_name 'Leonard Lindoy' 'Bianca Antonioli' 'Bernd Buchner' 'Jack K. Clegg' 'Kerstin Gloe' 'Karsten Gloe' ; L.Gotzke ; 'Axel Heine' 'Anne Jager' 'Katrina A. Jolliffe' 'Vladislav Kataev' 'Olga Kataeva' 'Ruediger Klingeler' ; T.Krause ; 'Andreia Popa' 'Wilhelm Seichter' 'Marco Wenzel' # Attachment 'Cu2an6.CIF' data_an6 _database_code_depnum_ccdc_archive 'CCDC 718366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H50 Cl2 Cu2 N6, 2(F6 P)' _chemical_formula_sum 'C38 H50 Cl2 Cu2 F12 N6 P2' _chemical_formula_weight 1078.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.992(5) _cell_length_b 7.1180(10) _cell_length_c 26.973(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.76(3) _cell_angle_gamma 90.00 _cell_volume 4601.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 146 _cell_measurement_theta_min 4.322 _cell_measurement_theta_max 21.487 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 1.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56474 _exptl_absorpt_correction_T_max 0.67318 _exptl_absorpt_process_details 'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39746 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6667 _reflns_number_gt 4915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)' _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^)+(0.0671P)^2^+8.7751P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6667 _refine_ls_number_parameters 279 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.049 _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 P1 P 0.0000 0.89458(17) 0.2500 0.0519(3) Uani 1 2 d S . . F1 F 0.0165(2) 0.6831(7) 0.2612(2) 0.0848(8) Uani 0.50 1 d PU . 1 F2 F -0.0658(3) 0.8967(10) 0.2263(2) 0.0848(8) Uani 0.50 1 d PU . 1 F3 F -0.0018(3) 0.8977(16) 0.1899(4) 0.0848(8) Uani 0.50 1 d PU . 1 F1A F -0.0188(2) 1.1089(8) 0.23558(19) 0.0848(8) Uani 0.50 1 d PU . 2 F2A F -0.0560(6) 1.0138(17) 0.2216(5) 0.0848(8) Uani 0.25 1 d PU . 3 F2B F 0.0591(5) 0.7884(18) 0.2797(4) 0.0848(8) Uani 0.25 1 d PU . 3 F3A F 0.0131(3) 0.8935(16) 0.1969(4) 0.0848(8) Uani 0.50 1 d PU . 3 P2 P 0.2500 0.7500 0.0000 0.0569(3) Uani 1 2 d S . . F4 F 0.2786(2) 0.7002(8) 0.0628(3) 0.0815(8) Uani 0.50 1 d P A 1 F5 F 0.3161(4) 0.7453(14) 0.0111(3) 0.0815(8) Uani 0.50 1 d P A 1 F6 F 0.2578(3) 0.9632(12) 0.0162(3) 0.0815(8) Uani 0.50 1 d P A 1 F4A F 0.2426(3) 0.9783(12) -0.0037(3) 0.0815(8) Uani 0.50 1 d P A 2 F5A F 0.3083(4) 0.7723(14) -0.0048(3) 0.0815(8) Uani 0.50 1 d P A 2 F6A F 0.2641(3) 0.7678(8) 0.0618(3) 0.0815(8) Uani 0.50 1 d P A 2 Cl1 Cl 0.03584(3) 0.74232(9) 0.01750(3) 0.04312(16) Uani 1 1 d . . . Cu1 Cu 0.027964(13) 0.51099(4) 0.070404(12) 0.03312(10) Uani 1 1 d . . . N1 N 0.02507(9) 0.3168(3) 0.12397(8) 0.0365(4) Uani 1 1 d . . . C1 C -0.03612(12) 0.2894(4) 0.11027(12) 0.0454(6) Uani 1 1 d . . . H1A H -0.0518 0.2082 0.0791 0.055 Uiso 1 1 calc R . . H1B H -0.0418 0.2304 0.1402 0.055 Uiso 1 1 calc R . . C2 C -0.06451(12) 0.4768(4) 0.09853(11) 0.0441(6) Uani 1 1 d . . . C3 C -0.11267(13) 0.5156(6) 0.10710(14) 0.0597(9) Uani 1 1 d . . . H3 H -0.1282 0.4262 0.1223 0.072 Uiso 1 1 calc R . . C4 C -0.13699(15) 0.6894(7) 0.09254(17) 0.0735(12) Uani 1 1 d . . . H4 H -0.1690 0.7196 0.0983 0.088 Uiso 1 1 calc R . . C5 C -0.11373(15) 0.8183(6) 0.06934(16) 0.0679(10) Uani 1 1 d . . . H5 H -0.1301 0.9356 0.0589 0.081 Uiso 1 1 calc R . . C6 C -0.06628(13) 0.7717(5) 0.06190(13) 0.0514(7) Uani 1 1 d . . . H6 H -0.0506 0.8592 0.0463 0.062 Uiso 1 1 calc R . . N2 N -0.04161(9) 0.6038(3) 0.07636(9) 0.0406(5) Uani 1 1 d . . . C7 C 0.05215(13) 0.1471(4) 0.11399(12) 0.0451(6) Uani 1 1 d . . . H7A H 0.0247 0.0720 0.0862 0.054 Uiso 1 1 calc R . . H7B H 0.0668 0.0722 0.1465 0.054 Uiso 1 1 calc R . . C8 C 0.09866(11) 0.1977(4) 0.09669(10) 0.0389(5) Uani 1 1 d . . . C9 C 0.14082(14) 0.0738(5) 0.09954(12) 0.0510(7) Uani 1 1 d . . . H9 H 0.1414 -0.0466 0.1131 0.061 Uiso 1 1 calc R . . C10 C 0.18159(14) 0.1292(6) 0.08229(13) 0.0587(8) Uani 1 1 d . . . H10 H 0.2098 0.0466 0.0834 0.070 Uiso 1 1 calc R . . C11 C 0.18011(13) 0.3103(6) 0.06310(13) 0.0570(8) Uani 1 1 d . . . H11 H 0.2080 0.3525 0.0523 0.068 Uiso 1 1 calc R . . C12 C 0.13713(12) 0.4267(5) 0.06025(11) 0.0451(6) Uani 1 1 d . . . H12 H 0.1360 0.5478 0.0469 0.054 Uiso 1 1 calc R . . N3 N 0.09641(9) 0.3709(3) 0.07621(8) 0.0367(4) Uani 1 1 d . . . C13 C 0.05059(12) 0.3779(5) 0.18182(10) 0.0464(6) Uani 1 1 d . . . H13A H 0.0465 0.2755 0.2038 0.056 Uiso 1 1 calc R . . H13B H 0.0289 0.4827 0.1863 0.056 Uiso 1 1 calc R . . C14 C 0.11155(12) 0.4361(5) 0.20416(11) 0.0441(6) Uani 1 1 d . . . H14 H 0.1324 0.3497 0.1906 0.053 Uiso 1 1 calc R . . C15 C 0.12057(14) 0.6352(5) 0.18928(12) 0.0535(7) Uani 1 1 d . . . H15A H 0.0975 0.7202 0.1999 0.064 Uiso 1 1 calc R . . H15B H 0.1089 0.6438 0.1506 0.064 Uiso 1 1 calc R . . C16 C 0.18104(18) 0.6959(8) 0.21593(16) 0.0883(15) Uani 1 1 d . . . H16A H 0.1845 0.8257 0.2068 0.106 Uiso 1 1 calc R . . H16B H 0.2038 0.6194 0.2026 0.106 Uiso 1 1 calc R . . C17 C 0.2021(2) 0.6761(9) 0.27682(17) 0.1011(18) Uani 1 1 d . . . H17A H 0.2414 0.7079 0.2928 0.121 Uiso 1 1 calc R . . H17B H 0.1821 0.7627 0.2907 0.121 Uiso 1 1 calc R . . C18 C 0.19380(17) 0.4780(8) 0.29217(16) 0.0869(15) Uani 1 1 d . . . H18A H 0.2056 0.4700 0.3309 0.104 Uiso 1 1 calc R . . H18B H 0.2169 0.3931 0.2815 0.104 Uiso 1 1 calc R . . C19 C 0.13352(14) 0.4182(6) 0.26564(12) 0.0579(8) Uani 1 1 d . . . H19A H 0.1110 0.4954 0.2791 0.069 Uiso 1 1 calc R . . H19B H 0.1300 0.2887 0.2751 0.069 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 P1 0.0725(7) 0.0442(6) 0.0538(6) 0.000 0.0406(6) 0.000 F1 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F2 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F3 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F1A 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F2A 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F2B 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) F3A 0.106(2) 0.0873(13) 0.0794(15) 0.0157(10) 0.0556(15) 0.0217(14) P2 0.0541(6) 0.0562(7) 0.0696(8) -0.0077(6) 0.0340(6) -0.0076(5) F4 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) F5 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) F6 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) F4A 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) F5A 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) F6A 0.073(2) 0.0793(18) 0.0967(19) 0.004(2) 0.0377(18) 0.0057(17) Cl1 0.0554(4) 0.0337(3) 0.0413(3) 0.0059(2) 0.0199(3) -0.0042(3) Cu1 0.03735(17) 0.03180(16) 0.03290(16) 0.00203(11) 0.01655(12) -0.00231(12) N1 0.0402(11) 0.0396(11) 0.0327(10) 0.0011(8) 0.0174(9) -0.0077(9) C1 0.0449(14) 0.0538(16) 0.0423(14) -0.0008(12) 0.0221(12) -0.0160(12) C2 0.0380(13) 0.0612(18) 0.0333(12) -0.0119(12) 0.0141(10) -0.0111(12) C3 0.0401(15) 0.089(3) 0.0533(17) -0.0150(17) 0.0214(14) -0.0102(16) C4 0.0415(17) 0.108(3) 0.073(2) -0.027(2) 0.0241(17) 0.0030(19) C5 0.0494(18) 0.072(2) 0.070(2) -0.0211(19) 0.0095(16) 0.0127(17) C6 0.0448(15) 0.0469(16) 0.0558(17) -0.0115(13) 0.0123(13) 0.0011(12) N2 0.0383(11) 0.0439(12) 0.0396(11) -0.0093(9) 0.0150(9) -0.0039(9) C7 0.0549(16) 0.0344(13) 0.0480(15) 0.0062(11) 0.0222(13) -0.0034(12) C8 0.0459(14) 0.0375(13) 0.0315(11) -0.0005(10) 0.0129(10) -0.0008(11) C9 0.0569(17) 0.0449(15) 0.0460(15) 0.0005(13) 0.0142(13) 0.0101(13) C10 0.0489(17) 0.074(2) 0.0500(16) -0.0037(16) 0.0156(14) 0.0186(16) C11 0.0404(15) 0.083(2) 0.0507(17) 0.0019(16) 0.0211(13) 0.0044(15) C12 0.0427(14) 0.0527(16) 0.0421(14) 0.0031(12) 0.0190(12) -0.0042(12) N3 0.0380(11) 0.0393(11) 0.0342(10) 0.0009(8) 0.0157(9) -0.0009(9) C13 0.0488(15) 0.0613(18) 0.0321(12) 0.0011(12) 0.0190(11) -0.0097(13) C14 0.0427(14) 0.0566(16) 0.0321(12) 0.0016(11) 0.0134(11) 0.0013(12) C15 0.0531(17) 0.0636(19) 0.0388(14) -0.0012(13) 0.0123(12) -0.0119(15) C16 0.066(2) 0.124(4) 0.061(2) 0.002(2) 0.0098(18) -0.046(3) C17 0.072(3) 0.149(5) 0.058(2) -0.005(3) -0.001(2) -0.046(3) C18 0.050(2) 0.146(5) 0.0471(19) 0.012(2) -0.0001(16) 0.003(2) C19 0.0537(17) 0.080(2) 0.0341(13) 0.0071(15) 0.0106(12) 0.0030(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 P1 F1 1.562(5) 2 ? P1 F1 1.562(5) . ? P1 F2 1.576(6) 2 ? P1 F2 1.576(6) . ? P1 F3A 1.595(10) . ? P1 F3A 1.595(10) 2 ? P1 F2A 1.602(12) 2 ? P1 F2A 1.602(12) . ? P1 F1A 1.603(5) 2 ? P1 F1A 1.603(5) . ? P1 F3 1.604(10) . ? P1 F3 1.604(10) 2 ? F1 F1 0.837(10) 2 ? F1A F1A 0.987(10) 2 ? F2A F2B 1.606(16) 2 ? F2B F2A 1.606(16) 2 ? P2 F6A 1.567(8) . ? P2 F6A 1.567(8) 7_565 ? P2 F6 1.570(9) . ? P2 F6 1.570(9) 7_565 ? P2 F5A 1.577(9) . ? P2 F5A 1.577(9) 7_565 ? P2 F4 1.605(8) . ? P2 F4 1.605(8) 7_565 ? P2 F5 1.627(10) . ? P2 F5 1.627(10) 7_565 ? P2 F4A 1.635(9) . ? P2 F4A 1.635(9) 7_565 ? Cl1 Cu1 2.2396(7) . ? Cu1 N2 1.989(2) . ? Cu1 N3 1.992(2) . ? Cu1 N1 2.022(2) . ? N1 C7 1.474(4) . ? N1 C1 1.500(3) . ? N1 C13 1.504(3) . ? C1 C2 1.498(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.344(4) . ? C2 C3 1.386(4) . ? C3 C4 1.375(6) . ? C3 H3 0.9300 . ? C4 C5 1.375(6) . ? C4 H4 0.9300 . ? C5 C6 1.365(5) . ? C5 H5 0.9300 . ? C6 N2 1.341(4) . ? C6 H6 0.9300 . ? C7 C8 1.499(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.343(3) . ? C8 C9 1.385(4) . ? C9 C10 1.370(5) . ? C9 H9 0.9300 . ? C10 C11 1.384(5) . ? C10 H10 0.9300 . ? C11 C12 1.369(4) . ? C11 H11 0.9300 . ? C12 N3 1.348(3) . ? C12 H12 0.9300 . ? C13 C14 1.519(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.515(5) . ? C14 C19 1.536(4) . ? C14 H14 0.9800 . ? C15 C16 1.517(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.524(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.508(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.510(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? 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 F1 P1 F2 105.1(3) 2 2 ? F1 P1 F2 75.9(3) . 2 ? F1 P1 F2 76.0(3) 2 . ? F1 P1 F2 105.1(3) . . ? F2 P1 F2 178.9(5) 2 . ? F1 P1 F3A 87.7(5) 2 . ? F1 P1 F3A 91.8(4) . . ? F2 P1 F3A 77.8(3) 2 . ? F2 P1 F3A 102.2(3) . . ? F1 P1 F3A 91.8(4) 2 2 ? F1 P1 F3A 87.7(5) . 2 ? F2 P1 F3A 102.2(3) 2 2 ? F2 P1 F3A 77.8(3) . 2 ? F3A P1 F3A 179.5(8) . 2 ? F1 P1 F2A 137.2(6) 2 2 ? F1 P1 F2A 106.7(5) . 2 ? F2 P1 F2A 146.3(6) . 2 ? F3A P1 F2A 87.8(5) . 2 ? F3A P1 F2A 92.5(4) 2 2 ? F1 P1 F2A 106.7(5) 2 . ? F1 P1 F2A 137.2(6) . . ? F2 P1 F2A 146.3(6) 2 . ? F3A P1 F2A 92.5(4) . . ? F3A P1 F2A 87.8(5) 2 . ? F2A P1 F2A 116.0(10) 2 . ? F1 P1 F1A 177.2(3) 2 2 ? F1 P1 F1A 146.6(3) . 2 ? F2 P1 F1A 73.2(3) 2 2 ? F2 P1 F1A 105.7(4) . 2 ? F3A P1 F1A 94.1(5) . 2 ? F3A P1 F1A 86.4(4) 2 2 ? F2A P1 F1A 75.4(6) . 2 ? F1 P1 F1A 146.6(3) 2 . ? F1 P1 F1A 177.2(3) . . ? F2 P1 F1A 105.7(4) 2 . ? F2 P1 F1A 73.2(3) . . ? F3A P1 F1A 86.4(4) . . ? F3A P1 F1A 94.1(5) 2 . ? F2A P1 F1A 75.4(6) 2 . ? F1 P1 F3 85.4(5) 2 . ? F1 P1 F3 96.2(4) . . ? F2 P1 F3 90.7(3) 2 . ? F2 P1 F3 89.3(3) . . ? F3A P1 F3 167.1(5) 2 . ? F2A P1 F3 98.1(5) 2 . ? F2A P1 F3 81.0(4) . . ? F1A P1 F3 96.8(5) 2 . ? F1A P1 F3 81.7(4) . . ? F1 P1 F3 96.2(4) 2 2 ? F1 P1 F3 85.4(5) . 2 ? F2 P1 F3 89.3(3) 2 2 ? F2 P1 F3 90.7(3) . 2 ? F3A P1 F3 167.1(5) . 2 ? F2A P1 F3 81.0(4) 2 2 ? F2A P1 F3 98.1(5) . 2 ? F1A P1 F3 81.7(4) 2 2 ? F1A P1 F3 96.8(5) . 2 ? F3 P1 F3 178.4(8) . 2 ? F1 F1 P1 74.46(19) 2 . ? F1A F1A P1 72.07(19) 2 . ? P1 F2A F2B 60.6(6) . 2 ? F2A F2B P1 59.6(6) 2 . ? F6A P2 F6A 180.00(14) . 7_565 ? F6A P2 F6 71.0(3) . . ? F6A P2 F6 109.0(3) 7_565 . ? F6A P2 F6 109.0(3) . 7_565 ? F6A P2 F6 71.0(3) 7_565 7_565 ? F6 P2 F6 180.0(5) . 7_565 ? F6A P2 F5A 104.0(3) . . ? F6A P2 F5A 76.0(3) 7_565 . ? F6 P2 F5A 84.3(5) . . ? F6 P2 F5A 95.7(5) 7_565 . ? F6A P2 F5A 76.0(3) . 7_565 ? F6A P2 F5A 104.0(3) 7_565 7_565 ? F6 P2 F5A 95.7(5) . 7_565 ? F6 P2 F5A 84.3(5) 7_565 7_565 ? F5A P2 F5A 180.0(5) . 7_565 ? F6A P2 F4 158.0(2) 7_565 . ? F6 P2 F4 87.8(3) . . ? F6 P2 F4 92.2(3) 7_565 . ? F5A P2 F4 92.4(3) . . ? F5A P2 F4 87.6(3) 7_565 . ? F6A P2 F4 158.0(2) . 7_565 ? F6 P2 F4 92.2(3) . 7_565 ? F6 P2 F4 87.8(3) 7_565 7_565 ? F5A P2 F4 87.6(3) . 7_565 ? F5A P2 F4 92.4(3) 7_565 7_565 ? F4 P2 F4 180.0(5) . 7_565 ? F6A P2 F5 90.7(3) . . ? F6A P2 F5 89.3(3) 7_565 . ? F6 P2 F5 87.4(4) . . ? F6 P2 F5 92.6(4) 7_565 . ? F5A P2 F5 164.3(4) 7_565 . ? F4 P2 F5 77.1(3) . . ? F4 P2 F5 102.9(3) 7_565 . ? F6A P2 F5 89.3(3) . 7_565 ? F6A P2 F5 90.7(3) 7_565 7_565 ? F6 P2 F5 92.6(4) . 7_565 ? F6 P2 F5 87.4(4) 7_565 7_565 ? F5A P2 F5 164.3(4) . 7_565 ? F4 P2 F5 102.9(3) . 7_565 ? F4 P2 F5 77.1(3) 7_565 7_565 ? F5 P2 F5 180.0(5) . 7_565 ? F6A P2 F4A 87.6(3) . . ? F6A P2 F4A 92.4(3) 7_565 . ? F6 P2 F4A 160.7(3) 7_565 . ? F5A P2 F4A 89.4(4) . . ? F5A P2 F4A 90.6(4) 7_565 . ? F4 P2 F4A 106.2(3) . . ? F4 P2 F4A 73.8(3) 7_565 . ? F5 P2 F4A 97.0(4) . . ? F5 P2 F4A 83.0(4) 7_565 . ? F6A P2 F4A 92.4(3) . 7_565 ? F6A P2 F4A 87.6(3) 7_565 7_565 ? F6 P2 F4A 160.7(3) . 7_565 ? F5A P2 F4A 90.6(4) . 7_565 ? F5A P2 F4A 89.4(4) 7_565 7_565 ? F4 P2 F4A 73.8(3) . 7_565 ? F4 P2 F4A 106.2(3) 7_565 7_565 ? F5 P2 F4A 83.0(4) . 7_565 ? F5 P2 F4A 97.0(4) 7_565 7_565 ? F4A P2 F4A 180.0(5) . 7_565 ? N2 Cu1 N3 166.41(9) . . ? N2 Cu1 N1 83.29(10) . . ? N3 Cu1 N1 83.14(9) . . ? N2 Cu1 Cl1 96.74(8) . . ? N3 Cu1 Cl1 96.84(7) . . ? N1 Cu1 Cl1 174.76(6) . . ? C7 N1 C1 112.6(2) . . ? C7 N1 C13 112.1(2) . . ? C1 N1 C13 107.0(2) . . ? C7 N1 Cu1 106.11(15) . . ? C1 N1 Cu1 104.00(16) . . ? C13 N1 Cu1 114.86(17) . . ? C2 C1 N1 109.0(2) . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C3 121.6(3) . . ? N2 C2 C1 115.3(2) . . ? C3 C2 C1 123.1(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 119.1(4) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N2 C6 C5 122.1(3) . . ? N2 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 N2 C2 119.0(3) . . ? C6 N2 Cu1 128.3(2) . . ? C2 N2 Cu1 112.7(2) . . ? N1 C7 C8 111.1(2) . . ? N1 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N1 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C9 121.0(3) . . ? N3 C8 C7 115.9(2) . . ? C9 C8 C7 123.1(3) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N3 C12 C11 121.9(3) . . ? N3 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C8 N3 C12 119.2(2) . . ? C8 N3 Cu1 112.80(17) . . ? C12 N3 Cu1 128.0(2) . . ? N1 C13 C14 117.7(2) . . ? N1 C13 H13A 107.9 . . ? C14 C13 H13A 107.9 . . ? N1 C13 H13B 107.9 . . ? C14 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C15 C14 C13 113.3(3) . . ? C15 C14 C19 109.4(3) . . ? C13 C14 C19 107.5(2) . . ? C15 C14 H14 108.9 . . ? C13 C14 H14 108.9 . . ? C19 C14 H14 108.9 . . ? C14 C15 C16 112.3(3) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 111.0(3) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 110.6(4) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 C18 C19 111.4(4) . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C14 111.9(3) . . ? C18 C19 H19A 109.2 . . ? C14 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C14 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 P1 F1 F1 -159.5(8) 2 . . 2 ? F2 P1 F1 F1 20.6(8) . . . 2 ? F3A P1 F1 F1 -82.5(8) . . . 2 ? F3A P1 F1 F1 97.3(8) 2 . . 2 ? F2A P1 F1 F1 -170.8(8) 2 . . 2 ? F2A P1 F1 F1 13.1(11) . . . 2 ? F1A P1 F1 F1 177.3(6) 2 . . 2 ? F3 P1 F1 F1 -70.4(8) . . . 2 ? F3 P1 F1 F1 110.0(8) 2 . . 2 ? F1 P1 F1A F1A 177.6(5) 2 . . 2 ? F2 P1 F1A F1A -25.7(6) 2 . . 2 ? F2 P1 F1A F1A 154.1(6) . . . 2 ? F3A P1 F1A F1A -102.0(7) . . . 2 ? F3A P1 F1A F1A 78.1(6) 2 . . 2 ? F2A P1 F1A F1A -13.4(7) 2 . . 2 ? F2A P1 F1A F1A 160.0(10) . . . 2 ? F3 P1 F1A F1A -114.1(7) . . . 2 ? F3 P1 F1A F1A 65.5(6) 2 . . 2 ? F1 P1 F2A F2B 3.1(6) 2 . . 2 ? F1 P1 F2A F2B -3.9(8) . . . 2 ? F2 P1 F2A F2B 163.1(7) 2 . . 2 ? F2 P1 F2A F2B -17.4(7) . . . 2 ? F3A P1 F2A F2B 91.5(6) . . . 2 ? F3A P1 F2A F2B -88.1(6) 2 . . 2 ? F2A P1 F2A F2B -179.8(6) 2 . . 2 ? F1A P1 F2A F2B -175.0(5) 2 . . 2 ? F1A P1 F2A F2B 173.1(9) . . . 2 ? F3 P1 F2A F2B 85.5(6) . . . 2 ? F3 P1 F2A F2B -95.8(6) 2 . . 2 ? F1 P1 F2B F2A 177.3(6) 2 . . 2 ? F1 P1 F2B F2A -175.9(8) . . . 2 ? F2 P1 F2B F2A 19.0(8) 2 . . 2 ? F2 P1 F2B F2A -160.3(9) . . . 2 ? F3A P1 F2B F2A 89.1(6) . . . 2 ? F3A P1 F2B F2A -91.4(6) 2 . . 2 ? F1A P1 F2B F2A -4.6(6) 2 . . 2 ? F1A P1 F2B F2A 6.9(7) . . . 2 ? F3 P1 F2B F2A 94.2(6) . . . 2 ? F3 P1 F2B F2A -84.4(6) 2 . . 2 ? N2 Cu1 N1 C7 150.73(18) . . . . ? N3 Cu1 N1 C7 -28.60(17) . . . . ? N2 Cu1 N1 C1 31.79(17) . . . . ? N3 Cu1 N1 C1 -147.54(17) . . . . ? N2 Cu1 N1 C13 -84.85(19) . . . . ? N3 Cu1 N1 C13 95.82(19) . . . . ? C7 N1 C1 C2 -155.9(2) . . . . ? C13 N1 C1 C2 80.5(3) . . . . ? Cu1 N1 C1 C2 -41.5(2) . . . . ? N1 C1 C2 N2 31.8(3) . . . . ? N1 C1 C2 C3 -151.4(3) . . . . ? N2 C2 C3 C4 -0.3(5) . . . . ? C1 C2 C3 C4 -176.9(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? C4 C5 C6 N2 0.2(5) . . . . ? C5 C6 N2 C2 0.5(4) . . . . ? C5 C6 N2 Cu1 -178.6(2) . . . . ? C3 C2 N2 C6 -0.5(4) . . . . ? C1 C2 N2 C6 176.4(2) . . . . ? C3 C2 N2 Cu1 178.8(2) . . . . ? C1 C2 N2 Cu1 -4.3(3) . . . . ? N3 Cu1 N2 C6 165.5(3) . . . . ? N1 Cu1 N2 C6 162.7(2) . . . . ? Cl1 Cu1 N2 C6 -12.1(2) . . . . ? N3 Cu1 N2 C2 -13.7(5) . . . . ? N1 Cu1 N2 C2 -16.54(18) . . . . ? Cl1 Cu1 N2 C2 168.73(17) . . . . ? C1 N1 C7 C8 147.0(2) . . . . ? C13 N1 C7 C8 -92.2(3) . . . . ? Cu1 N1 C7 C8 33.9(3) . . . . ? N1 C7 C8 N3 -21.3(3) . . . . ? N1 C7 C8 C9 160.8(3) . . . . ? N3 C8 C9 C10 1.3(4) . . . . ? C7 C8 C9 C10 179.1(3) . . . . ? C8 C9 C10 C11 1.1(5) . . . . ? C9 C10 C11 C12 -2.1(5) . . . . ? C10 C11 C12 N3 0.8(5) . . . . ? C9 C8 N3 C12 -2.7(4) . . . . ? C7 C8 N3 C12 179.4(2) . . . . ? C9 C8 N3 Cu1 174.5(2) . . . . ? C7 C8 N3 Cu1 -3.4(3) . . . . ? C11 C12 N3 C8 1.6(4) . . . . ? C11 C12 N3 Cu1 -175.1(2) . . . . ? N2 Cu1 N3 C8 15.8(5) . . . . ? N1 Cu1 N3 C8 18.60(17) . . . . ? Cl1 Cu1 N3 C8 -166.68(16) . . . . ? N2 Cu1 N3 C12 -167.3(3) . . . . ? N1 Cu1 N3 C12 -164.5(2) . . . . ? Cl1 Cu1 N3 C12 10.2(2) . . . . ? C7 N1 C13 C14 62.7(3) . . . . ? C1 N1 C13 C14 -173.4(3) . . . . ? Cu1 N1 C13 C14 -58.5(3) . . . . ? N1 C13 C14 C15 80.3(3) . . . . ? N1 C13 C14 C19 -158.6(3) . . . . ? C13 C14 C15 C16 175.1(3) . . . . ? C19 C14 C15 C16 55.2(4) . . . . ? C14 C15 C16 C17 -56.2(6) . . . . ? C15 C16 C17 C18 55.5(6) . . . . ? C16 C17 C18 C19 -56.0(6) . . . . ? C17 C18 C19 C14 56.5(5) . . . . ? C15 C14 C19 C18 -55.1(4) . . . . ? C13 C14 C19 C18 -178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.734 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.078 # Attachment 'Cu8Complexof7tilo16.cif' data_tilo16 _database_code_depnum_ccdc_archive 'CCDC 718367' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cl4 Cu2 N6' _chemical_formula_sum 'C32 H32 Cl4 Cu2 N6' _chemical_formula_weight 769.52 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' 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 'P 21/n' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.702(1) _cell_length_b 12.422(1) _cell_length_c 14.911(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.17(1) _cell_angle_gamma 90.00 _cell_volume 1611.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 189 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 21.28 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7627 _exptl_absorpt_correction_T_max 0.8496 _exptl_absorpt_process_details 'SADABS version 2.03.(Sheldrick,Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37856 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 30.51 _reflns_number_total 4935 _reflns_number_gt 3785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal-99 (E.Keller 1999)' _computing_publication_material 'XCIF 6.12 (Sheldrick, 1997)' _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^)+(0.0384P)^2^+1.2425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4935 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96749(3) 0.150920(19) 0.236345(16) 0.02538(8) Uani 1 1 d . . . Cl2 Cl 0.80563(6) 0.20107(4) 0.37126(3) 0.03417(12) Uani 1 1 d . . . Cl3 Cl 1.07180(8) 0.30606(5) 0.18800(5) 0.04886(16) Uani 1 1 d . . . N1 N 0.9185(2) -0.01090(14) 0.24775(11) 0.0275(3) Uani 1 1 d . . . C2 C 1.0086(3) -0.07932(17) 0.18346(14) 0.0318(4) Uani 1 1 d . . . H2A H 0.9673 -0.1536 0.1850 0.038 Uiso 1 1 calc R . . H2B H 1.1169 -0.0822 0.2039 0.038 Uiso 1 1 calc R . . C3 C 1.0044(2) -0.03911(16) 0.08799(13) 0.0277(4) Uani 1 1 d . . . C4 C 0.9038(2) -0.08363(17) 0.02547(14) 0.0303(4) Uani 1 1 d . . . H4 H 0.8383 -0.1413 0.0423 0.036 Uiso 1 1 calc R . . C5 C 0.8990(2) -0.04392(18) -0.06146(14) 0.0307(4) Uani 1 1 d . . . H5 H 0.8287 -0.0739 -0.1034 0.037 Uiso 1 1 calc R . . N20 N 1.1429(2) 0.10509(17) 0.31616(13) 0.0361(4) Uani 1 1 d . . . C21 C 1.2719(3) 0.1596(3) 0.3351(2) 0.0546(7) Uani 1 1 d . . . H21 H 1.2988 0.2204 0.2999 0.065 Uiso 1 1 calc R . . C22 C 1.3677(4) 0.1280(4) 0.4063(2) 0.0740(11) Uani 1 1 d . . . H22 H 1.4606 0.1655 0.4185 0.089 Uiso 1 1 calc R . . C23 C 1.3241(4) 0.0414(4) 0.4583(2) 0.0731(11) Uani 1 1 d . . . H23 H 1.3829 0.0226 0.5098 0.088 Uiso 1 1 calc R . . C24 C 1.1979(4) -0.0172(3) 0.43644(17) 0.0556(8) Uani 1 1 d . . . H24 H 1.1710 -0.0797 0.4696 0.067 Uiso 1 1 calc R . . C25 C 1.1093(3) 0.0167(2) 0.36444(14) 0.0388(5) Uani 1 1 d . . . C26 C 0.9654(3) -0.04013(18) 0.33964(14) 0.0388(5) Uani 1 1 d . . . H26A H 0.9816 -0.1189 0.3434 0.047 Uiso 1 1 calc R . . H26B H 0.8830 -0.0204 0.3822 0.047 Uiso 1 1 calc R . . N30 N 0.7855(2) 0.14556(15) 0.15373(12) 0.0307(4) Uani 1 1 d . . . C31 C 0.7460(3) 0.2199(2) 0.09218(16) 0.0431(6) Uani 1 1 d . . . H31 H 0.8122 0.2795 0.0824 0.052 Uiso 1 1 calc R . . C32 C 0.6124(3) 0.2121(3) 0.04302(18) 0.0547(8) Uani 1 1 d . . . H32 H 0.5876 0.2647 -0.0009 0.066 Uiso 1 1 calc R . . C33 C 0.5166(3) 0.1278(3) 0.0583(2) 0.0597(9) Uani 1 1 d . . . H33 H 0.4220 0.1227 0.0266 0.072 Uiso 1 1 calc R . . C34 C 0.5565(3) 0.0490(3) 0.12000(19) 0.0541(7) Uani 1 1 d . . . H34 H 0.4909 -0.0107 0.1307 0.065 Uiso 1 1 calc R . . C35 C 0.6957(2) 0.0597(2) 0.16620(15) 0.0351(5) Uani 1 1 d . . . C36 C 0.7506(3) -0.02142(19) 0.23339(16) 0.0379(5) Uani 1 1 d . . . H36A H 0.6964 -0.0104 0.2909 0.045 Uiso 1 1 calc R . . H36B H 0.7267 -0.0949 0.2117 0.045 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 0.02659(12) 0.02241(12) 0.02713(13) 0.00398(10) -0.00067(9) -0.00228(10) Cl2 0.0428(3) 0.0296(2) 0.0302(2) -0.0022(2) 0.0059(2) 0.0080(2) Cl3 0.0525(4) 0.0320(3) 0.0622(4) 0.0117(3) 0.0094(3) -0.0122(3) N1 0.0374(9) 0.0232(8) 0.0221(8) 0.0008(6) 0.0076(6) -0.0018(7) C2 0.0425(12) 0.0274(10) 0.0257(10) 0.0003(8) 0.0066(8) 0.0049(9) C3 0.0321(10) 0.0270(9) 0.0240(9) -0.0023(8) 0.0076(7) 0.0030(8) C4 0.0322(10) 0.0307(10) 0.0282(10) -0.0008(8) 0.0081(8) -0.0044(9) C5 0.0316(10) 0.0350(11) 0.0254(9) -0.0047(8) 0.0042(8) -0.0041(9) N20 0.0313(9) 0.0415(10) 0.0355(10) -0.0046(8) -0.0043(7) 0.0029(8) C21 0.0344(13) 0.0686(19) 0.0606(17) -0.0087(15) -0.0088(12) -0.0015(13) C22 0.0382(15) 0.120(3) 0.064(2) -0.014(2) -0.0163(14) 0.0016(18) C23 0.0524(18) 0.117(3) 0.0501(17) -0.0016(19) -0.0088(14) 0.042(2) C24 0.0653(18) 0.0678(19) 0.0336(12) 0.0000(12) -0.0034(12) 0.0363(16) C25 0.0530(14) 0.0386(12) 0.0248(10) -0.0017(9) 0.0010(9) 0.0190(11) C26 0.0652(16) 0.0284(10) 0.0229(10) 0.0055(8) 0.0083(10) 0.0069(11) N30 0.0320(9) 0.0330(9) 0.0270(8) -0.0027(7) -0.0012(7) 0.0045(8) C31 0.0495(14) 0.0449(13) 0.0347(12) -0.0011(10) -0.0070(10) 0.0144(12) C32 0.0526(16) 0.071(2) 0.0402(14) -0.0083(13) -0.0137(12) 0.0270(16) C33 0.0388(14) 0.092(2) 0.0477(15) -0.0250(16) -0.0148(12) 0.0168(16) C34 0.0320(12) 0.074(2) 0.0564(16) -0.0272(15) 0.0030(11) -0.0072(13) C35 0.0288(10) 0.0425(12) 0.0340(11) -0.0149(10) 0.0054(8) -0.0013(9) C36 0.0396(12) 0.0333(11) 0.0409(12) -0.0064(10) 0.0146(9) -0.0128(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N30 2.0043(19) . ? Cu1 N20 2.015(2) . ? Cu1 N1 2.0620(17) . ? Cu1 Cl3 2.2498(7) . ? Cu1 Cl2 2.5370(9) . ? N1 C26 1.474(3) . ? N1 C36 1.482(3) . ? N1 C2 1.503(3) . ? C2 C3 1.509(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.389(3) 3_755 ? C3 C4 1.392(3) . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C3 1.389(3) 3_755 ? C5 H5 0.9500 . ? N20 C21 1.340(3) . ? N20 C25 1.346(3) . ? C21 C22 1.405(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.356(5) . ? C23 H23 0.9500 . ? C24 C25 1.385(3) . ? C24 H24 0.9500 . ? C25 C26 1.483(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N30 C35 1.336(3) . ? N30 C31 1.346(3) . ? C31 C32 1.376(4) . ? C31 H31 0.9500 . ? C32 C33 1.358(5) . ? C32 H32 0.9500 . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.398(3) . ? C34 H34 0.9500 . ? C35 C36 1.498(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N30 Cu1 N20 161.69(8) . . ? N30 Cu1 N1 81.67(7) . . ? N20 Cu1 N1 80.35(8) . . ? N30 Cu1 Cl3 98.64(6) . . ? N20 Cu1 Cl3 97.21(6) . . ? N1 Cu1 Cl3 160.95(5) . . ? N30 Cu1 Cl2 93.21(6) . . ? N20 Cu1 Cl2 91.29(6) . . ? N1 Cu1 Cl2 93.36(5) . . ? Cl3 Cu1 Cl2 105.62(3) . . ? C26 N1 C36 112.51(17) . . ? C26 N1 C2 108.05(17) . . ? C36 N1 C2 111.96(17) . . ? C26 N1 Cu1 105.07(13) . . ? C36 N1 Cu1 106.15(13) . . ? C2 N1 Cu1 112.96(12) . . ? N1 C2 C3 113.78(17) . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C5 C3 C4 118.98(18) 3_755 . ? C5 C3 C2 120.11(19) 3_755 . ? C4 C3 C2 120.91(19) . . ? C5 C4 C3 120.10(19) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C3 120.9(2) . 3_755 ? C4 C5 H5 119.5 . . ? C3 C5 H5 119.5 3_755 . ? C21 N20 C25 118.9(2) . . ? C21 N20 Cu1 127.9(2) . . ? C25 N20 Cu1 112.39(16) . . ? N20 C21 C22 120.9(3) . . ? N20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 118.6(3) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 118.2(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N20 C25 C24 122.7(3) . . ? N20 C25 C26 116.1(2) . . ? C24 C25 C26 121.1(3) . . ? N1 C26 C25 110.24(18) . . ? N1 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N1 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C35 N30 C31 119.6(2) . . ? C35 N30 Cu1 113.73(15) . . ? C31 N30 Cu1 126.61(17) . . ? N30 C31 C32 121.9(3) . . ? N30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 118.9(3) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 120.1(2) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 118.4(3) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N30 C35 C34 120.9(2) . . ? N30 C35 C36 116.41(19) . . ? C34 C35 C36 122.7(2) . . ? N1 C36 C35 110.46(17) . . ? N1 C36 H36A 109.6 . . ? C35 C36 H36A 109.6 . . ? N1 C36 H36B 109.6 . . ? C35 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? 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 N30 Cu1 N1 C26 -148.77(15) . . . . ? N20 Cu1 N1 C26 34.73(14) . . . . ? Cl3 Cu1 N1 C26 118.87(17) . . . . ? Cl2 Cu1 N1 C26 -56.01(13) . . . . ? N30 Cu1 N1 C36 -29.38(13) . . . . ? N20 Cu1 N1 C36 154.12(14) . . . . ? Cl3 Cu1 N1 C36 -121.74(17) . . . . ? Cl2 Cu1 N1 C36 63.38(12) . . . . ? N30 Cu1 N1 C2 93.68(15) . . . . ? N20 Cu1 N1 C2 -82.82(15) . . . . ? Cl3 Cu1 N1 C2 1.3(3) . . . . ? Cl2 Cu1 N1 C2 -173.56(13) . . . . ? C26 N1 C2 C3 -164.73(19) . . . . ? C36 N1 C2 C3 70.8(2) . . . . ? Cu1 N1 C2 C3 -48.9(2) . . . . ? N1 C2 C3 C5 81.0(2) . . . 3_755 ? N1 C2 C3 C4 -98.5(2) . . . . ? C5 C3 C4 C5 -1.1(3) 3_755 . . . ? C2 C3 C4 C5 178.47(19) . . . . ? C3 C4 C5 C3 1.1(3) . . . 3_755 ? N30 Cu1 N20 C21 153.9(2) . . . . ? N1 Cu1 N20 C21 165.0(2) . . . . ? Cl3 Cu1 N20 C21 4.1(2) . . . . ? Cl2 Cu1 N20 C21 -101.8(2) . . . . ? N30 Cu1 N20 C25 -36.8(3) . . . . ? N1 Cu1 N20 C25 -25.73(15) . . . . ? Cl3 Cu1 N20 C25 173.38(15) . . . . ? Cl2 Cu1 N20 C25 67.46(15) . . . . ? C25 N20 C21 C22 -2.5(4) . . . . ? Cu1 N20 C21 C22 166.1(2) . . . . ? N20 C21 C22 C23 -1.9(5) . . . . ? C21 C22 C23 C24 5.3(5) . . . . ? C22 C23 C24 C25 -4.1(5) . . . . ? C21 N20 C25 C24 3.8(3) . . . . ? Cu1 N20 C25 C24 -166.56(19) . . . . ? C21 N20 C25 C26 -179.7(2) . . . . ? Cu1 N20 C25 C26 10.0(2) . . . . ? C23 C24 C25 N20 -0.5(4) . . . . ? C23 C24 C25 C26 -176.8(2) . . . . ? C36 N1 C26 C25 -153.68(18) . . . . ? C2 N1 C26 C25 82.2(2) . . . . ? Cu1 N1 C26 C25 -38.6(2) . . . . ? N20 C25 C26 N1 20.3(3) . . . . ? C24 C25 C26 N1 -163.1(2) . . . . ? N20 Cu1 N30 C35 30.7(3) . . . . ? N1 Cu1 N30 C35 19.66(14) . . . . ? Cl3 Cu1 N30 C35 -179.60(14) . . . . ? Cl2 Cu1 N30 C35 -73.26(14) . . . . ? N20 Cu1 N30 C31 -151.8(2) . . . . ? N1 Cu1 N30 C31 -162.8(2) . . . . ? Cl3 Cu1 N30 C31 -2.09(19) . . . . ? Cl2 Cu1 N30 C31 104.24(19) . . . . ? C35 N30 C31 C32 2.0(3) . . . . ? Cu1 N30 C31 C32 -175.37(19) . . . . ? N30 C31 C32 C33 1.2(4) . . . . ? C31 C32 C33 C34 -2.5(4) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? C31 N30 C35 C34 -3.8(3) . . . . ? Cu1 N30 C35 C34 173.89(17) . . . . ? C31 N30 C35 C36 177.8(2) . . . . ? Cu1 N30 C35 C36 -4.5(2) . . . . ? C33 C34 C35 N30 2.5(4) . . . . ? C33 C34 C35 C36 -179.2(2) . . . . ? C26 N1 C36 C35 148.82(18) . . . . ? C2 N1 C36 C35 -89.3(2) . . . . ? Cu1 N1 C36 C35 34.43(19) . . . . ? N30 C35 C36 N1 -21.1(3) . . . . ? C34 C35 C36 N1 160.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.893 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.073 _chemical_compound_source Synthesis _exptl_crystal_recrystallization_method 'Vapor Diffusion' # Attachment 'Cu9BAJCSADx.CIF' data_bajcsad _database_code_depnum_ccdc_archive 'CCDC 718368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C41 H45 Cl Cu2 N12 O7, C4 H10 O, 2(Cl O4)' _chemical_formula_sum 'C45 H55 Cl3 Cu2 N12 O16' _chemical_formula_weight 1253.44 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.266(3) _cell_length_b 23.434(4) _cell_length_c 15.982(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.86(2) _cell_angle_gamma 90.000 _cell_volume 5279(2) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 25132 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 33.00 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.165 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'SADABS (Sheldrick,1999-2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex 2 CCD ' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 169744 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.40 _reflns_number_total 9704 _reflns_number_gt 7957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (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^)+(0.0536P)^2^+25.5575P] 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 9704 _refine_ls_number_parameters 714 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.110 _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 Cu1 Cu 0.91894(4) 0.17604(2) 0.87479(4) 0.02765(16) Uani 1 1 d . A . Cu2 Cu 0.72718(4) 0.14643(3) 0.92059(4) 0.02857(16) Uani 1 1 d . . . O1 O 0.8279(2) 0.11535(13) 0.8661(2) 0.0285(7) Uani 1 1 d . A . C52 C 0.8381(4) 0.0585(2) 0.8400(4) 0.0425(13) Uani 1 1 d . . . H52A H 0.8758 0.0579 0.7936 0.064 Uiso 1 1 calc R A . H52B H 0.7754 0.0421 0.8205 0.064 Uiso 1 1 calc R . . H52C H 0.8704 0.0361 0.8877 0.064 Uiso 1 1 calc R . . O2 O 0.8241(2) 0.20481(14) 0.9368(2) 0.0301(7) Uani 1 1 d . A . C53 C 0.8318(4) 0.2512(3) 0.9923(4) 0.0521(16) Uani 1 1 d . . . H53A H 0.8678 0.2399 1.0470 0.078 Uiso 1 1 calc R A . H53B H 0.7683 0.2638 1.0003 0.078 Uiso 1 1 calc R . . H53C H 0.8647 0.2826 0.9685 0.078 Uiso 1 1 calc R . . O100 O 0.8019(3) 0.1009(2) 1.0539(3) 0.0595(12) Uani 1 1 d D A 1 H101 H 0.812(4) 0.077(3) 1.100(3) 0.089 Uiso 1 1 d D B 1 H102 H 0.860(2) 0.110(3) 1.043(4) 0.089 Uiso 1 1 d D C 1 C1 C 0.7326(3) 0.12220(19) 0.6440(3) 0.0251(10) Uani 1 1 d . . . N2 N 0.8142(3) 0.15125(16) 0.6510(2) 0.0261(8) Uani 1 1 d . . . C3 C 0.8174(3) 0.19598(19) 0.7036(3) 0.0247(10) Uani 1 1 d . . . N4 N 0.7469(3) 0.21430(16) 0.7426(2) 0.0271(9) Uani 1 1 d . . . C5 C 0.6759(3) 0.1773(2) 0.7388(3) 0.0259(10) Uani 1 1 d . . . N6 N 0.6632(3) 0.12999(17) 0.6909(2) 0.0275(9) Uani 1 1 d . . . N7 N 0.7204(3) 0.08016(17) 0.5846(2) 0.0272(8) Uani 1 1 d . . . N8 N 0.9023(3) 0.22349(17) 0.7229(2) 0.0297(9) Uani 1 1 d . . . N9 N 0.6094(3) 0.18692(18) 0.7913(3) 0.0308(9) Uani 1 1 d . . . C10 C 0.6346(3) 0.0461(2) 0.5732(3) 0.0322(11) Uani 1 1 d . D . H10A H 0.6237 0.0311 0.5145 0.039 Uiso 1 1 calc R . . H10B H 0.5802 0.0709 0.5802 0.039 Uiso 1 1 calc R . . C11 C 0.6375(3) -0.0032(2) 0.6338(3) 0.0307(11) Uani 1 1 d . . . N12 N 0.7221(3) -0.02266(18) 0.6695(2) 0.0295(9) Uani 1 1 d D D 1 H12 H 0.777(2) -0.008(2) 0.657(3) 0.035 Uiso 1 1 d D E 1 C13 C 0.7317(4) -0.0669(3) 0.7231(3) 0.0435(13) Uani 1 1 d . . . H13 H 0.7932 -0.0795 0.7472 0.052 Uiso 1 1 calc R D 1 C14 C 0.6537(5) -0.0939(3) 0.7433(4) 0.0560(17) Uani 1 1 d . D . H14 H 0.6601 -0.1250 0.7819 0.067 Uiso 1 1 calc R . . C15 C 0.5660(5) -0.0754(3) 0.7070(4) 0.0564(17) Uani 1 1 d . . . H15 H 0.5109 -0.0943 0.7195 0.068 Uiso 1 1 calc R D . C16 C 0.5571(4) -0.0296(3) 0.6522(4) 0.0444(13) Uani 1 1 d . D . H16 H 0.4961 -0.0165 0.6275 0.053 Uiso 1 1 calc R . . C17 C 0.7883(4) 0.0753(2) 0.5255(3) 0.0323(11) Uani 1 1 d . . . H17A H 0.7950 0.1131 0.4992 0.039 Uiso 1 1 calc R . . H17B H 0.7629 0.0485 0.4798 0.039 Uiso 1 1 calc R . . C18 C 0.8847(4) 0.0551(2) 0.5658(3) 0.0302(11) Uani 1 1 d . . . N19 N 0.8887(3) 0.01676(17) 0.6282(3) 0.0301(9) Uani 1 1 d . . . C20 C 0.9734(4) -0.0032(2) 0.6636(3) 0.0371(12) Uani 1 1 d . . . H20 H 0.9765 -0.0293 0.7095 0.045 Uiso 1 1 calc R . . C21 C 1.0563(4) 0.0127(3) 0.6357(4) 0.0497(15) Uani 1 1 d . . . H21 H 1.1152 -0.0032 0.6607 0.060 Uiso 1 1 calc R . . C22 C 1.0524(5) 0.0519(3) 0.5710(4) 0.0539(16) Uani 1 1 d . . . H22 H 1.1087 0.0640 0.5512 0.065 Uiso 1 1 calc R . . C23 C 0.9654(4) 0.0734(2) 0.5356(4) 0.0410(13) Uani 1 1 d . . . H23 H 0.9609 0.1004 0.4909 0.049 Uiso 1 1 calc R . . C24 C 0.9848(4) 0.2030(2) 0.6896(3) 0.0327(11) Uani 1 1 d . . . H24A H 1.0249 0.2362 0.6803 0.039 Uiso 1 1 calc R . . H24B H 0.9634 0.1852 0.6337 0.039 Uiso 1 1 calc R . . C25 C 1.0455(3) 0.1602(2) 0.7447(3) 0.0320(11) Uani 1 1 d . A . N26 N 1.0170(3) 0.13882(18) 0.8143(3) 0.0326(9) Uani 1 1 d . . . C27 C 1.0696(4) 0.0979(2) 0.8583(4) 0.0440(14) Uani 1 1 d . A . H27 H 1.0484 0.0821 0.9069 0.053 Uiso 1 1 calc R . . C28 C 1.1526(4) 0.0780(3) 0.8355(4) 0.0541(17) Uani 1 1 d . . . H28 H 1.1880 0.0489 0.8675 0.065 Uiso 1 1 calc R A . C29 C 1.1833(4) 0.1010(3) 0.7660(4) 0.0562(17) Uani 1 1 d . A . H29 H 1.2414 0.0889 0.7496 0.067 Uiso 1 1 calc R . . C30 C 1.1290(4) 0.1418(3) 0.7202(4) 0.0457(14) Uani 1 1 d . . . H30 H 1.1490 0.1576 0.6711 0.055 Uiso 1 1 calc R A . C31 C 0.9062(4) 0.2814(2) 0.7569(3) 0.0343(11) Uani 1 1 d . . . H31A H 0.8446 0.2906 0.7751 0.041 Uiso 1 1 calc R . . H31B H 0.9160 0.3086 0.7116 0.041 Uiso 1 1 calc R . . C32 C 0.9842(4) 0.2890(2) 0.8307(3) 0.0307(11) Uani 1 1 d . A . N33 N 0.9976(3) 0.24721(17) 0.8887(3) 0.0314(9) Uani 1 1 d . . . C34 C 1.0656(4) 0.2539(2) 0.9567(3) 0.0368(12) Uani 1 1 d . A . H34 H 1.0748 0.2245 0.9981 0.044 Uiso 1 1 calc R . . C35 C 1.1217(4) 0.3013(3) 0.9682(3) 0.0402(13) Uani 1 1 d . . . H35 H 1.1690 0.3049 1.0167 0.048 Uiso 1 1 calc R A . C36 C 1.1084(4) 0.3438(3) 0.9082(4) 0.0452(14) Uani 1 1 d . A . H36 H 1.1469 0.3771 0.9146 0.054 Uiso 1 1 calc R . . C37 C 1.0391(4) 0.3379(2) 0.8388(3) 0.0381(12) Uani 1 1 d . . . H37 H 1.0291 0.3670 0.7970 0.046 Uiso 1 1 calc R A . C38 C 0.6046(4) 0.2425(2) 0.8319(3) 0.0358(12) Uani 1 1 d . A . H38A H 0.5517 0.2647 0.8002 0.043 Uiso 1 1 calc R . . H38B H 0.6642 0.2636 0.8291 0.043 Uiso 1 1 calc R . . C39 C 0.5901(4) 0.2376(2) 0.9233(3) 0.0329(11) Uani 1 1 d . . . N40 N 0.6348(3) 0.19540(19) 0.9695(3) 0.0329(9) Uani 1 1 d . A . C41 C 0.6255(4) 0.1904(2) 1.0518(3) 0.0383(12) Uani 1 1 d . . . H41 H 0.6558 0.1597 1.0840 0.046 Uiso 1 1 calc R A . C42 C 0.5728(4) 0.2289(3) 1.0904(4) 0.0471(15) Uani 1 1 d . A . H42 H 0.5678 0.2250 1.1488 0.057 Uiso 1 1 calc R . . C43 C 0.5279(4) 0.2727(3) 1.0441(4) 0.0514(16) Uani 1 1 d . . . H43 H 0.4916 0.2996 1.0698 0.062 Uiso 1 1 calc R A . C44 C 0.5360(4) 0.2775(3) 0.9591(4) 0.0445(14) Uani 1 1 d . A . H44 H 0.5051 0.3076 0.9258 0.053 Uiso 1 1 calc R . . C45 C 0.5292(4) 0.1488(2) 0.7878(3) 0.0376(12) Uani 1 1 d . A . H45A H 0.5048 0.1407 0.7276 0.045 Uiso 1 1 calc R . . H45B H 0.4784 0.1688 0.8119 0.045 Uiso 1 1 calc R . . C46 C 0.5485(4) 0.0931(2) 0.8333(3) 0.0344(11) Uani 1 1 d . . . N47 N 0.6283(3) 0.08545(18) 0.8887(3) 0.0343(10) Uani 1 1 d . A . C48 C 0.6407(5) 0.0352(2) 0.9299(4) 0.0456(14) Uani 1 1 d . . . H48 H 0.6981 0.0293 0.9678 0.055 Uiso 1 1 calc R A . C49 C 0.5753(5) -0.0078(3) 0.9199(4) 0.0558(17) Uani 1 1 d . A . H49 H 0.5857 -0.0421 0.9516 0.067 Uiso 1 1 calc R . . C50 C 0.4935(5) 0.0001(3) 0.8622(4) 0.0570(17) Uani 1 1 d . . . H50 H 0.4469 -0.0292 0.8529 0.068 Uiso 1 1 calc R A . C51 C 0.4806(4) 0.0500(3) 0.8191(4) 0.0486(15) Uani 1 1 d . A . H51 H 0.4249 0.0556 0.7789 0.058 Uiso 1 1 calc R . . C54 C 0.3679(5) 0.3488(3) 0.4656(5) 0.0618(18) Uani 1 1 d . . . H54A H 0.4348 0.3381 0.4696 0.093 Uiso 1 1 calc R . . H54B H 0.3542 0.3588 0.5220 0.093 Uiso 1 1 calc R . . H54C H 0.3549 0.3817 0.4278 0.093 Uiso 1 1 calc R . . C55 C 0.3060(7) 0.2992(5) 0.4308(8) 0.113(4) Uani 1 1 d . . . H55A H 0.3175 0.2654 0.4681 0.135 Uiso 1 1 calc R . . H55B H 0.2380 0.3095 0.4241 0.135 Uiso 1 1 calc R . . O3 O 0.3363(5) 0.2883(3) 0.3469(5) 0.108(2) Uani 1 1 d . . . C56A C 0.2908(6) 0.2460(4) 0.3064(8) 0.097(4) Uani 1 1 d . . . H56A H 0.2215 0.2527 0.2983 0.117 Uiso 1 1 calc R . . H56B H 0.3049 0.2098 0.3377 0.117 Uiso 1 1 calc R . . C57A C 0.3301(10) 0.2439(4) 0.2135(9) 0.136(5) Uani 1 1 d . . . H57A H 0.3285 0.2824 0.1894 0.204 Uiso 1 1 calc R . . H57B H 0.2896 0.2186 0.1748 0.204 Uiso 1 1 calc R . . H57C H 0.3954 0.2296 0.2218 0.204 Uiso 1 1 calc R . . Cl1 Cl 1.07435(10) 0.11754(6) 1.10067(8) 0.0454(3) Uani 1 1 d . A . O4 O 1.0422(4) 0.0799(2) 1.1601(3) 0.0699(14) Uani 1 1 d . . . O5 O 0.9968(3) 0.1312(2) 1.0344(3) 0.0588(12) Uani 1 1 d . . . O6 O 1.1472(4) 0.0917(3) 1.0646(3) 0.094(2) Uani 1 1 d . . . O7 O 1.1075(5) 0.1688(2) 1.1432(4) 0.0861(18) Uani 1 1 d . . . Cl2A Cl 0.2827(3) -0.0890(2) 0.7257(3) 0.0415(8) Uani 0.70 1 d PD F 1 O8A O 0.2442(6) -0.0620(3) 0.7906(4) 0.0865(12) Uiso 0.70 1 d PD F 1 O9A O 0.2147(6) -0.1212(4) 0.6713(5) 0.0865(12) Uiso 0.70 1 d PD F 1 O10A O 0.3234(6) -0.0468(3) 0.6781(5) 0.0865(12) Uiso 0.70 1 d PD F 1 O11A O 0.3557(6) -0.1266(4) 0.7639(5) 0.0865(12) Uiso 0.70 1 d PD F 1 Cl2B Cl 0.3004(8) -0.0969(6) 0.7022(7) 0.067(3) Uani 0.30 1 d PD G 2 O8B O 0.3441(11) -0.1194(7) 0.6345(8) 0.0865(12) Uiso 0.30 1 d PD G 2 O9B O 0.1992(9) -0.1010(9) 0.6913(11) 0.0865(12) Uiso 0.30 1 d PD G 2 O10B O 0.3007(16) -0.0335(7) 0.7008(11) 0.0865(12) Uiso 0.30 1 d PD G 2 O11B O 0.3471(13) -0.1168(8) 0.7851(11) 0.0865(12) Uiso 0.30 1 d PD G 2 Cl3 Cl 0.33613(9) 0.10203(6) 0.54820(8) 0.0369(3) Uani 1 1 d . . . O12 O 0.2637(3) 0.0627(2) 0.5144(3) 0.0601(12) Uani 1 1 d . . . O13 O 0.3511(5) 0.1380(3) 0.4808(4) 0.108(2) Uani 1 1 d . . . O14 O 0.4185(4) 0.0740(3) 0.5805(6) 0.124(3) Uani 1 1 d . . . O15 O 0.3046(5) 0.1367(4) 0.6074(5) 0.129(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0298(3) 0.0275(3) 0.0245(3) -0.0024(2) 0.0005(2) 0.0011(2) Cu2 0.0286(3) 0.0313(3) 0.0247(3) -0.0021(2) 0.0005(2) 0.0029(2) O1 0.0311(18) 0.0252(17) 0.0291(17) -0.0033(13) 0.0038(14) 0.0023(14) C52 0.050(3) 0.031(3) 0.047(3) -0.008(2) 0.012(3) 0.004(2) O2 0.0319(18) 0.0296(17) 0.0279(17) -0.0094(14) 0.0014(14) 0.0006(14) C53 0.047(3) 0.054(4) 0.057(4) -0.035(3) 0.012(3) -0.008(3) O100 0.048(3) 0.089(4) 0.039(2) 0.016(2) 0.000(2) 0.006(2) C1 0.030(2) 0.023(2) 0.018(2) 0.0023(17) -0.0075(18) 0.0064(19) N2 0.030(2) 0.027(2) 0.0191(18) -0.0015(16) -0.0007(16) 0.0022(17) C3 0.029(2) 0.026(2) 0.018(2) 0.0046(18) -0.0015(18) 0.0040(19) N4 0.033(2) 0.027(2) 0.0196(19) -0.0004(15) -0.0029(16) 0.0021(17) C5 0.030(2) 0.028(2) 0.017(2) 0.0037(18) -0.0035(18) 0.008(2) N6 0.029(2) 0.030(2) 0.0216(19) -0.0006(16) -0.0009(16) 0.0046(17) N7 0.029(2) 0.029(2) 0.0221(19) -0.0040(16) -0.0003(16) 0.0004(17) N8 0.033(2) 0.027(2) 0.028(2) -0.0052(17) -0.0003(17) -0.0018(17) N9 0.028(2) 0.034(2) 0.030(2) -0.0032(18) 0.0049(17) 0.0062(17) C10 0.029(3) 0.033(3) 0.030(3) -0.006(2) -0.007(2) 0.002(2) C11 0.031(3) 0.033(3) 0.027(2) -0.009(2) 0.003(2) -0.005(2) N12 0.029(2) 0.034(2) 0.025(2) -0.0005(17) 0.0030(17) -0.0010(18) C13 0.046(3) 0.050(3) 0.034(3) 0.008(3) 0.007(2) 0.003(3) C14 0.069(5) 0.053(4) 0.049(4) 0.013(3) 0.020(3) -0.002(3) C15 0.051(4) 0.060(4) 0.062(4) -0.002(3) 0.024(3) -0.016(3) C16 0.036(3) 0.050(3) 0.047(3) -0.008(3) 0.008(3) -0.001(3) C17 0.046(3) 0.032(3) 0.018(2) -0.0011(19) 0.006(2) -0.002(2) C18 0.040(3) 0.027(2) 0.025(2) -0.008(2) 0.009(2) -0.003(2) N19 0.032(2) 0.030(2) 0.028(2) -0.0047(17) 0.0065(17) 0.0000(17) C20 0.035(3) 0.039(3) 0.037(3) -0.004(2) 0.004(2) 0.005(2) C21 0.036(3) 0.053(4) 0.059(4) -0.016(3) 0.002(3) 0.010(3) C22 0.043(3) 0.060(4) 0.064(4) -0.017(3) 0.022(3) -0.007(3) C23 0.048(3) 0.042(3) 0.037(3) -0.009(2) 0.020(3) -0.008(3) C24 0.035(3) 0.037(3) 0.027(2) -0.006(2) 0.008(2) -0.005(2) C25 0.029(3) 0.039(3) 0.026(2) -0.010(2) 0.000(2) -0.002(2) N26 0.034(2) 0.032(2) 0.031(2) -0.0062(18) 0.0038(18) 0.0043(18) C27 0.048(3) 0.048(3) 0.033(3) -0.003(2) -0.003(2) 0.012(3) C28 0.048(4) 0.066(4) 0.045(3) -0.004(3) -0.004(3) 0.027(3) C29 0.035(3) 0.082(5) 0.051(4) -0.016(3) 0.005(3) 0.021(3) C30 0.038(3) 0.064(4) 0.034(3) -0.009(3) 0.006(2) 0.003(3) C31 0.041(3) 0.024(2) 0.034(3) -0.004(2) -0.005(2) -0.003(2) C32 0.033(3) 0.031(3) 0.028(2) -0.005(2) 0.004(2) -0.002(2) N33 0.033(2) 0.030(2) 0.031(2) -0.0039(17) 0.0035(18) -0.0036(18) C34 0.033(3) 0.048(3) 0.029(3) -0.004(2) 0.004(2) 0.000(2) C35 0.032(3) 0.054(3) 0.033(3) -0.013(3) 0.000(2) -0.006(2) C36 0.046(3) 0.046(3) 0.044(3) -0.010(3) 0.009(3) -0.018(3) C37 0.047(3) 0.034(3) 0.033(3) -0.003(2) 0.006(2) -0.008(2) C38 0.043(3) 0.035(3) 0.030(3) 0.000(2) 0.008(2) 0.015(2) C39 0.029(3) 0.039(3) 0.030(3) -0.006(2) 0.002(2) 0.003(2) N40 0.030(2) 0.040(2) 0.028(2) -0.0050(18) 0.0011(17) 0.0028(18) C41 0.035(3) 0.051(3) 0.029(3) -0.002(2) 0.003(2) 0.001(2) C42 0.042(3) 0.068(4) 0.031(3) -0.015(3) 0.005(2) 0.000(3) C43 0.052(4) 0.062(4) 0.041(3) -0.019(3) 0.009(3) 0.014(3) C44 0.046(3) 0.045(3) 0.042(3) -0.011(3) 0.007(3) 0.008(3) C45 0.030(3) 0.054(3) 0.029(3) -0.003(2) 0.004(2) 0.004(2) C46 0.032(3) 0.044(3) 0.029(3) -0.010(2) 0.010(2) -0.001(2) N47 0.037(2) 0.038(2) 0.029(2) -0.0040(18) 0.0080(18) 0.0003(19) C48 0.053(4) 0.044(3) 0.039(3) 0.003(3) 0.005(3) -0.001(3) C49 0.076(5) 0.046(4) 0.047(4) 0.002(3) 0.014(3) -0.013(3) C50 0.051(4) 0.059(4) 0.061(4) -0.008(3) 0.011(3) -0.024(3) C51 0.040(3) 0.062(4) 0.045(3) -0.009(3) 0.009(3) -0.008(3) C54 0.071(5) 0.046(4) 0.066(4) 0.001(3) 0.002(4) -0.004(3) C55 0.076(6) 0.128(9) 0.143(10) 0.054(8) 0.044(7) 0.027(6) O3 0.072(4) 0.128(6) 0.122(6) 0.022(5) 0.015(4) 0.014(4) C56A 0.060(5) 0.047(4) 0.183(12) 0.020(6) 0.013(6) -0.009(4) C57A 0.161(12) 0.054(5) 0.168(12) 0.026(7) -0.052(10) -0.021(6) Cl1 0.0481(8) 0.0539(8) 0.0313(7) 0.0082(6) -0.0036(6) 0.0094(7) O4 0.092(4) 0.073(3) 0.043(3) 0.020(2) 0.004(2) -0.004(3) O5 0.044(2) 0.082(3) 0.045(2) 0.020(2) -0.0118(19) 0.005(2) O6 0.069(4) 0.150(6) 0.063(3) 0.018(4) 0.013(3) 0.050(4) O7 0.107(5) 0.073(4) 0.070(3) -0.002(3) -0.013(3) -0.023(3) Cl2A 0.0420(14) 0.0503(17) 0.0319(18) 0.0105(13) 0.0044(12) -0.0068(11) Cl2B 0.076(8) 0.057(5) 0.057(7) 0.021(5) -0.027(5) -0.029(5) Cl3 0.0270(6) 0.0425(7) 0.0410(7) -0.0001(6) 0.0047(5) 0.0049(5) O12 0.042(2) 0.061(3) 0.074(3) -0.002(2) 0.001(2) -0.011(2) O13 0.117(5) 0.110(5) 0.095(5) 0.032(4) 0.014(4) -0.051(4) O14 0.042(3) 0.103(5) 0.212(8) 0.028(5) -0.033(4) 0.021(3) O15 0.109(5) 0.166(7) 0.111(5) -0.081(5) 0.020(4) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.917(3) . ? Cu1 O2 1.919(3) . ? Cu1 N33 2.004(4) . ? Cu1 N26 2.018(4) . ? Cu1 O5 2.824(4) . ? Cu1 Cu2 3.0195(10) . ? Cu2 O1 1.933(3) . ? Cu2 O2 1.934(3) . ? Cu2 N40 1.995(4) . ? Cu2 N47 2.017(4) . ? Cu2 O100 2.474(4) . ? O1 C52 1.410(6) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O2 C53 1.396(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O100 H101 0.92(6) . ? O100 H102 0.90(4) . ? C1 N2 1.339(6) . ? C1 N6 1.343(6) . ? C1 N7 1.360(6) . ? N2 C3 1.341(6) . ? C3 N4 1.332(6) . ? C3 N8 1.365(6) . ? N4 C5 1.327(6) . ? C5 N6 1.344(6) . ? C5 N9 1.380(6) . ? N7 C10 1.449(6) . ? N7 C17 1.459(6) . ? N8 C24 1.446(6) . ? N8 C31 1.460(6) . ? N9 C45 1.446(7) . ? N9 C38 1.460(6) . ? C10 C11 1.504(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.333(6) . ? C11 C16 1.375(7) . ? N12 C13 1.338(7) . ? N12 H12 0.91(3) . ? C13 C14 1.362(9) . ? C13 H13 0.9500 . ? C14 C15 1.365(10) . ? C14 H14 0.9500 . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.502(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N19 1.337(6) . ? C18 C23 1.384(7) . ? N19 C20 1.337(7) . ? C20 C21 1.378(8) . ? C20 H20 0.9500 . ? C21 C22 1.379(9) . ? C21 H21 0.9500 . ? C22 C23 1.377(9) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.516(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N26 1.338(7) . ? C25 C30 1.378(7) . ? N26 C27 1.348(7) . ? C27 C28 1.372(8) . ? C27 H27 0.9500 . ? C28 C29 1.367(9) . ? C28 H28 0.9500 . ? C29 C30 1.369(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.503(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N33 1.342(6) . ? C32 C37 1.382(7) . ? N33 C34 1.349(6) . ? C34 C35 1.366(8) . ? C34 H34 0.9500 . ? C35 C36 1.375(8) . ? C35 H35 0.9500 . ? C36 C37 1.374(8) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.511(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N40 1.335(7) . ? C39 C44 1.392(7) . ? N40 C41 1.348(7) . ? C41 C42 1.378(8) . ? C41 H41 0.9500 . ? C42 C43 1.367(9) . ? C42 H42 0.9500 . ? C43 C44 1.385(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.499(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N47 1.343(7) . ? C46 C51 1.393(8) . ? N47 C48 1.348(7) . ? C48 C49 1.366(9) . ? C48 H48 0.9500 . ? C49 C50 1.384(10) . ? C49 H49 0.9500 . ? C50 C51 1.356(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C54 C55 1.513(13) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O3 1.492(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? O3 C56A 1.302(11) . ? C56A C57A 1.666(16) . ? C56A H56A 0.9900 . ? C56A H56B 0.9900 . ? C57A H57A 0.9800 . ? C57A H57B 0.9800 . ? C57A H57C 0.9800 . ? Cl1 O6 1.401(5) . ? Cl1 O4 1.424(5) . ? Cl1 O7 1.424(5) . ? Cl1 O5 1.444(4) . ? Cl2A O8A 1.398(6) . ? Cl2A O9A 1.416(6) . ? Cl2A O10A 1.423(7) . ? Cl2A O11A 1.426(7) . ? Cl2B O8B 1.430(8) . ? Cl2B O9B 1.432(8) . ? Cl2B O11B 1.46(2) . ? Cl2B O10B 1.486(19) . ? Cl3 O15 1.374(6) . ? Cl3 O14 1.376(5) . ? Cl3 O13 1.410(6) . ? Cl3 O12 1.428(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 O2 76.93(14) . . ? O1 Cu1 N33 170.93(16) . . ? O2 Cu1 N33 94.45(16) . . ? O1 Cu1 N26 99.04(16) . . ? O2 Cu1 N26 174.80(16) . . ? N33 Cu1 N26 89.73(17) . . ? O1 Cu1 O5 87.55(14) . . ? O2 Cu1 O5 82.78(14) . . ? N33 Cu1 O5 94.20(16) . . ? N26 Cu1 O5 93.85(16) . . ? O1 Cu1 Cu2 38.52(10) . . ? O2 Cu1 Cu2 38.57(10) . . ? N33 Cu1 Cu2 132.63(12) . . ? N26 Cu1 Cu2 137.56(12) . . ? O5 Cu1 Cu2 86.59(10) . . ? O1 Cu2 O2 76.21(14) . . ? O1 Cu2 N40 167.02(16) . . ? O2 Cu2 N40 92.41(16) . . ? O1 Cu2 N47 99.11(16) . . ? O2 Cu2 N47 173.02(15) . . ? N40 Cu2 N47 91.62(17) . . ? O1 Cu2 O100 88.49(15) . . ? O2 Cu2 O100 89.15(16) . . ? N40 Cu2 O100 97.69(17) . . ? N47 Cu2 O100 95.96(18) . . ? O1 Cu2 Cu1 38.15(10) . . ? O2 Cu2 Cu1 38.22(10) . . ? N40 Cu2 Cu1 129.82(13) . . ? N47 Cu2 Cu1 136.53(12) . . ? O100 Cu2 Cu1 91.24(11) . . ? C52 O1 Cu1 128.4(3) . . ? C52 O1 Cu2 127.4(3) . . ? Cu1 O1 Cu2 103.32(15) . . ? O1 C52 H52A 109.5 . . ? O1 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O1 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C53 O2 Cu1 127.5(3) . . ? C53 O2 Cu2 128.4(3) . . ? Cu1 O2 Cu2 103.21(15) . . ? O2 C53 H53A 109.5 . . ? O2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Cu2 O100 H101 161(4) . . ? Cu2 O100 H102 91(4) . . ? H101 O100 H102 105.9(16) . . ? N2 C1 N6 126.2(4) . . ? N2 C1 N7 116.2(4) . . ? N6 C1 N7 117.5(4) . . ? C1 N2 C3 113.2(4) . . ? N4 C3 N2 126.2(4) . . ? N4 C3 N8 116.8(4) . . ? N2 C3 N8 116.9(4) . . ? C5 N4 C3 113.2(4) . . ? N4 C5 N6 126.9(4) . . ? N4 C5 N9 117.2(4) . . ? N6 C5 N9 115.8(4) . . ? C1 N6 C5 112.5(4) . . ? C1 N7 C10 120.1(4) . . ? C1 N7 C17 118.8(4) . . ? C10 N7 C17 120.5(4) . . ? C3 N8 C24 120.3(4) . . ? C3 N8 C31 120.2(4) . . ? C24 N8 C31 117.4(4) . . ? C5 N9 C45 119.4(4) . . ? C5 N9 C38 119.9(4) . . ? C45 N9 C38 118.5(4) . . ? N7 C10 C11 113.7(4) . . ? N7 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N7 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N12 C11 C16 119.0(5) . . ? N12 C11 C10 118.2(4) . . ? C16 C11 C10 122.9(5) . . ? C11 N12 C13 122.4(5) . . ? C11 N12 H12 122(4) . . ? C13 N12 H12 115(4) . . ? N12 C13 C14 120.3(6) . . ? N12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 118.7(6) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C16 120.4(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 119.2(6) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? N7 C17 C18 113.7(4) . . ? N7 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? N7 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N19 C18 C23 121.7(5) . . ? N19 C18 C17 117.6(4) . . ? C23 C18 C17 120.5(5) . . ? C18 N19 C20 118.9(4) . . ? N19 C20 C21 122.2(5) . . ? N19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C20 C21 C22 119.1(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 118.7(6) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C18 119.4(6) . . ? C22 C23 H23 120.3 . . ? C18 C23 H23 120.3 . . ? N8 C24 C25 115.5(4) . . ? N8 C24 H24A 108.4 . . ? C25 C24 H24A 108.4 . . ? N8 C24 H24B 108.4 . . ? C25 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? N26 C25 C30 120.3(5) . . ? N26 C25 C24 120.7(4) . . ? C30 C25 C24 118.9(5) . . ? C25 N26 C27 119.0(5) . . ? C25 N26 Cu1 123.9(3) . . ? C27 N26 Cu1 115.4(4) . . ? N26 C27 C28 122.4(6) . . ? N26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 118.7(6) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 118.9(6) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C25 120.6(6) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? N8 C31 C32 112.5(4) . . ? N8 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N8 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? N33 C32 C37 121.5(5) . . ? N33 C32 C31 117.7(4) . . ? C37 C32 C31 120.8(5) . . ? C32 N33 C34 118.6(4) . . ? C32 N33 Cu1 120.9(3) . . ? C34 N33 Cu1 120.5(4) . . ? N33 C34 C35 122.4(5) . . ? N33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C36 118.7(5) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C37 C36 C35 119.6(5) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C32 119.1(5) . . ? C36 C37 H37 120.5 . . ? C32 C37 H37 120.5 . . ? N9 C38 C39 112.6(4) . . ? N9 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? N9 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.8 . . ? N40 C39 C44 121.2(5) . . ? N40 C39 C38 117.8(4) . . ? C44 C39 C38 120.9(5) . . ? C39 N40 C41 119.5(4) . . ? C39 N40 Cu2 119.8(3) . . ? C41 N40 Cu2 120.2(4) . . ? N40 C41 C42 121.6(5) . . ? N40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C43 C42 C41 119.4(5) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 119.3(5) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C39 118.9(6) . . ? C43 C44 H44 120.5 . . ? C39 C44 H44 120.5 . . ? N9 C45 C46 115.8(4) . . ? N9 C45 H45A 108.3 . . ? C46 C45 H45A 108.3 . . ? N9 C45 H45B 108.3 . . ? C46 C45 H45B 108.3 . . ? H45A C45 H45B 107.4 . . ? N47 C46 C51 120.6(5) . . ? N47 C46 C45 120.6(5) . . ? C51 C46 C45 118.8(5) . . ? C46 N47 C48 118.2(5) . . ? C46 N47 Cu2 124.2(4) . . ? C48 N47 Cu2 117.5(4) . . ? N47 C48 C49 123.5(6) . . ? N47 C48 H48 118.3 . . ? C49 C48 H48 118.3 . . ? C48 C49 C50 118.1(6) . . ? C48 C49 H49 121.0 . . ? C50 C49 H49 121.0 . . ? C51 C50 C49 119.2(6) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C50 C51 C46 120.4(6) . . ? C50 C51 H51 119.8 . . ? C46 C51 H51 119.8 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O3 C55 C54 103.2(7) . . ? O3 C55 H55A 111.1 . . ? C54 C55 H55A 111.1 . . ? O3 C55 H55B 111.1 . . ? C54 C55 H55B 111.1 . . ? H55A C55 H55B 109.1 . . ? C56A O3 C55 112.7(9) . . ? O3 C56A C57A 104.8(8) . . ? O3 C56A H56A 110.8 . . ? C57A C56A H56A 110.8 . . ? O3 C56A H56B 110.8 . . ? C57A C56A H56B 110.8 . . ? H56A C56A H56B 108.9 . . ? C56A C57A H57A 109.5 . . ? C56A C57A H57B 109.5 . . ? H57A C57A H57B 109.5 . . ? C56A C57A H57C 109.5 . . ? H57A C57A H57C 109.5 . . ? H57B C57A H57C 109.5 . . ? O6 Cl1 O4 110.0(4) . . ? O6 Cl1 O7 110.3(4) . . ? O4 Cl1 O7 108.8(3) . . ? O6 Cl1 O5 109.1(3) . . ? O4 Cl1 O5 109.8(3) . . ? O7 Cl1 O5 108.8(3) . . ? Cl1 O5 Cu1 153.5(3) . . ? O8A Cl2A O9A 112.7(5) . . ? O8A Cl2A O10A 108.7(5) . . ? O9A Cl2A O10A 109.8(7) . . ? O8A Cl2A O11A 107.9(6) . . ? O9A Cl2A O11A 108.6(5) . . ? O10A Cl2A O11A 109.1(5) . . ? O8B Cl2B O9B 115.6(10) . . ? O8B Cl2B O11B 112.2(8) . . ? O9B Cl2B O11B 113.5(9) . . ? O8B Cl2B O10B 110.8(10) . . ? O9B Cl2B O10B 94.0(15) . . ? O11B Cl2B O10B 109.3(10) . . ? O15 Cl3 O14 112.0(5) . . ? O15 Cl3 O13 106.1(5) . . ? O14 Cl3 O13 110.5(5) . . ? O15 Cl3 O12 110.3(4) . . ? O14 Cl3 O12 111.1(4) . . ? O13 Cl3 O12 106.4(3) . . ? 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 O2 Cu1 Cu2 O1 -173.0(2) . . . . ? N33 Cu1 Cu2 O1 177.1(2) . . . . ? N26 Cu1 Cu2 O1 1.6(2) . . . . ? O5 Cu1 Cu2 O1 -90.35(19) . . . . ? O1 Cu1 Cu2 O2 173.0(2) . . . . ? N33 Cu1 Cu2 O2 -9.9(2) . . . . ? N26 Cu1 Cu2 O2 174.7(2) . . . . ? O5 Cu1 Cu2 O2 82.68(19) . . . . ? O1 Cu1 Cu2 N40 -172.9(2) . . . . ? O2 Cu1 Cu2 N40 14.0(2) . . . . ? N33 Cu1 Cu2 N40 4.1(2) . . . . ? N26 Cu1 Cu2 N40 -171.3(2) . . . . ? O5 Cu1 Cu2 N40 96.71(19) . . . . ? O1 Cu1 Cu2 N47 -14.0(2) . . . . ? O2 Cu1 Cu2 N47 172.9(2) . . . . ? N33 Cu1 Cu2 N47 163.1(2) . . . . ? N26 Cu1 Cu2 N47 -12.4(3) . . . . ? O5 Cu1 Cu2 N47 -104.4(2) . . . . ? O1 Cu1 Cu2 O100 86.0(2) . . . . ? O2 Cu1 Cu2 O100 -87.1(2) . . . . ? N33 Cu1 Cu2 O100 -96.9(2) . . . . ? N26 Cu1 Cu2 O100 87.6(2) . . . . ? O5 Cu1 Cu2 O100 -4.37(17) . . . . ? O2 Cu1 O1 C52 -165.7(4) . . . . ? N26 Cu1 O1 C52 10.9(4) . . . . ? O5 Cu1 O1 C52 -82.6(4) . . . . ? Cu2 Cu1 O1 C52 -170.2(5) . . . . ? O2 Cu1 O1 Cu2 4.45(14) . . . . ? N26 Cu1 O1 Cu2 -178.89(16) . . . . ? O5 Cu1 O1 Cu2 87.60(16) . . . . ? O2 Cu2 O1 C52 165.9(4) . . . . ? N40 Cu2 O1 C52 -164.8(6) . . . . ? N47 Cu2 O1 C52 -19.4(4) . . . . ? O100 Cu2 O1 C52 76.4(4) . . . . ? Cu1 Cu2 O1 C52 170.3(5) . . . . ? O2 Cu2 O1 Cu1 -4.43(14) . . . . ? N40 Cu2 O1 Cu1 24.9(7) . . . . ? N47 Cu2 O1 Cu1 170.28(16) . . . . ? O100 Cu2 O1 Cu1 -93.93(18) . . . . ? O1 Cu1 O2 C53 165.3(5) . . . . ? N33 Cu1 O2 C53 -17.6(5) . . . . ? O5 Cu1 O2 C53 76.1(5) . . . . ? Cu2 Cu1 O2 C53 169.7(5) . . . . ? O1 Cu1 O2 Cu2 -4.45(14) . . . . ? N33 Cu1 O2 Cu2 172.72(17) . . . . ? O5 Cu1 O2 Cu2 -93.60(16) . . . . ? O1 Cu2 O2 C53 -165.2(5) . . . . ? N40 Cu2 O2 C53 21.2(5) . . . . ? O100 Cu2 O2 C53 -76.5(5) . . . . ? Cu1 Cu2 O2 C53 -169.6(5) . . . . ? O1 Cu2 O2 Cu1 4.43(14) . . . . ? N40 Cu2 O2 Cu1 -169.26(17) . . . . ? O100 Cu2 O2 Cu1 93.08(17) . . . . ? N6 C1 N2 C3 -8.4(6) . . . . ? N7 C1 N2 C3 173.0(4) . . . . ? C1 N2 C3 N4 -4.3(6) . . . . ? C1 N2 C3 N8 171.8(4) . . . . ? N2 C3 N4 C5 12.9(6) . . . . ? N8 C3 N4 C5 -163.3(4) . . . . ? C3 N4 C5 N6 -10.6(6) . . . . ? C3 N4 C5 N9 167.0(4) . . . . ? N2 C1 N6 C5 10.3(6) . . . . ? N7 C1 N6 C5 -171.1(4) . . . . ? N4 C5 N6 C1 0.1(6) . . . . ? N9 C5 N6 C1 -177.5(4) . . . . ? N2 C1 N7 C10 179.4(4) . . . . ? N6 C1 N7 C10 0.6(6) . . . . ? N2 C1 N7 C17 -9.0(6) . . . . ? N6 C1 N7 C17 172.3(4) . . . . ? N4 C3 N8 C24 174.2(4) . . . . ? N2 C3 N8 C24 -2.3(6) . . . . ? N4 C3 N8 C31 -22.5(6) . . . . ? N2 C3 N8 C31 161.0(4) . . . . ? N4 C5 N9 C45 178.3(4) . . . . ? N6 C5 N9 C45 -3.9(6) . . . . ? N4 C5 N9 C38 15.3(6) . . . . ? N6 C5 N9 C38 -166.8(4) . . . . ? C1 N7 C10 C11 -83.9(5) . . . . ? C17 N7 C10 C11 104.6(5) . . . . ? N7 C10 C11 N12 -22.4(6) . . . . ? N7 C10 C11 C16 159.2(5) . . . . ? C16 C11 N12 C13 -0.4(7) . . . . ? C10 C11 N12 C13 -178.8(5) . . . . ? C11 N12 C13 C14 0.0(8) . . . . ? N12 C13 C14 C15 0.8(10) . . . . ? C13 C14 C15 C16 -1.2(10) . . . . ? N12 C11 C16 C15 0.0(8) . . . . ? C10 C11 C16 C15 178.4(5) . . . . ? C14 C15 C16 C11 0.8(10) . . . . ? C1 N7 C17 C18 70.0(5) . . . . ? C10 N7 C17 C18 -118.4(5) . . . . ? N7 C17 C18 N19 35.4(6) . . . . ? N7 C17 C18 C23 -148.1(5) . . . . ? C23 C18 N19 C20 1.7(7) . . . . ? C17 C18 N19 C20 178.1(4) . . . . ? C18 N19 C20 C21 -2.6(7) . . . . ? N19 C20 C21 C22 2.2(9) . . . . ? C20 C21 C22 C23 -0.9(9) . . . . ? C21 C22 C23 C18 0.1(9) . . . . ? N19 C18 C23 C22 -0.5(8) . . . . ? C17 C18 C23 C22 -176.8(5) . . . . ? C3 N8 C24 C25 -90.7(5) . . . . ? C31 N8 C24 C25 105.6(5) . . . . ? N8 C24 C25 N26 7.3(7) . . . . ? N8 C24 C25 C30 -175.4(5) . . . . ? C30 C25 N26 C27 -2.0(7) . . . . ? C24 C25 N26 C27 175.3(5) . . . . ? C30 C25 N26 Cu1 162.4(4) . . . . ? C24 C25 N26 Cu1 -20.3(6) . . . . ? O1 Cu1 N26 C25 120.8(4) . . . . ? N33 Cu1 N26 C25 -56.9(4) . . . . ? O5 Cu1 N26 C25 -151.1(4) . . . . ? Cu2 Cu1 N26 C25 119.8(4) . . . . ? O1 Cu1 N26 C27 -74.3(4) . . . . ? N33 Cu1 N26 C27 108.0(4) . . . . ? O5 Cu1 N26 C27 13.9(4) . . . . ? Cu2 Cu1 N26 C27 -75.3(4) . . . . ? C25 N26 C27 C28 1.5(8) . . . . ? Cu1 N26 C27 C28 -164.3(5) . . . . ? N26 C27 C28 C29 0.5(10) . . . . ? C27 C28 C29 C30 -1.8(10) . . . . ? C28 C29 C30 C25 1.2(10) . . . . ? N26 C25 C30 C29 0.7(8) . . . . ? C24 C25 C30 C29 -176.6(5) . . . . ? C3 N8 C31 C32 135.0(5) . . . . ? C24 N8 C31 C32 -61.3(6) . . . . ? N8 C31 C32 N33 -42.1(6) . . . . ? N8 C31 C32 C37 138.8(5) . . . . ? C37 C32 N33 C34 0.9(7) . . . . ? C31 C32 N33 C34 -178.2(5) . . . . ? C37 C32 N33 Cu1 -178.8(4) . . . . ? C31 C32 N33 Cu1 2.1(6) . . . . ? O2 Cu1 N33 C32 -91.6(4) . . . . ? N26 Cu1 N33 C32 91.5(4) . . . . ? O5 Cu1 N33 C32 -174.7(4) . . . . ? Cu2 Cu1 N33 C32 -85.5(4) . . . . ? O2 Cu1 N33 C34 88.7(4) . . . . ? N26 Cu1 N33 C34 -88.2(4) . . . . ? O5 Cu1 N33 C34 5.6(4) . . . . ? Cu2 Cu1 N33 C34 94.9(4) . . . . ? C32 N33 C34 C35 -0.6(8) . . . . ? Cu1 N33 C34 C35 179.1(4) . . . . ? N33 C34 C35 C36 0.0(8) . . . . ? C34 C35 C36 C37 0.4(9) . . . . ? C35 C36 C37 C32 -0.2(9) . . . . ? N33 C32 C37 C36 -0.5(8) . . . . ? C31 C32 C37 C36 178.6(5) . . . . ? C5 N9 C38 C39 -137.9(4) . . . . ? C45 N9 C38 C39 59.0(6) . . . . ? N9 C38 C39 N40 37.9(7) . . . . ? N9 C38 C39 C44 -145.4(5) . . . . ? C44 C39 N40 C41 1.8(8) . . . . ? C38 C39 N40 C41 178.5(5) . . . . ? C44 C39 N40 Cu2 -170.6(4) . . . . ? C38 C39 N40 Cu2 6.1(6) . . . . ? O1 Cu2 N40 C39 48.3(9) . . . . ? O2 Cu2 N40 C39 76.7(4) . . . . ? N47 Cu2 N40 C39 -97.6(4) . . . . ? O100 Cu2 N40 C39 166.2(4) . . . . ? Cu1 Cu2 N40 C39 68.1(4) . . . . ? O1 Cu2 N40 C41 -124.1(7) . . . . ? O2 Cu2 N40 C41 -95.7(4) . . . . ? N47 Cu2 N40 C41 90.0(4) . . . . ? O100 Cu2 N40 C41 -6.2(4) . . . . ? Cu1 Cu2 N40 C41 -104.3(4) . . . . ? C39 N40 C41 C42 -1.9(8) . . . . ? Cu2 N40 C41 C42 170.5(4) . . . . ? N40 C41 C42 C43 0.9(9) . . . . ? C41 C42 C43 C44 0.2(9) . . . . ? C42 C43 C44 C39 -0.2(9) . . . . ? N40 C39 C44 C43 -0.7(9) . . . . ? C38 C39 C44 C43 -177.3(6) . . . . ? C5 N9 C45 C46 78.9(6) . . . . ? C38 N9 C45 C46 -118.0(5) . . . . ? N9 C45 C46 N47 14.5(7) . . . . ? N9 C45 C46 C51 -167.6(5) . . . . ? C51 C46 N47 C48 0.1(7) . . . . ? C45 C46 N47 C48 177.9(5) . . . . ? C51 C46 N47 Cu2 -175.5(4) . . . . ? C45 C46 N47 Cu2 2.3(6) . . . . ? O1 Cu2 N47 C46 -109.9(4) . . . . ? N40 Cu2 N47 C46 62.8(4) . . . . ? O100 Cu2 N47 C46 160.7(4) . . . . ? Cu1 Cu2 N47 C46 -101.2(4) . . . . ? O1 Cu2 N47 C48 74.5(4) . . . . ? N40 Cu2 N47 C48 -112.8(4) . . . . ? O100 Cu2 N47 C48 -14.9(4) . . . . ? Cu1 Cu2 N47 C48 83.2(4) . . . . ? C46 N47 C48 C49 -1.9(8) . . . . ? Cu2 N47 C48 C49 174.0(5) . . . . ? N47 C48 C49 C50 2.4(10) . . . . ? C48 C49 C50 C51 -1.0(10) . . . . ? C49 C50 C51 C46 -0.6(10) . . . . ? N47 C46 C51 C50 1.2(9) . . . . ? C45 C46 C51 C50 -176.8(5) . . . . ? C54 C55 O3 C56A 179.6(7) . . . . ? C55 O3 C56A C57A 176.6(7) . . . . ? O6 Cl1 O5 Cu1 -46.3(8) . . . . ? O4 Cl1 O5 Cu1 -167.0(6) . . . . ? O7 Cl1 O5 Cu1 74.1(7) . . . . ? O1 Cu1 O5 Cl1 144.0(7) . . . . ? O2 Cu1 O5 Cl1 -138.9(7) . . . . ? N33 Cu1 O5 Cl1 -44.9(7) . . . . ? N26 Cu1 O5 Cl1 45.1(7) . . . . ? Cu2 Cu1 O5 Cl1 -177.5(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O100 H101 O8A 0.92(6) 2.07(5) 2.818(8) 139(6) 3_657 O100 H102 O5 0.90(4) 2.037(16) 2.932(7) 173(6) . N12 H12 N19 0.91(3) 1.82(3) 2.724(6) 176(5) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.497 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.096 # Attachment 'cu3BAMONOx.CIF' data_bamono _database_code_depnum_ccdc_archive 'CCDC 718369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H38 Cl2 Cu2 N6), 4(F6 P), C H2 Cl2' _chemical_formula_sum ' C77 H78 Cl6 Cu4 F24 N12 P4 ' _chemical_formula_weight 2218.29 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.347(2) _cell_length_b 14.191(2) _cell_length_c 14.720(2) _cell_angle_alpha 90.000 _cell_angle_beta 115.575(17) _cell_angle_gamma 90.00 _cell_volume 2514.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 221 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 21.46 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'SADABS version 2.03.(Sheldrick,Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18022 _diffrn_reflns_av_R_equivalents 0.1935 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3139 _reflns_number_gt 1597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal-99 (E.Keller 1999)' _computing_publication_material 'XCIF 6.12 (Sheldrick, 1997)' _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^)+(0.1590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3139 _refine_ls_number_parameters 280 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1653 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2584 _refine_ls_wR_factor_gt 0.2205 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4467(11) 0.4441(10) 0.1985(10) 0.076(4) Uani 1 1 d . . . H1 H 0.4684 0.5069 0.2070 0.091 Uiso 1 1 calc R . . C2 C 0.3747(11) 0.4132(12) 0.2372(11) 0.085(4) Uani 1 1 d . . . H2 H 0.3496 0.4541 0.2722 0.102 Uiso 1 1 calc R . . C3 C 0.3410(11) 0.3201(13) 0.2226(11) 0.085(4) Uani 1 1 d . . . H3 H 0.2914 0.2977 0.2465 0.102 Uiso 1 1 calc R . . C4 C 0.3822(11) 0.2601(11) 0.1715(11) 0.081(4) Uani 1 1 d . . . H4 H 0.3615 0.1970 0.1620 0.098 Uiso 1 1 calc R . . C5 C 0.4539(10) 0.2958(8) 0.1353(9) 0.062(3) Uani 1 1 d . . . C6 C 0.5002(10) 0.2385(7) 0.0764(10) 0.062(3) Uani 1 1 d . . . H6A H 0.5121 0.1742 0.1012 0.074 Uiso 1 1 calc R . . H6B H 0.4472 0.2373 0.0061 0.074 Uiso 1 1 calc R . . C7 C 0.6262(12) 0.2595(8) -0.0044(10) 0.071(4) Uani 1 1 d . . . H7A H 0.5562 0.2588 -0.0645 0.085 Uiso 1 1 calc R . . H7B H 0.6616 0.1986 0.0020 0.085 Uiso 1 1 calc R . . C8 C 0.7001(10) 0.3359(9) -0.0123(9) 0.061(3) Uani 1 1 d . . . C9 C 0.7663(13) 0.3236(12) -0.0634(12) 0.088(4) Uani 1 1 d . . . H9 H 0.7681 0.2655 -0.0918 0.105 Uiso 1 1 calc R . . C10 C 0.8266(14) 0.3948(13) -0.0714(12) 0.092(5) Uani 1 1 d . . . H10 H 0.8697 0.3867 -0.1064 0.111 Uiso 1 1 calc R . . C11 C 0.8252(13) 0.4832(14) -0.0266(12) 0.098(5) Uani 1 1 d . . . H11 H 0.8676 0.5339 -0.0302 0.118 Uiso 1 1 calc R . . C12 C 0.7577(11) 0.4898(10) 0.0224(11) 0.073(4) Uani 1 1 d . . . H12 H 0.7548 0.5471 0.0519 0.088 Uiso 1 1 calc R . . C13 C 0.7073(11) 0.2427(10) 0.1788(10) 0.075(4) Uani 1 1 d . . . H13A H 0.7744 0.2557 0.1708 0.090 Uiso 1 1 calc R . . H13B H 0.7013 0.1750 0.1837 0.090 Uiso 1 1 calc R . . C14 C 0.7163(10) 0.2890(9) 0.2767(9) 0.064(3) Uani 1 1 d . . . C15 C 0.7633(11) 0.3764(9) 0.3058(11) 0.072(4) Uani 1 1 d . . . H15 H 0.7920 0.4086 0.2672 0.086 Uiso 1 1 calc R . . C16 C 0.7676(13) 0.4154(12) 0.3919(14) 0.101(5) Uani 1 1 d . . . H16 H 0.8048 0.4721 0.4148 0.122 Uiso 1 1 calc R . . C17 C 0.7178(14) 0.3724(16) 0.4456(14) 0.106(5) Uani 1 1 d . . . H17 H 0.7184 0.4016 0.5024 0.127 Uiso 1 1 calc R . . C18 C 0.6670(13) 0.2860(14) 0.4152(12) 0.091(5) Uani 1 1 d . . . H18 H 0.6338 0.2566 0.4518 0.109 Uiso 1 1 calc R . . C19 C 0.6655(11) 0.2432(10) 0.3302(11) 0.074(4) Uani 1 1 d . . . H19 H 0.6314 0.1850 0.3089 0.089 Uiso 1 1 calc R . . N1 N 0.4865(7) 0.3862(6) 0.1489(7) 0.053(2) Uani 1 1 d . . . N2 N 0.6065(8) 0.2788(6) 0.0858(7) 0.056(2) Uani 1 1 d . . . N3 N 0.6962(7) 0.4186(7) 0.0301(7) 0.057(2) Uani 1 1 d . . . F1 F -0.0353(19) 0.5189(14) 0.2532(18) 0.125(2) Uani 0.50 1 d P A 1 F2 F 0.178(2) 0.3977(15) 0.3384(19) 0.125(2) Uani 0.50 1 d P A 1 F3 F 0.098(2) 0.4150(16) 0.189(2) 0.125(2) Uani 0.50 1 d P A 1 F4 F 0.148(2) 0.5428(17) 0.2827(19) 0.125(2) Uani 0.50 1 d P A 1 F5 F 0.080(2) 0.4500(15) 0.3946(18) 0.125(2) Uani 0.50 1 d P A 1 F6 F 0.003(2) 0.3591(15) 0.2791(18) 0.125(2) Uani 0.50 1 d P A 1 F1A F 0.0030(19) 0.5405(15) 0.2134(18) 0.125(2) Uani 0.50 1 d P A 2 F2A F 0.143(2) 0.3561(15) 0.3098(19) 0.125(2) Uani 0.50 1 d P A 2 F3A F 0.060(2) 0.4447(17) 0.170(2) 0.125(2) Uani 0.50 1 d P A 2 F4A F 0.180(2) 0.5141(16) 0.321(2) 0.125(2) Uani 0.50 1 d P A 2 F5A F 0.060(2) 0.4992(14) 0.3669(19) 0.125(2) Uani 0.50 1 d P A 2 F6A F -0.0383(19) 0.3965(15) 0.2291(18) 0.125(2) Uani 0.50 1 d P A 2 P1 P 0.0700(3) 0.4535(3) 0.2782(3) 0.0765(11) Uani 1 1 d . . . Cl1 Cl 0.5880(2) 0.5780(2) 0.1095(2) 0.0659(9) Uani 1 1 d . . . Cu1 Cu 0.58994(11) 0.42090(9) 0.08965(11) 0.0527(5) Uani 1 1 d . . . C20 C -0.0035(17) 0.185(2) 0.140(3) 0.058(12) Uiso 0.25 1 d PD . . H20A H -0.0180 0.2459 0.1063 0.069 Uiso 0.25 1 calc PR . . H20B H -0.0066 0.1945 0.2044 0.069 Uiso 0.25 1 calc PR . . Cl2 Cl 0.1257(11) 0.1508(10) 0.1626(12) 0.091(4) Uiso 0.25 1 d PD . . Cl3 Cl -0.1061(11) 0.1087(11) 0.0693(13) 0.099(5) Uiso 0.25 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.078(9) 0.082(10) 0.063(10) 0.003(7) 0.027(8) 0.013(7) C2 0.077(9) 0.116(13) 0.075(11) -0.006(9) 0.046(8) -0.002(9) C3 0.068(9) 0.119(13) 0.073(12) 0.007(9) 0.037(9) -0.001(9) C4 0.077(9) 0.085(10) 0.075(11) 0.017(8) 0.026(9) -0.021(8) C5 0.071(8) 0.052(8) 0.060(9) -0.005(6) 0.026(7) -0.003(6) C6 0.079(8) 0.038(6) 0.068(9) -0.003(6) 0.031(7) -0.008(6) C7 0.096(10) 0.053(7) 0.067(10) -0.009(6) 0.039(8) 0.008(7) C8 0.065(8) 0.072(9) 0.047(9) 0.004(6) 0.025(7) 0.012(6) C9 0.100(11) 0.097(11) 0.080(12) 0.005(8) 0.052(10) 0.014(9) C10 0.097(11) 0.121(14) 0.078(12) 0.014(10) 0.055(10) 0.019(10) C11 0.076(10) 0.145(17) 0.062(12) 0.017(10) 0.019(9) -0.010(10) C12 0.068(8) 0.082(10) 0.070(10) 0.015(7) 0.029(8) 0.010(8) C13 0.080(9) 0.087(9) 0.056(10) 0.018(7) 0.027(8) 0.038(7) C14 0.061(7) 0.078(9) 0.044(8) 0.023(6) 0.013(6) 0.029(7) C15 0.080(9) 0.060(8) 0.075(11) 0.010(7) 0.032(8) -0.002(7) C16 0.082(11) 0.109(12) 0.085(14) -0.027(11) 0.010(10) -0.005(9) C17 0.086(12) 0.143(17) 0.075(14) -0.003(12) 0.024(10) 0.026(12) C18 0.080(10) 0.133(15) 0.062(12) 0.029(10) 0.033(9) 0.017(10) C19 0.079(9) 0.074(9) 0.071(11) 0.026(7) 0.033(8) 0.016(7) N1 0.059(6) 0.054(6) 0.045(7) 0.007(4) 0.022(5) 0.010(4) N2 0.071(7) 0.054(5) 0.046(7) -0.006(4) 0.027(5) 0.004(5) N3 0.057(6) 0.054(6) 0.058(7) -0.002(5) 0.022(5) -0.012(5) F1 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F2 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F3 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F4 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F5 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F6 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F1A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F2A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F3A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F4A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F5A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) F6A 0.144(6) 0.106(6) 0.122(6) 0.018(4) 0.055(5) 0.011(4) P1 0.078(2) 0.074(2) 0.081(3) -0.007(2) 0.038(2) 0.001(2) Cl1 0.0749(19) 0.0520(16) 0.064(2) -0.0072(15) 0.0238(17) -0.0069(16) Cu1 0.0576(9) 0.0464(8) 0.0541(10) -0.0030(7) 0.0240(7) -0.0012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.351(15) . ? C1 C2 1.382(18) . ? C1 H1 0.9300 . ? C2 C3 1.381(19) . ? C2 H2 0.9300 . ? C3 C4 1.396(19) . ? C3 H3 0.9300 . ? C4 C5 1.378(17) . ? C4 H4 0.9300 . ? C5 N1 1.342(14) . ? C5 C6 1.502(16) . ? C6 N2 1.480(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.487(14) . ? C7 C8 1.503(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.340(14) . ? C8 C9 1.397(17) . ? C9 C10 1.33(2) . ? C9 H9 0.9300 . ? C10 C11 1.42(2) . ? C10 H10 0.9300 . ? C11 C12 1.38(2) . ? C11 H11 0.9300 . ? C12 N3 1.336(15) . ? C12 H12 0.9300 . ? C13 N2 1.535(15) . ? C13 C14 1.542(18) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.372(17) . ? C14 C19 1.401(17) . ? C15 C16 1.36(2) . ? C15 H15 0.9300 . ? C16 C17 1.38(2) . ? C16 H16 0.9300 . ? C17 C18 1.38(2) . ? C17 H17 0.9300 . ? C18 C19 1.38(2) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? N1 Cu1 1.987(9) . ? N2 Cu1 2.032(9) . ? N3 Cu1 1.964(9) . ? F1 P1 1.59(2) . ? F2 P1 1.55(2) . ? F3 P1 1.61(3) . ? F4 P1 1.63(3) . ? F5 P1 1.66(2) . ? F6 P1 1.61(2) . ? F1A P1 1.58(2) . ? F2A P1 1.64(2) . ? F3A P1 1.54(3) . ? F4A P1 1.58(3) . ? F5A P1 1.51(2) . ? F6A P1 1.54(2) . ? Cl1 Cu1 2.250(3) . ? C20 Cl2 1.683(19) . ? C20 Cl3 1.709(19) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.4(13) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.5(13) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.3(13) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 119.0(13) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.9(12) . . ? N1 C5 C6 114.6(10) . . ? C4 C5 C6 123.5(11) . . ? N2 C6 C5 110.7(9) . . ? N2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 108.1(9) . . ? N2 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? N2 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N3 C8 C9 121.4(12) . . ? N3 C8 C7 116.0(10) . . ? C9 C8 C7 122.6(12) . . ? C10 C9 C8 120.1(15) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0(14) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 116.4(15) . . ? C12 C11 H11 121.8 . . ? C10 C11 H11 121.8 . . ? N3 C12 C11 123.8(14) . . ? N3 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? N2 C13 C14 112.1(9) . . ? N2 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N2 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C19 120.8(13) . . ? C15 C14 C13 121.2(12) . . ? C19 C14 C13 117.8(13) . . ? C16 C15 C14 119.2(14) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.2(16) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 120.0(17) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 119.8(15) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C14 118.9(15) . . ? C18 C19 H19 120.6 . . ? C14 C19 H19 120.6 . . ? C5 N1 C1 118.9(10) . . ? C5 N1 Cu1 114.4(7) . . ? C1 N1 Cu1 126.7(9) . . ? C6 N2 C7 112.2(9) . . ? C6 N2 C13 113.0(9) . . ? C7 N2 C13 108.1(9) . . ? C6 N2 Cu1 105.9(6) . . ? C7 N2 Cu1 105.7(7) . . ? C13 N2 Cu1 111.7(7) . . ? C12 N3 C8 118.3(10) . . ? C12 N3 Cu1 127.8(9) . . ? C8 N3 Cu1 113.7(7) . . ? F5A P1 F6A 102.6(13) . . ? F5A P1 F3A 157.5(11) . . ? F6A P1 F3A 80.1(14) . . ? F5A P1 F2 97.6(13) . . ? F6A P1 F2 117.1(12) . . ? F3A P1 F2 100.9(12) . . ? F5A P1 F4A 80.6(13) . . ? F6A P1 F4A 175.8(12) . . ? F3A P1 F4A 95.9(15) . . ? F2 P1 F4A 64.7(11) . . ? F5A P1 F1A 87.2(12) . . ? F6A P1 F1A 87.4(12) . . ? F3A P1 F1A 70.6(12) . . ? F2 P1 F1A 152.9(13) . . ? F4A P1 F1A 90.0(11) . . ? F5A P1 F1 63.5(12) . . ? F6A P1 F1 68.9(11) . . ? F3A P1 F1 97.8(12) . . ? F2 P1 F1 161.1(13) . . ? F4A P1 F1 110.6(12) . . ? F5A P1 F3 170.9(13) . . ? F6A P1 F3 86.4(13) . . ? F2 P1 F3 78.8(12) . . ? F4A P1 F3 90.3(14) . . ? F1A P1 F3 92.3(12) . . ? F1 P1 F3 120.1(12) . . ? F5A P1 F6 95.6(12) . . ? F3A P1 F6 97.9(13) . . ? F2 P1 F6 87.3(12) . . ? F4A P1 F6 150.7(11) . . ? F1A P1 F6 119.0(12) . . ? F1 P1 F6 93.0(12) . . ? F3 P1 F6 92.7(13) . . ? F5A P1 F4 85.7(12) . . ? F6A P1 F4 152.5(12) . . ? F3A P1 F4 82.7(13) . . ? F2 P1 F4 87.1(12) . . ? F1A P1 F4 66.6(11) . . ? F1 P1 F4 92.5(11) . . ? F3 P1 F4 85.8(14) . . ? F6 P1 F4 174.3(11) . . ? F5A P1 F2A 112.3(12) . . ? F6A P1 F2A 90.8(12) . . ? F3A P1 F2A 89.9(12) . . ? F4A P1 F2A 90.5(11) . . ? F1A P1 F2A 160.4(13) . . ? F1 P1 F2A 156.5(12) . . ? F3 P1 F2A 68.0(11) . . ? F6 P1 F2A 63.9(11) . . ? F4 P1 F2A 110.5(12) . . ? F6A P1 F5 96.3(12) . . ? F3A P1 F5 173.6(12) . . ? F2 P1 F5 75.9(12) . . ? F4A P1 F5 87.8(13) . . ? F1A P1 F5 114.8(12) . . ? F1 P1 F5 85.8(11) . . ? F3 P1 F5 152.8(11) . . ? F6 P1 F5 76.4(11) . . ? F4 P1 F5 102.6(12) . . ? F2A P1 F5 84.9(11) . . ? N3 Cu1 N1 164.7(4) . . ? N3 Cu1 N2 82.1(4) . . ? N1 Cu1 N2 82.6(4) . . ? N3 Cu1 Cl1 97.2(3) . . ? N1 Cu1 Cl1 98.0(3) . . ? N2 Cu1 Cl1 173.9(3) . . ? Cl2 C20 Cl3 114.6(15) . . ? Cl2 C20 H20A 108.6 . . ? Cl3 C20 H20A 108.6 . . ? Cl2 C20 H20B 108.6 . . ? Cl3 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1(2) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 N1 1(2) . . . . ? C3 C4 C5 C6 -178.0(13) . . . . ? N1 C5 C6 N2 25.6(15) . . . . ? C4 C5 C6 N2 -155.4(12) . . . . ? N2 C7 C8 N3 -25.7(15) . . . . ? N2 C7 C8 C9 156.5(12) . . . . ? N3 C8 C9 C10 0(2) . . . . ? C7 C8 C9 C10 177.3(13) . . . . ? C8 C9 C10 C11 1(2) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? C10 C11 C12 N3 1(2) . . . . ? N2 C13 C14 C15 -82.0(15) . . . . ? N2 C13 C14 C19 92.1(13) . . . . ? C19 C14 C15 C16 5(2) . . . . ? C13 C14 C15 C16 178.7(12) . . . . ? C14 C15 C16 C17 -5(2) . . . . ? C15 C16 C17 C18 3(3) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C17 C18 C19 C14 0(2) . . . . ? C15 C14 C19 C18 -2.3(19) . . . . ? C13 C14 C19 C18 -176.4(11) . . . . ? C4 C5 N1 C1 -0.9(18) . . . . ? C6 C5 N1 C1 178.1(11) . . . . ? C4 C5 N1 Cu1 -179.9(10) . . . . ? C6 C5 N1 Cu1 -0.9(13) . . . . ? C2 C1 N1 C5 1.1(19) . . . . ? C2 C1 N1 Cu1 180.0(10) . . . . ? C5 C6 N2 C7 -150.9(10) . . . . ? C5 C6 N2 C13 86.6(12) . . . . ? C5 C6 N2 Cu1 -36.0(11) . . . . ? C8 C7 N2 C6 153.6(9) . . . . ? C8 C7 N2 C13 -81.2(12) . . . . ? C8 C7 N2 Cu1 38.6(11) . . . . ? C14 C13 N2 C6 -75.7(13) . . . . ? C14 C13 N2 C7 159.5(11) . . . . ? C14 C13 N2 Cu1 43.6(13) . . . . ? C11 C12 N3 C8 0.0(19) . . . . ? C11 C12 N3 Cu1 -175.7(11) . . . . ? C9 C8 N3 C12 -0.1(19) . . . . ? C7 C8 N3 C12 -177.9(11) . . . . ? C9 C8 N3 Cu1 176.2(10) . . . . ? C7 C8 N3 Cu1 -1.7(14) . . . . ? C12 N3 Cu1 N1 -164.5(13) . . . . ? C8 N3 Cu1 N1 20(2) . . . . ? C12 N3 Cu1 N2 -164.4(11) . . . . ? C8 N3 Cu1 N2 19.8(8) . . . . ? C12 N3 Cu1 Cl1 9.5(10) . . . . ? C8 N3 Cu1 Cl1 -166.3(8) . . . . ? C5 N1 Cu1 N3 -16.1(19) . . . . ? C1 N1 Cu1 N3 165.0(13) . . . . ? C5 N1 Cu1 N2 -16.2(8) . . . . ? C1 N1 Cu1 N2 164.9(11) . . . . ? C5 N1 Cu1 Cl1 170.0(7) . . . . ? C1 N1 Cu1 Cl1 -9.0(10) . . . . ? C6 N2 Cu1 N3 -151.6(8) . . . . ? C7 N2 Cu1 N3 -32.3(8) . . . . ? C13 N2 Cu1 N3 85.0(8) . . . . ? C6 N2 Cu1 N1 28.4(7) . . . . ? C7 N2 Cu1 N1 147.6(8) . . . . ? C13 N2 Cu1 N1 -95.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.880 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.134 # Attachment 'NEWCu6GLOE1A.CIF' data_gloe1a _database_code_depnum_ccdc_archive 'CCDC 718370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H25 Cl2 Cu N3 O9),(H2 O)' _chemical_formula_sum 'C54 H52 Cl4 Cu2 N6 O19' _chemical_formula_weight 1357.90 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1257(3) _cell_length_b 10.5924(2) _cell_length_c 36.7101(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.343(1) _cell_angle_gamma 90.00 _cell_volume 5419.88(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2521 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 33.25 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details 'SADABS (Sheldrick,1999-2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex 2 CCD ' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 118862 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 31.56 _reflns_number_total 17776 _reflns_number_gt 9736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (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^)+(0.0256P)^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_number_reflns 17776 _refine_ls_number_parameters 784 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.85897(17) 0.5774(2) 0.17114(7) 0.0191(6) Uani 1 1 d . . . C2 C 0.89478(19) 0.4574(2) 0.17905(7) 0.0253(6) Uani 1 1 d . . . H2 H 0.8560 0.3856 0.1718 0.030 Uiso 1 1 calc R . . C3 C 0.9869(2) 0.4425(3) 0.19752(7) 0.0292(7) Uani 1 1 d . . . H3 H 1.0121 0.3605 0.2034 0.035 Uiso 1 1 calc R . . C4 C 1.04235(19) 0.5485(3) 0.20742(7) 0.0288(7) Uani 1 1 d . . . H4 H 1.1065 0.5405 0.2198 0.035 Uiso 1 1 calc R . . C5 C 1.00278(18) 0.6657(3) 0.19892(7) 0.0245(6) Uani 1 1 d . . . H5 H 1.0406 0.7386 0.2058 0.029 Uiso 1 1 calc R . . C6 C 0.75866(17) 0.6032(2) 0.15193(7) 0.0186(5) Uani 1 1 d . . . H6A H 0.7369 0.5341 0.1344 0.022 Uiso 1 1 calc R . . H6B H 0.7145 0.6076 0.1703 0.022 Uiso 1 1 calc R . . C7 C 0.66067(16) 0.7845(2) 0.12530(7) 0.0182(5) Uani 1 1 d . . . H7A H 0.6235 0.7537 0.1442 0.022 Uiso 1 1 calc R . . H7B H 0.6262 0.7596 0.1007 0.022 Uiso 1 1 calc R . . C8 C 0.66875(17) 0.9260(2) 0.12748(6) 0.0182(5) Uani 1 1 d . . . C9 C 0.75527(19) 1.0974(2) 0.15452(7) 0.0237(6) Uani 1 1 d . . . H9 H 0.8114 1.1302 0.1692 0.028 Uiso 1 1 calc R . . C10 C 0.68304(19) 1.1791(2) 0.14034(7) 0.0267(6) Uani 1 1 d . . . H10 H 0.6883 1.2667 0.1458 0.032 Uiso 1 1 calc R . . C11 C 0.6026(2) 1.1318(3) 0.11804(7) 0.0282(6) Uani 1 1 d . . . H11 H 0.5530 1.1870 0.1072 0.034 Uiso 1 1 calc R . . C12 C 0.59513(18) 1.0039(2) 0.11176(7) 0.0231(6) Uani 1 1 d . . . H12 H 0.5399 0.9697 0.0968 0.028 Uiso 1 1 calc R . . C13 C 0.80014(16) 0.7165(2) 0.09644(6) 0.0166(5) Uani 1 1 d . . . H13A H 0.8111 0.8031 0.0879 0.020 Uiso 1 1 calc R . . H13B H 0.8636 0.6751 0.1024 0.020 Uiso 1 1 calc R . . C14 C 0.74173(16) 0.6455(2) 0.06482(6) 0.0153(5) Uani 1 1 d . . . C15 C 0.74996(16) 0.5137(2) 0.06177(6) 0.0163(5) Uani 1 1 d . . . C16 C 0.82057(17) 0.4404(2) 0.08485(7) 0.0205(6) Uani 1 1 d . . . H16 H 0.8659 0.4821 0.1028 0.025 Uiso 1 1 calc R . . C17 C 0.82466(19) 0.3126(2) 0.08186(7) 0.0253(6) Uani 1 1 d . . . H17 H 0.8730 0.2670 0.0975 0.030 Uiso 1 1 calc R . . C18 C 0.75778(19) 0.2465(2) 0.05575(7) 0.0266(6) Uani 1 1 d . . . H18 H 0.7589 0.1569 0.0548 0.032 Uiso 1 1 calc R . . C19 C 0.69193(18) 0.3127(2) 0.03207(7) 0.0233(6) Uani 1 1 d . . . H19 H 0.6480 0.2683 0.0142 0.028 Uiso 1 1 calc R . . C20 C 0.68722(17) 0.4467(2) 0.03338(7) 0.0179(5) Uani 1 1 d . . . C21 C 0.62541(17) 0.5137(2) 0.00743(6) 0.0194(5) Uani 1 1 d . . . H21 H 0.5842 0.4690 -0.0112 0.023 Uiso 1 1 calc R . . C22 C 0.62169(17) 0.6458(2) 0.00774(7) 0.0191(5) Uani 1 1 d . . . C23 C 0.56083(17) 0.7126(2) -0.02044(7) 0.0228(6) Uani 1 1 d . . . H23 H 0.5218 0.6673 -0.0396 0.027 Uiso 1 1 calc R . . C24 C 0.55806(18) 0.8407(3) -0.02018(7) 0.0261(6) Uani 1 1 d . . . H24 H 0.5167 0.8843 -0.0391 0.031 Uiso 1 1 calc R . . C25 C 0.61622(17) 0.9099(2) 0.00796(7) 0.0227(6) Uani 1 1 d . . . H25 H 0.6147 0.9995 0.0075 0.027 Uiso 1 1 calc R . . C26 C 0.67456(17) 0.8486(2) 0.03570(7) 0.0199(6) Uani 1 1 d . . . H26 H 0.7125 0.8966 0.0545 0.024 Uiso 1 1 calc R . . C27 C 0.67986(16) 0.7141(2) 0.03710(6) 0.0174(5) Uani 1 1 d . . . C28 C 0.34973(17) 0.0623(2) 0.17001(7) 0.0186(5) Uani 1 1 d . . . C29 C 0.38607(18) -0.0578(2) 0.17650(7) 0.0234(6) Uani 1 1 d . . . H29 H 0.3481 -0.1292 0.1680 0.028 Uiso 1 1 calc R . . C30 C 0.47807(19) -0.0740(2) 0.19552(7) 0.0272(6) Uani 1 1 d . . . H30 H 0.5042 -0.1561 0.2001 0.033 Uiso 1 1 calc R . . C31 C 0.53135(19) 0.0320(3) 0.20771(7) 0.0269(6) Uani 1 1 d . . . H31 H 0.5951 0.0237 0.2205 0.032 Uiso 1 1 calc R . . C32 C 0.49070(18) 0.1495(2) 0.20099(7) 0.0241(6) Uani 1 1 d . . . H32 H 0.5272 0.2221 0.2095 0.029 Uiso 1 1 calc R . . C33 C 0.25083(16) 0.0893(2) 0.14916(7) 0.0179(5) Uani 1 1 d . . . H33A H 0.2318 0.0227 0.1305 0.021 Uiso 1 1 calc R . . H33B H 0.2037 0.0904 0.1664 0.021 Uiso 1 1 calc R . . C34 C 0.15618(16) 0.2740(2) 0.12314(7) 0.0171(5) Uani 1 1 d . . . H34A H 0.1164 0.2422 0.1410 0.021 Uiso 1 1 calc R . . H34B H 0.1242 0.2506 0.0980 0.021 Uiso 1 1 calc R . . C35 C 0.16395(17) 0.4151(2) 0.12610(6) 0.0166(5) Uani 1 1 d . . . C36 C 0.24995(18) 0.5834(2) 0.15562(7) 0.0220(6) Uani 1 1 d . . . H36 H 0.3045 0.6142 0.1718 0.026 Uiso 1 1 calc R . . C37 C 0.18152(18) 0.6682(2) 0.13917(7) 0.0246(6) Uani 1 1 d . . . H37 H 0.1884 0.7559 0.1443 0.029 Uiso 1 1 calc R . . C38 C 0.10326(18) 0.6238(2) 0.11516(7) 0.0241(6) Uani 1 1 d . . . H38 H 0.0561 0.6805 0.1032 0.029 Uiso 1 1 calc R . . C39 C 0.09454(17) 0.4953(2) 0.10875(6) 0.0204(6) Uani 1 1 d . . . H39 H 0.0409 0.4628 0.0925 0.025 Uiso 1 1 calc R . . C40 C 0.30126(16) 0.2112(2) 0.09703(6) 0.0160(5) Uani 1 1 d . . . H40A H 0.3645 0.1699 0.1038 0.019 Uiso 1 1 calc R . . H40B H 0.3128 0.2991 0.0897 0.019 Uiso 1 1 calc R . . C41 C 0.24572(16) 0.1428(2) 0.06401(6) 0.0150(5) Uani 1 1 d . . . C42 C 0.25376(16) 0.0105(2) 0.06035(6) 0.0163(5) Uani 1 1 d . . . C43 C 0.32362(17) -0.0643(2) 0.08338(7) 0.0211(6) Uani 1 1 d . . . H43 H 0.3689 -0.0235 0.1016 0.025 Uiso 1 1 calc R . . C44 C 0.32729(19) -0.1920(2) 0.08010(7) 0.0254(6) Uani 1 1 d . . . H44 H 0.3755 -0.2383 0.0956 0.030 Uiso 1 1 calc R . . C45 C 0.26019(19) -0.2567(2) 0.05389(7) 0.0267(6) Uani 1 1 d . . . H45 H 0.2610 -0.3463 0.0526 0.032 Uiso 1 1 calc R . . C46 C 0.19463(18) -0.1897(2) 0.03052(7) 0.0238(6) Uani 1 1 d . . . H46 H 0.1501 -0.2333 0.0127 0.029 Uiso 1 1 calc R . . C47 C 0.19091(17) -0.0556(2) 0.03205(7) 0.0176(5) Uani 1 1 d . . . C48 C 0.12735(16) 0.0134(2) 0.00653(6) 0.0191(5) Uani 1 1 d . . . H48 H 0.0849 -0.0303 -0.0120 0.023 Uiso 1 1 calc R . . C49 C 0.12458(16) 0.1439(2) 0.00753(6) 0.0184(5) Uani 1 1 d . . . C50 C 0.06215(17) 0.2135(2) -0.01986(7) 0.0220(6) Uani 1 1 d . . . H50 H 0.0214 0.1695 -0.0388 0.026 Uiso 1 1 calc R . . C51 C 0.06021(18) 0.3408(2) -0.01918(7) 0.0248(6) Uani 1 1 d . . . H51 H 0.0177 0.3855 -0.0374 0.030 Uiso 1 1 calc R . . C52 C 0.12112(18) 0.4080(2) 0.00850(7) 0.0232(6) Uani 1 1 d . . . H52 H 0.1205 0.4977 0.0082 0.028 Uiso 1 1 calc R . . C53 C 0.18070(17) 0.3462(2) 0.03553(7) 0.0194(6) Uani 1 1 d . . . H53 H 0.2204 0.3935 0.0540 0.023 Uiso 1 1 calc R . . C54 C 0.18461(16) 0.2113(2) 0.03661(6) 0.0155(5) Uani 1 1 d . . . N1 N 0.91250(14) 0.68047(19) 0.18127(5) 0.0194(5) Uani 1 1 d . . . N2 N 0.75760(13) 0.72630(18) 0.13155(5) 0.0158(4) Uani 1 1 d . . . N3 N 0.74881(14) 0.97203(18) 0.14815(5) 0.0179(5) Uani 1 1 d . . . N4 N 0.40056(14) 0.16461(18) 0.18267(5) 0.0181(5) Uani 1 1 d . . . N5 N 0.25257(13) 0.21465(18) 0.13068(5) 0.0149(4) Uani 1 1 d . . . N6 N 0.24129(14) 0.45852(18) 0.14934(5) 0.0174(4) Uani 1 1 d . . . O1 O 0.97595(12) 0.87432(16) 0.12950(5) 0.0284(4) Uani 1 1 d . . . O2 O 0.89131(13) 1.01466(16) 0.08732(5) 0.0320(5) Uani 1 1 d . . . O3 O 0.98890(13) 1.09274(16) 0.14056(5) 0.0321(5) Uani 1 1 d . . . O4 O 1.05872(14) 1.00143(19) 0.09291(5) 0.0450(6) Uani 1 1 d . . . O5 O 0.74066(13) 0.84393(17) 0.21637(5) 0.0334(5) Uani 1 1 d . . . O6 O 0.77492(14) 0.64728(17) 0.24534(5) 0.0408(5) Uani 1 1 d . . . O7 O 0.63716(12) 0.75850(17) 0.25406(5) 0.0330(5) Uani 1 1 d . . . O8 O 0.78790(14) 0.83363(19) 0.28096(5) 0.0406(5) Uani 1 1 d . . . O9 O 0.93454(14) 0.94855(18) 0.19916(5) 0.0305(5) Uani 1 1 d D . . O11 O 0.46636(12) 0.38273(16) 0.14307(5) 0.0279(4) Uani 1 1 d . . . O12 O 0.39677(13) 0.50502(16) 0.09229(5) 0.0325(5) Uani 1 1 d . . . O13 O 0.56403(13) 0.47916(19) 0.10522(5) 0.0413(5) Uani 1 1 d . . . O14 O 0.48529(14) 0.60343(17) 0.14426(5) 0.0374(5) Uani 1 1 d . . . O15 O 0.19821(14) 0.28090(19) 0.21146(5) 0.0404(5) Uani 1 1 d . . . O16 O 0.22815(19) 0.0832(2) 0.24025(6) 0.0779(9) Uani 1 1 d . . . O17 O 0.10527(19) 0.2123(2) 0.25450(8) 0.0850(10) Uani 1 1 d . . . O18 O 0.2628(2) 0.2727(3) 0.27449(7) 0.0970(10) Uani 1 1 d . . . O19 O 0.39148(14) 0.41974(19) 0.21366(5) 0.0345(5) Uani 1 1 d D . . O20 O 0.57143(14) 0.51256(18) 0.23176(5) 0.0342(5) Uani 1 1 d D . . Cl1 Cl 0.97917(4) 0.99679(6) 0.112122(17) 0.02178(14) Uani 1 1 d . . . Cl2 Cl 0.73545(4) 0.77042(6) 0.249214(18) 0.02450(15) Uani 1 1 d . . . Cl3 Cl 0.47856(4) 0.49414(6) 0.120916(17) 0.02295(14) Uani 1 1 d . . . Cl4 Cl 0.19610(6) 0.21065(8) 0.24484(2) 0.0495(2) Uani 1 1 d . . . Cu1 Cu 0.84428(2) 0.84010(3) 0.166655(8) 0.01847(8) Uani 1 1 d . . . Cu2 Cu 0.33187(2) 0.32488(3) 0.169666(8) 0.01923(8) Uani 1 1 d . . . H1O H 0.9208(18) 0.962(2) 0.2217(3) 0.029 Uiso 1 1 d D . . H2O H 0.9890(9) 0.988(2) 0.1972(7) 0.029 Uiso 1 1 d D . . H3O H 0.4435(11) 0.461(2) 0.2094(7) 0.029 Uiso 1 1 d D . . H4O H 0.3684(17) 0.434(2) 0.2344(4) 0.029 Uiso 1 1 d D . . H5O H 0.6238(10) 0.477(2) 0.2256(7) 0.029 Uiso 1 1 d D . . H6O H 0.5874(18) 0.5922(8) 0.2375(7) 0.029 Uiso 1 1 d 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 C1 0.0182(13) 0.0227(14) 0.0165(13) 0.0034(11) 0.0028(11) -0.0010(11) C2 0.0302(15) 0.0215(15) 0.0240(15) 0.0072(12) 0.0039(13) 0.0005(12) C3 0.0328(16) 0.0282(16) 0.0267(16) 0.0103(12) 0.0052(13) 0.0077(13) C4 0.0199(14) 0.0429(19) 0.0227(15) 0.0082(13) 0.0010(12) 0.0075(13) C5 0.0190(13) 0.0337(17) 0.0189(14) 0.0009(12) -0.0028(11) -0.0035(12) C6 0.0212(13) 0.0143(13) 0.0209(14) 0.0024(11) 0.0051(11) -0.0029(10) C7 0.0155(12) 0.0193(13) 0.0191(13) -0.0013(11) 0.0014(11) -0.0017(10) C8 0.0221(13) 0.0194(14) 0.0146(13) -0.0007(10) 0.0073(11) 0.0025(11) C9 0.0293(15) 0.0226(15) 0.0194(14) -0.0015(11) 0.0046(12) -0.0039(12) C10 0.0383(16) 0.0172(14) 0.0266(15) 0.0003(12) 0.0112(13) 0.0012(12) C11 0.0304(16) 0.0290(16) 0.0258(16) 0.0042(12) 0.0061(13) 0.0105(13) C12 0.0207(14) 0.0263(15) 0.0218(14) -0.0022(12) 0.0019(11) 0.0014(12) C13 0.0141(12) 0.0182(13) 0.0171(13) 0.0022(10) 0.0013(10) -0.0025(10) C14 0.0135(12) 0.0193(13) 0.0138(12) -0.0008(10) 0.0046(10) -0.0019(10) C15 0.0163(12) 0.0175(13) 0.0159(12) -0.0009(10) 0.0051(10) -0.0029(10) C16 0.0212(13) 0.0212(14) 0.0186(14) -0.0015(11) 0.0017(11) 0.0001(11) C17 0.0292(15) 0.0226(15) 0.0244(15) 0.0018(12) 0.0054(12) 0.0061(12) C18 0.0342(16) 0.0181(15) 0.0290(16) -0.0012(12) 0.0102(13) 0.0027(12) C19 0.0245(14) 0.0208(15) 0.0259(15) -0.0056(12) 0.0083(12) -0.0074(11) C20 0.0172(13) 0.0194(14) 0.0185(13) -0.0034(11) 0.0074(11) -0.0019(10) C21 0.0167(13) 0.0229(14) 0.0182(13) -0.0049(11) 0.0017(11) -0.0048(11) C22 0.0160(12) 0.0237(14) 0.0180(13) -0.0016(11) 0.0041(11) -0.0017(11) C23 0.0182(13) 0.0316(16) 0.0177(14) 0.0011(12) 0.0000(11) 0.0000(11) C24 0.0219(14) 0.0341(17) 0.0218(15) 0.0072(12) 0.0024(12) 0.0061(12) C25 0.0233(14) 0.0220(15) 0.0231(15) 0.0039(12) 0.0044(12) 0.0057(11) C26 0.0205(13) 0.0216(15) 0.0182(14) -0.0012(11) 0.0045(11) -0.0002(11) C27 0.0149(12) 0.0199(14) 0.0180(13) -0.0003(11) 0.0044(11) -0.0012(10) C28 0.0196(13) 0.0173(13) 0.0178(13) 0.0043(10) -0.0004(11) -0.0024(10) C29 0.0284(15) 0.0175(14) 0.0228(15) 0.0037(11) -0.0003(12) -0.0028(11) C30 0.0320(16) 0.0217(15) 0.0268(16) 0.0083(12) 0.0014(13) 0.0050(12) C31 0.0217(14) 0.0342(17) 0.0218(15) 0.0063(12) -0.0055(12) 0.0010(12) C32 0.0208(13) 0.0245(15) 0.0247(15) 0.0009(12) -0.0035(12) -0.0030(11) C33 0.0186(13) 0.0164(13) 0.0176(13) 0.0001(10) 0.0003(11) -0.0018(10) C34 0.0127(12) 0.0195(13) 0.0179(13) -0.0003(11) -0.0011(10) -0.0009(10) C35 0.0157(12) 0.0211(14) 0.0136(13) -0.0008(10) 0.0039(11) -0.0006(10) C36 0.0229(14) 0.0212(14) 0.0219(14) -0.0036(11) 0.0035(12) -0.0020(11) C37 0.0315(15) 0.0148(14) 0.0281(15) -0.0016(12) 0.0068(13) 0.0010(12) C38 0.0260(15) 0.0261(15) 0.0206(14) 0.0030(12) 0.0055(12) 0.0087(12) C39 0.0183(13) 0.0246(15) 0.0176(13) -0.0030(11) 0.0003(11) 0.0016(11) C40 0.0142(12) 0.0160(13) 0.0169(13) 0.0008(10) -0.0004(10) -0.0029(10) C41 0.0121(11) 0.0171(13) 0.0166(13) -0.0004(10) 0.0042(10) -0.0034(10) C42 0.0154(12) 0.0184(13) 0.0156(12) 0.0000(10) 0.0043(10) -0.0003(10) C43 0.0227(14) 0.0207(14) 0.0201(14) -0.0002(11) 0.0044(12) 0.0028(11) C44 0.0290(15) 0.0216(15) 0.0257(15) 0.0046(12) 0.0050(13) 0.0073(12) C45 0.0395(16) 0.0134(14) 0.0287(16) -0.0007(11) 0.0102(13) 0.0021(12) C46 0.0288(15) 0.0217(15) 0.0227(14) -0.0064(12) 0.0094(12) -0.0041(12) C47 0.0184(13) 0.0165(14) 0.0196(14) -0.0016(10) 0.0086(11) -0.0018(10) C48 0.0168(13) 0.0223(14) 0.0179(13) -0.0048(11) 0.0015(11) -0.0058(11) C49 0.0157(12) 0.0244(14) 0.0155(13) -0.0007(11) 0.0040(11) 0.0016(10) C50 0.0187(13) 0.0289(15) 0.0179(14) -0.0005(11) 0.0015(11) -0.0013(11) C51 0.0228(14) 0.0302(16) 0.0206(14) 0.0065(12) 0.0011(12) 0.0059(12) C52 0.0260(15) 0.0208(14) 0.0240(15) 0.0009(12) 0.0074(12) 0.0039(11) C53 0.0212(13) 0.0203(14) 0.0165(13) 0.0014(11) 0.0030(11) 0.0002(11) C54 0.0139(12) 0.0180(13) 0.0146(13) -0.0011(10) 0.0026(10) -0.0012(10) N1 0.0184(11) 0.0239(12) 0.0155(11) 0.0019(9) 0.0021(9) -0.0011(9) N2 0.0149(10) 0.0151(11) 0.0171(11) 0.0002(9) 0.0015(9) -0.0009(8) N3 0.0222(11) 0.0175(11) 0.0140(11) 0.0002(9) 0.0032(9) -0.0030(9) N4 0.0182(11) 0.0187(11) 0.0158(11) 0.0014(9) -0.0025(9) -0.0014(9) N5 0.0142(10) 0.0145(10) 0.0150(10) 0.0000(8) -0.0007(9) -0.0011(8) N6 0.0175(11) 0.0153(11) 0.0192(11) -0.0003(9) 0.0019(9) -0.0016(8) O1 0.0326(11) 0.0190(10) 0.0316(11) 0.0002(8) -0.0008(9) -0.0012(8) O2 0.0312(11) 0.0282(11) 0.0329(11) 0.0033(9) -0.0060(9) 0.0006(9) O3 0.0469(12) 0.0238(11) 0.0273(11) -0.0093(8) 0.0112(10) -0.0150(9) O4 0.0367(12) 0.0622(15) 0.0418(13) -0.0203(11) 0.0239(10) -0.0244(11) O5 0.0432(12) 0.0376(12) 0.0208(10) 0.0111(9) 0.0097(9) 0.0072(9) O6 0.0454(13) 0.0310(12) 0.0476(13) 0.0094(10) 0.0126(11) 0.0171(10) O7 0.0262(10) 0.0360(12) 0.0381(12) 0.0021(9) 0.0092(9) 0.0001(9) O8 0.0391(12) 0.0538(14) 0.0257(11) -0.0018(10) -0.0040(9) -0.0117(10) O9 0.0333(12) 0.0336(12) 0.0236(11) -0.0084(9) 0.0017(10) -0.0133(9) O11 0.0242(10) 0.0203(10) 0.0379(12) 0.0102(8) 0.0012(9) -0.0022(8) O12 0.0341(11) 0.0262(11) 0.0332(11) 0.0045(9) -0.0062(9) -0.0010(9) O13 0.0275(11) 0.0505(14) 0.0493(13) 0.0007(11) 0.0163(10) -0.0070(10) O14 0.0512(13) 0.0227(11) 0.0382(12) -0.0076(9) 0.0067(10) -0.0114(9) O15 0.0439(12) 0.0555(14) 0.0230(11) 0.0123(10) 0.0091(10) 0.0114(11) O16 0.114(2) 0.0736(18) 0.0495(16) 0.0184(13) 0.0237(16) 0.0719(17) O17 0.093(2) 0.0657(18) 0.116(2) 0.0479(17) 0.0748(19) 0.0411(16) O18 0.121(3) 0.122(3) 0.0391(16) 0.0013(16) -0.0157(17) 0.038(2) O19 0.0297(12) 0.0371(13) 0.0332(12) -0.0137(10) -0.0051(10) -0.0022(9) O20 0.0374(12) 0.0287(12) 0.0349(12) 0.0012(10) 0.0008(10) -0.0031(10) Cl1 0.0233(3) 0.0196(3) 0.0231(3) -0.0032(3) 0.0059(3) -0.0063(3) Cl2 0.0241(3) 0.0280(4) 0.0213(3) 0.0053(3) 0.0032(3) 0.0051(3) Cl3 0.0203(3) 0.0199(3) 0.0282(4) 0.0011(3) 0.0028(3) -0.0050(3) Cl4 0.0623(6) 0.0586(6) 0.0324(5) 0.0206(4) 0.0216(4) 0.0380(5) Cu1 0.02019(16) 0.01780(17) 0.01581(16) -0.00125(13) -0.00195(13) -0.00218(13) Cu2 0.01883(16) 0.01703(17) 0.01900(17) -0.00167(13) -0.00537(13) -0.00010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.346(3) . ? C1 C2 1.381(3) . ? C1 C6 1.502(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 N1 1.343(3) . ? C5 H5 0.9500 . ? C6 N2 1.502(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.485(3) . ? C7 C8 1.504(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.347(3) . ? C8 C12 1.379(3) . ? C9 N3 1.349(3) . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.375(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.511(3) . ? C13 N2 1.511(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.407(3) . ? C14 C27 1.428(3) . ? C15 C16 1.429(3) . ? C15 C20 1.441(3) . ? C16 C17 1.360(3) . ? C16 H16 0.9500 . ? C17 C18 1.417(3) . ? C17 H17 0.9500 . ? C18 C19 1.360(3) . ? C18 H18 0.9500 . ? C19 C20 1.422(3) . ? C19 H19 0.9500 . ? C20 C21 1.380(3) . ? C21 C22 1.400(3) . ? C21 H21 0.9500 . ? C22 C23 1.422(3) . ? C22 C27 1.440(3) . ? C23 C24 1.357(3) . ? C23 H23 0.9500 . ? C24 C25 1.416(3) . ? C24 H24 0.9500 . ? C25 C26 1.365(3) . ? C25 H25 0.9500 . ? C26 C27 1.427(3) . ? C26 H26 0.9500 . ? C28 N4 1.340(3) . ? C28 C29 1.379(3) . ? C28 C33 1.507(3) . ? C29 C30 1.382(3) . ? C29 H29 0.9500 . ? C30 C31 1.385(4) . ? C30 H30 0.9500 . ? C31 C32 1.376(3) . ? C31 H31 0.9500 . ? C32 N4 1.350(3) . ? C32 H32 0.9500 . ? C33 N5 1.493(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N5 1.484(3) . ? C34 C35 1.501(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N6 1.353(3) . ? C35 C39 1.373(3) . ? C36 N6 1.345(3) . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.380(3) . ? C37 H37 0.9500 . ? C38 C39 1.383(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 N5 1.509(3) . ? C40 C41 1.517(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.415(3) . ? C41 C54 1.415(3) . ? C42 C43 1.430(3) . ? C42 C47 1.434(3) . ? C43 C44 1.360(3) . ? C43 H43 0.9500 . ? C44 C45 1.413(3) . ? C44 H44 0.9500 . ? C45 C46 1.356(3) . ? C45 H45 0.9500 . ? C46 C47 1.423(3) . ? C46 H46 0.9500 . ? C47 C48 1.394(3) . ? C48 C49 1.384(3) . ? C48 H48 0.9500 . ? C49 C50 1.430(3) . ? C49 C54 1.440(3) . ? C50 C51 1.350(3) . ? C50 H50 0.9500 . ? C51 C52 1.412(3) . ? C51 H51 0.9500 . ? C52 C53 1.360(3) . ? C52 H52 0.9500 . ? C53 C54 1.430(3) . ? C53 H53 0.9500 . ? N1 Cu1 1.977(2) . ? N2 Cu1 2.0250(19) . ? N3 Cu1 1.984(2) . ? N4 Cu2 1.9751(19) . ? N5 Cu2 2.0361(18) . ? N6 Cu2 1.9718(19) . ? O1 Cl1 1.4496(17) . ? O1 Cu1 2.5050(18) . ? O2 Cl1 1.4277(18) . ? O3 Cl1 1.4474(17) . ? O4 Cl1 1.4211(18) . ? O5 Cl2 1.4470(17) . ? O5 Cu1 2.5185(17) . ? O6 Cl2 1.4347(18) . ? O7 Cl2 1.4337(18) . ? O8 Cl2 1.4405(19) . ? O9 Cu1 1.9686(18) . ? O9 H1O 0.890(14) . ? O9 H2O 0.890(16) . ? O11 Cl3 1.4591(17) . ? O11 Cu2 2.3538(17) . ? O12 Cl3 1.4345(18) . ? O13 Cl3 1.4286(18) . ? O14 Cl3 1.4343(18) . ? O15 Cl4 1.4381(19) . ? O15 Cu2 2.6600(19) . ? O16 Cl4 1.442(2) . ? O17 Cl4 1.386(2) . ? O18 Cl4 1.474(3) . ? O19 Cu2 1.9712(19) . ? O19 H3O 0.890(18) . ? O19 H4O 0.890(18) . ? O20 H5O 0.891(17) . ? O20 H6O 0.890(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.2(2) . . ? N1 C1 C6 115.3(2) . . ? C2 C1 C6 123.5(2) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.7(2) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.3(2) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N2 C6 C1 108.92(18) . . ? N2 C6 H6A 109.9 . . ? C1 C6 H6A 109.9 . . ? N2 C6 H6B 109.9 . . ? C1 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C8 110.20(19) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C12 121.8(2) . . ? N3 C8 C7 116.1(2) . . ? C12 C8 C7 121.9(2) . . ? N3 C9 C10 121.9(2) . . ? N3 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C11 119.0(2) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.3(2) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C8 C12 C11 119.2(2) . . ? C8 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 N2 116.49(18) . . ? C14 C13 H13A 108.2 . . ? N2 C13 H13A 108.2 . . ? C14 C13 H13B 108.2 . . ? N2 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C27 119.8(2) . . ? C15 C14 C13 120.9(2) . . ? C27 C14 C13 119.3(2) . . ? C14 C15 C16 123.4(2) . . ? C14 C15 C20 119.8(2) . . ? C16 C15 C20 116.7(2) . . ? C17 C16 C15 121.9(2) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.9(2) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 119.3(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.6(2) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 121.2(2) . . ? C21 C20 C15 119.5(2) . . ? C19 C20 C15 119.3(2) . . ? C20 C21 C22 121.9(2) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C23 120.7(2) . . ? C21 C22 C27 119.4(2) . . ? C23 C22 C27 119.9(2) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.6(2) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.5(2) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C14 C27 C26 123.8(2) . . ? C14 C27 C22 119.1(2) . . ? C26 C27 C22 117.0(2) . . ? N4 C28 C29 121.5(2) . . ? N4 C28 C33 115.0(2) . . ? C29 C28 C33 123.4(2) . . ? C30 C29 C28 119.6(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 118.7(2) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 119.1(2) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? N4 C32 C31 122.0(2) . . ? N4 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? N5 C33 C28 108.48(18) . . ? N5 C33 H33A 110.0 . . ? C28 C33 H33A 110.0 . . ? N5 C33 H33B 110.0 . . ? C28 C33 H33B 110.0 . . ? H33A C33 H33B 108.4 . . ? N5 C34 C35 110.74(18) . . ? N5 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? N5 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? N6 C35 C39 121.6(2) . . ? N6 C35 C34 115.2(2) . . ? C39 C35 C34 123.0(2) . . ? N6 C36 C37 121.7(2) . . ? N6 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C38 119.2(2) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 119.0(2) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C35 C39 C38 119.5(2) . . ? C35 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N5 C40 C41 114.86(18) . . ? N5 C40 H40A 108.6 . . ? C41 C40 H40A 108.6 . . ? N5 C40 H40B 108.6 . . ? C41 C40 H40B 108.6 . . ? H40A C40 H40B 107.5 . . ? C42 C41 C54 119.3(2) . . ? C42 C41 C40 120.7(2) . . ? C54 C41 C40 120.0(2) . . ? C41 C42 C43 123.4(2) . . ? C41 C42 C47 120.2(2) . . ? C43 C42 C47 116.4(2) . . ? C44 C43 C42 122.1(2) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C45 120.8(2) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 119.4(2) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C47 121.6(2) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C48 C47 C46 121.4(2) . . ? C48 C47 C42 119.1(2) . . ? C46 C47 C42 119.5(2) . . ? C49 C48 C47 121.6(2) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C48 C49 C50 120.9(2) . . ? C48 C49 C54 119.9(2) . . ? C50 C49 C54 119.2(2) . . ? C51 C50 C49 120.9(2) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 120.3(2) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 121.0(2) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 121.2(2) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C41 C54 C53 123.3(2) . . ? C41 C54 C49 119.4(2) . . ? C53 C54 C49 117.3(2) . . ? C5 N1 C1 119.1(2) . . ? C5 N1 Cu1 127.87(18) . . ? C1 N1 Cu1 113.07(16) . . ? C7 N2 C6 111.83(17) . . ? C7 N2 C13 112.38(18) . . ? C6 N2 C13 113.09(18) . . ? C7 N2 Cu1 107.36(14) . . ? C6 N2 Cu1 104.10(13) . . ? C13 N2 Cu1 107.47(13) . . ? C9 N3 C8 118.8(2) . . ? C9 N3 Cu1 127.67(17) . . ? C8 N3 Cu1 113.57(16) . . ? C28 N4 C32 119.1(2) . . ? C28 N4 Cu2 113.36(16) . . ? C32 N4 Cu2 127.54(17) . . ? C34 N5 C33 112.28(17) . . ? C34 N5 C40 112.56(17) . . ? C33 N5 C40 113.21(18) . . ? C34 N5 Cu2 105.75(14) . . ? C33 N5 Cu2 103.79(13) . . ? C40 N5 Cu2 108.50(13) . . ? C36 N6 C35 119.0(2) . . ? C36 N6 Cu2 127.29(17) . . ? C35 N6 Cu2 113.73(15) . . ? Cl1 O1 Cu1 116.63(10) . . ? Cl2 O5 Cu1 135.18(11) . . ? Cu1 O9 H1O 116.1(17) . . ? Cu1 O9 H2O 135.1(17) . . ? H1O O9 H2O 109(2) . . ? Cl3 O11 Cu2 128.17(10) . . ? Cl4 O15 Cu2 134.18(11) . . ? Cu2 O19 H3O 111.1(17) . . ? Cu2 O19 H4O 128.6(17) . . ? H3O O19 H4O 120(2) . . ? H5O O20 H6O 106(2) . . ? O4 Cl1 O2 110.76(12) . . ? O4 Cl1 O3 110.09(11) . . ? O2 Cl1 O3 109.74(11) . . ? O4 Cl1 O1 109.46(12) . . ? O2 Cl1 O1 108.25(10) . . ? O3 Cl1 O1 108.49(11) . . ? O7 Cl2 O6 109.39(12) . . ? O7 Cl2 O8 108.78(12) . . ? O6 Cl2 O8 110.22(12) . . ? O7 Cl2 O5 109.40(11) . . ? O6 Cl2 O5 109.48(11) . . ? O8 Cl2 O5 109.56(11) . . ? O13 Cl3 O12 110.27(12) . . ? O13 Cl3 O14 110.62(12) . . ? O12 Cl3 O14 109.89(11) . . ? O13 Cl3 O11 108.60(11) . . ? O12 Cl3 O11 108.62(10) . . ? O14 Cl3 O11 108.80(11) . . ? O17 Cl4 O15 111.08(14) . . ? O17 Cl4 O16 111.30(17) . . ? O15 Cl4 O16 109.53(13) . . ? O17 Cl4 O18 108.22(18) . . ? O15 Cl4 O18 107.43(16) . . ? O16 Cl4 O18 109.18(16) . . ? O9 Cu1 N1 95.47(8) . . ? O9 Cu1 N3 97.69(8) . . ? N1 Cu1 N3 165.89(8) . . ? O9 Cu1 N2 176.70(8) . . ? N1 Cu1 N2 83.18(8) . . ? N3 Cu1 N2 83.93(8) . . ? O9 Cu1 O1 77.32(7) . . ? N1 Cu1 O1 84.21(7) . . ? N3 Cu1 O1 103.60(7) . . ? N2 Cu1 O1 99.52(7) . . ? O9 Cu1 O5 86.94(7) . . ? N1 Cu1 O5 97.60(7) . . ? N3 Cu1 O5 78.11(7) . . ? N2 Cu1 O5 96.21(7) . . ? O1 Cu1 O5 164.27(6) . . ? O19 Cu2 N6 96.24(8) . . ? O19 Cu2 N4 96.45(8) . . ? N6 Cu2 N4 166.34(8) . . ? O19 Cu2 N5 168.90(8) . . ? N6 Cu2 N5 84.06(8) . . ? N4 Cu2 N5 82.51(8) . . ? O19 Cu2 O11 86.62(7) . . ? N6 Cu2 O11 100.02(7) . . ? N4 Cu2 O11 85.77(7) . . ? N5 Cu2 O11 104.28(7) . . ? O19 Cu2 O15 82.27(7) . . ? N6 Cu2 O15 82.31(7) . . ? N4 Cu2 O15 94.41(7) . . ? N5 Cu2 O15 86.79(7) . . ? O11 Cu2 O15 168.84(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.2(4) . . . . ? C6 C1 C2 C3 -178.5(2) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C3 C4 C5 N1 -0.3(4) . . . . ? N1 C1 C6 N2 29.4(3) . . . . ? C2 C1 C6 N2 -152.2(2) . . . . ? N2 C7 C8 N3 -26.0(3) . . . . ? N2 C7 C8 C12 159.2(2) . . . . ? N3 C9 C10 C11 -1.9(4) . . . . ? C9 C10 C11 C12 2.5(4) . . . . ? N3 C8 C12 C11 -1.5(4) . . . . ? C7 C8 C12 C11 173.1(2) . . . . ? C10 C11 C12 C8 -0.9(4) . . . . ? N2 C13 C14 C15 -86.7(3) . . . . ? N2 C13 C14 C27 95.3(3) . . . . ? C27 C14 C15 C16 169.9(2) . . . . ? C13 C14 C15 C16 -8.0(3) . . . . ? C27 C14 C15 C20 -7.8(3) . . . . ? C13 C14 C15 C20 174.3(2) . . . . ? C14 C15 C16 C17 178.0(2) . . . . ? C20 C15 C16 C17 -4.2(3) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C16 C17 C18 C19 3.5(4) . . . . ? C17 C18 C19 C20 -1.3(4) . . . . ? C18 C19 C20 C21 174.8(2) . . . . ? C18 C19 C20 C15 -3.6(4) . . . . ? C14 C15 C20 C21 5.7(3) . . . . ? C16 C15 C20 C21 -172.2(2) . . . . ? C14 C15 C20 C19 -175.9(2) . . . . ? C16 C15 C20 C19 6.2(3) . . . . ? C19 C20 C21 C22 -178.3(2) . . . . ? C15 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 C23 176.8(2) . . . . ? C20 C21 C22 C27 -3.6(4) . . . . ? C21 C22 C23 C24 -179.5(2) . . . . ? C27 C22 C23 C24 0.9(4) . . . . ? C22 C23 C24 C25 0.5(4) . . . . ? C23 C24 C25 C26 -1.3(4) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C15 C14 C27 C26 -173.0(2) . . . . ? C13 C14 C27 C26 4.9(3) . . . . ? C15 C14 C27 C22 4.3(3) . . . . ? C13 C14 C27 C22 -177.8(2) . . . . ? C25 C26 C27 C14 178.0(2) . . . . ? C25 C26 C27 C22 0.6(3) . . . . ? C21 C22 C27 C14 1.4(3) . . . . ? C23 C22 C27 C14 -179.0(2) . . . . ? C21 C22 C27 C26 178.9(2) . . . . ? C23 C22 C27 C26 -1.4(3) . . . . ? N4 C28 C29 C30 -2.0(4) . . . . ? C33 C28 C29 C30 179.2(2) . . . . ? C28 C29 C30 C31 0.2(4) . . . . ? C29 C30 C31 C32 0.9(4) . . . . ? C30 C31 C32 N4 -0.4(4) . . . . ? N4 C28 C33 N5 30.2(3) . . . . ? C29 C28 C33 N5 -150.9(2) . . . . ? N5 C34 C35 N6 -28.0(3) . . . . ? N5 C34 C35 C39 156.6(2) . . . . ? N6 C36 C37 C38 -1.2(4) . . . . ? C36 C37 C38 C39 1.2(4) . . . . ? N6 C35 C39 C38 -0.2(4) . . . . ? C34 C35 C39 C38 174.9(2) . . . . ? C37 C38 C39 C35 -0.5(4) . . . . ? N5 C40 C41 C42 -85.7(3) . . . . ? N5 C40 C41 C54 93.9(2) . . . . ? C54 C41 C42 C43 170.4(2) . . . . ? C40 C41 C42 C43 -10.0(3) . . . . ? C54 C41 C42 C47 -8.6(3) . . . . ? C40 C41 C42 C47 171.0(2) . . . . ? C41 C42 C43 C44 177.5(2) . . . . ? C47 C42 C43 C44 -3.5(3) . . . . ? C42 C43 C44 C45 -1.2(4) . . . . ? C43 C44 C45 C46 3.4(4) . . . . ? C44 C45 C46 C47 -0.8(4) . . . . ? C45 C46 C47 C48 176.0(2) . . . . ? C45 C46 C47 C42 -4.0(4) . . . . ? C41 C42 C47 C48 5.0(3) . . . . ? C43 C42 C47 C48 -174.0(2) . . . . ? C41 C42 C47 C46 -175.0(2) . . . . ? C43 C42 C47 C46 5.9(3) . . . . ? C46 C47 C48 C49 -178.9(2) . . . . ? C42 C47 C48 C49 1.0(3) . . . . ? C47 C48 C49 C50 177.1(2) . . . . ? C47 C48 C49 C54 -3.4(4) . . . . ? C48 C49 C50 C51 -179.2(2) . . . . ? C54 C49 C50 C51 1.3(4) . . . . ? C49 C50 C51 C52 0.9(4) . . . . ? C50 C51 C52 C53 -1.9(4) . . . . ? C51 C52 C53 C54 0.8(4) . . . . ? C42 C41 C54 C53 -172.1(2) . . . . ? C40 C41 C54 C53 8.3(3) . . . . ? C42 C41 C54 C49 6.2(3) . . . . ? C40 C41 C54 C49 -173.4(2) . . . . ? C52 C53 C54 C41 179.6(2) . . . . ? C52 C53 C54 C49 1.3(3) . . . . ? C48 C49 C54 C41 -0.2(3) . . . . ? C50 C49 C54 C41 179.3(2) . . . . ? C48 C49 C54 C53 178.2(2) . . . . ? C50 C49 C54 C53 -2.3(3) . . . . ? C4 C5 N1 C1 -0.7(4) . . . . ? C4 C5 N1 Cu1 -179.68(18) . . . . ? C2 C1 N1 C5 0.9(4) . . . . ? C6 C1 N1 C5 179.4(2) . . . . ? C2 C1 N1 Cu1 -179.97(19) . . . . ? C6 C1 N1 Cu1 -1.5(3) . . . . ? C8 C7 N2 C6 145.20(19) . . . . ? C8 C7 N2 C13 -86.4(2) . . . . ? C8 C7 N2 Cu1 31.6(2) . . . . ? C1 C6 N2 C7 -156.21(19) . . . . ? C1 C6 N2 C13 75.7(2) . . . . ? C1 C6 N2 Cu1 -40.6(2) . . . . ? C14 C13 N2 C7 -56.5(3) . . . . ? C14 C13 N2 C6 71.3(2) . . . . ? C14 C13 N2 Cu1 -174.40(16) . . . . ? C10 C9 N3 C8 -0.4(4) . . . . ? C10 C9 N3 Cu1 -179.17(18) . . . . ? C12 C8 N3 C9 2.2(3) . . . . ? C7 C8 N3 C9 -172.7(2) . . . . ? C12 C8 N3 Cu1 -178.93(18) . . . . ? C7 C8 N3 Cu1 6.2(3) . . . . ? C29 C28 N4 C32 2.5(4) . . . . ? C33 C28 N4 C32 -178.6(2) . . . . ? C29 C28 N4 Cu2 -179.84(19) . . . . ? C33 C28 N4 Cu2 -1.0(3) . . . . ? C31 C32 N4 C28 -1.3(4) . . . . ? C31 C32 N4 Cu2 -178.58(19) . . . . ? C35 C34 N5 C33 146.85(19) . . . . ? C35 C34 N5 C40 -84.0(2) . . . . ? C35 C34 N5 Cu2 34.3(2) . . . . ? C28 C33 N5 C34 -155.92(19) . . . . ? C28 C33 N5 C40 75.3(2) . . . . ? C28 C33 N5 Cu2 -42.2(2) . . . . ? C41 C40 N5 C34 -57.7(3) . . . . ? C41 C40 N5 C33 71.0(2) . . . . ? C41 C40 N5 Cu2 -174.39(16) . . . . ? C37 C36 N6 C35 0.5(4) . . . . ? C37 C36 N6 Cu2 179.09(18) . . . . ? C39 C35 N6 C36 0.2(3) . . . . ? C34 C35 N6 C36 -175.2(2) . . . . ? C39 C35 N6 Cu2 -178.53(18) . . . . ? C34 C35 N6 Cu2 6.0(3) . . . . ? Cu1 O1 Cl1 O4 178.78(10) . . . . ? Cu1 O1 Cl1 O2 -60.40(13) . . . . ? Cu1 O1 Cl1 O3 58.63(13) . . . . ? Cu1 O5 Cl2 O7 -144.52(14) . . . . ? Cu1 O5 Cl2 O6 -24.66(19) . . . . ? Cu1 O5 Cl2 O8 96.32(17) . . . . ? Cu2 O11 Cl3 O13 -169.75(12) . . . . ? Cu2 O11 Cl3 O12 -49.81(16) . . . . ? Cu2 O11 Cl3 O14 69.78(15) . . . . ? Cu2 O15 Cl4 O17 -176.84(18) . . . . ? Cu2 O15 Cl4 O16 -53.5(2) . . . . ? Cu2 O15 Cl4 O18 65.0(2) . . . . ? C5 N1 Cu1 O9 -16.4(2) . . . . ? C1 N1 Cu1 O9 164.63(17) . . . . ? C5 N1 Cu1 N3 -175.2(3) . . . . ? C1 N1 Cu1 N3 5.8(4) . . . . ? C5 N1 Cu1 N2 160.6(2) . . . . ? C1 N1 Cu1 N2 -18.40(16) . . . . ? C5 N1 Cu1 O1 60.3(2) . . . . ? C1 N1 Cu1 O1 -118.74(17) . . . . ? C5 N1 Cu1 O5 -104.0(2) . . . . ? C1 N1 Cu1 O5 77.00(17) . . . . ? C9 N3 Cu1 O9 5.9(2) . . . . ? C8 N3 Cu1 O9 -172.85(16) . . . . ? C9 N3 Cu1 N1 164.7(3) . . . . ? C8 N3 Cu1 N1 -14.1(4) . . . . ? C9 N3 Cu1 N2 -171.2(2) . . . . ? C8 N3 Cu1 N2 10.05(16) . . . . ? C9 N3 Cu1 O1 -72.8(2) . . . . ? C8 N3 Cu1 O1 108.40(16) . . . . ? C9 N3 Cu1 O5 91.1(2) . . . . ? C8 N3 Cu1 O5 -87.63(16) . . . . ? C7 N2 Cu1 N1 151.03(15) . . . . ? C6 N2 Cu1 N1 32.33(14) . . . . ? C13 N2 Cu1 N1 -87.87(14) . . . . ? C7 N2 Cu1 N3 -23.21(14) . . . . ? C6 N2 Cu1 N3 -141.91(14) . . . . ? C13 N2 Cu1 N3 97.89(14) . . . . ? C7 N2 Cu1 O1 -126.04(14) . . . . ? C6 N2 Cu1 O1 115.26(13) . . . . ? C13 N2 Cu1 O1 -4.94(14) . . . . ? C7 N2 Cu1 O5 54.08(14) . . . . ? C6 N2 Cu1 O5 -64.62(14) . . . . ? C13 N2 Cu1 O5 175.19(13) . . . . ? Cl1 O1 Cu1 O9 -75.35(11) . . . . ? Cl1 O1 Cu1 N1 -172.30(12) . . . . ? Cl1 O1 Cu1 N3 19.63(12) . . . . ? Cl1 O1 Cu1 N2 105.63(11) . . . . ? Cl1 O1 Cu1 O5 -74.8(2) . . . . ? Cl2 O5 Cu1 O9 -86.93(17) . . . . ? Cl2 O5 Cu1 N1 8.19(17) . . . . ? Cl2 O5 Cu1 N3 174.54(17) . . . . ? Cl2 O5 Cu1 N2 92.11(16) . . . . ? Cl2 O5 Cu1 O1 -87.5(3) . . . . ? C36 N6 Cu2 O19 24.0(2) . . . . ? C35 N6 Cu2 O19 -157.38(16) . . . . ? C36 N6 Cu2 N4 -177.8(3) . . . . ? C35 N6 Cu2 N4 0.8(4) . . . . ? C36 N6 Cu2 N5 -167.2(2) . . . . ? C35 N6 Cu2 N5 11.46(16) . . . . ? C36 N6 Cu2 O11 -63.7(2) . . . . ? C35 N6 Cu2 O11 114.96(16) . . . . ? C36 N6 Cu2 O15 105.3(2) . . . . ? C35 N6 Cu2 O15 -76.08(16) . . . . ? C28 N4 Cu2 O19 149.37(17) . . . . ? C32 N4 Cu2 O19 -33.2(2) . . . . ? C28 N4 Cu2 N6 -8.8(4) . . . . ? C32 N4 Cu2 N6 168.6(3) . . . . ? C28 N4 Cu2 N5 -19.49(17) . . . . ? C32 N4 Cu2 N5 157.9(2) . . . . ? C28 N4 Cu2 O11 -124.52(17) . . . . ? C32 N4 Cu2 O11 52.9(2) . . . . ? C28 N4 Cu2 O15 66.67(17) . . . . ? C32 N4 Cu2 O15 -115.9(2) . . . . ? C34 N5 Cu2 O19 66.9(5) . . . . ? C33 N5 Cu2 O19 -51.4(5) . . . . ? C40 N5 Cu2 O19 -172.1(4) . . . . ? C34 N5 Cu2 N6 -25.25(14) . . . . ? C33 N5 Cu2 N6 -143.60(14) . . . . ? C40 N5 Cu2 N6 95.73(14) . . . . ? C34 N5 Cu2 N4 152.22(15) . . . . ? C33 N5 Cu2 N4 33.88(14) . . . . ? C40 N5 Cu2 N4 -86.79(14) . . . . ? C34 N5 Cu2 O11 -124.11(13) . . . . ? C33 N5 Cu2 O11 117.54(13) . . . . ? C40 N5 Cu2 O11 -3.13(15) . . . . ? C34 N5 Cu2 O15 57.35(14) . . . . ? C33 N5 Cu2 O15 -61.00(13) . . . . ? C40 N5 Cu2 O15 178.33(14) . . . . ? Cl3 O11 Cu2 O19 -90.54(14) . . . . ? Cl3 O11 Cu2 N6 5.21(15) . . . . ? Cl3 O11 Cu2 N4 172.73(14) . . . . ? Cl3 O11 Cu2 N5 91.57(14) . . . . ? Cl3 O11 Cu2 O15 -96.0(3) . . . . ? Cl4 O15 Cu2 O19 -67.18(18) . . . . ? Cl4 O15 Cu2 N6 -164.60(18) . . . . ? Cl4 O15 Cu2 N4 28.74(18) . . . . ? Cl4 O15 Cu2 N5 110.96(18) . . . . ? Cl4 O15 Cu2 O11 -61.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1O O20 0.892(14) 1.778(8) 2.640(3) 162(2) 2_655 O9 H2O O3 0.889(16) 2.36(2) 2.844(3) 114.7(19) . O19 H3O O20 0.890(18) 1.938(16) 2.706(3) 143(2) . O19 H4O O16 0.889(18) 2.371(17) 3.106(3) 140(2) 2 O20 H5O O8 0.891(17) 2.007(11) 2.839(3) 155(2) 2_645 O20 H5O Cl2 0.891(17) 3.002(16) 3.727(2) 140(2) 2_645 O20 H6O O7 0.890(12) 1.957(13) 2.841(3) 173(2) . O20 H6O O6 0.890(12) 2.68(2) 3.175(3) 116.0(19) . O20 H6O Cl2 0.890(12) 2.798(14) 3.572(2) 146(2) . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 31.56 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.169 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.088