# 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 _publ_contact_author_name 'Samiran Mitra' _publ_contact_author_email 'SMITRA 2002@YAHOO.COM' _publ_section_title ; Four New Dinuclear Cu(II) Hydrazone Complexes Using Various Organic Spacers: Syntheses, Crystal Structures, DNA Binding and Cleavage Studies and Selective Cell Inhibitory Effect Towards Leukemic and Normal Lymphocytes ; _publ_contact_author ; Prof. Corrado Rizzoli Universit\'a degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale G. P. Usberti 17/A I-43100 Parma" Italy ; loop_ _publ_author_name 'Samiran Mitra' 'Sambuddha Banerjee' 'Saurabh Das' 'Cedric Desplanches' 'David L Hughes' 'Chitra Mandal' ; S.Mondal ; 'Corrado Rizzoli' 'Soma Sen' # Attachment 'compounds_1-4.cif' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 638166' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 1' _chemical_melting_point ? _chemical_formula_structural '[Cu(L)(OH2)}2(mu-pyrazine)].2(ClO4)' _chemical_formula_moiety 'C30 H28 Cu2 N8 O4, 2(Cl O4)' _chemical_formula_sum 'C30 H28 Cl2 Cu2 N8 O12' _chemical_formula_weight 890.6 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.141(2) _cell_length_b 12.2329(17) _cell_length_c 17.302(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.719(18) _cell_angle_gamma 90.00 _cell_volume 1714.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'very dark' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.164 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 19745 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3824 _reflns_number_gt 3146 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0560P)^2^+2.3031P] 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 3824 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Cu Cu 0.09878(5) 0.73262(3) 0.489994(18) 0.02018(12) Uani 1 1 d . . . O1 O 0.0132(3) 0.70355(16) 0.59003(11) 0.0226(4) Uani 1 1 d . . . C1 C 0.0528(3) 0.6074(2) 0.61437(14) 0.0190(5) Uani 1 1 d . . . C11 C -0.0129(4) 0.5693(2) 0.68655(15) 0.0206(6) Uani 1 1 d . . . C12 C -0.1312(4) 0.6332(2) 0.71728(15) 0.0233(6) Uani 1 1 d . . . H12 H -0.1635 0.6994 0.6940 0.028 Uiso 1 1 calc R . . C13 C -0.2009(4) 0.5981(3) 0.78271(15) 0.0272(7) Uani 1 1 d . . . H13 H -0.2791 0.6413 0.8039 0.033 Uiso 1 1 calc R . . C14 C -0.1546(4) 0.4988(3) 0.81678(15) 0.0290(7) Uani 1 1 d . . . H14 H -0.2046 0.4746 0.8597 0.035 Uiso 1 1 calc R . . C15 C -0.0349(4) 0.4355(3) 0.78755(16) 0.0293(7) Uani 1 1 d . . . H15 H -0.0026 0.3697 0.8112 0.035 Uiso 1 1 calc R . . C16 C 0.0367(4) 0.4707(2) 0.72272(15) 0.0261(6) Uani 1 1 d . . . H16 H 0.1181 0.4287 0.7031 0.031 Uiso 1 1 calc R . . N2 N 0.1465(3) 0.53803(19) 0.57853(12) 0.0207(5) Uani 1 1 d . . . N3 N 0.1872(3) 0.58893(19) 0.51256(12) 0.0193(5) Uani 1 1 d . . . C4 C 0.2829(4) 0.5480(2) 0.46630(15) 0.0222(6) Uani 1 1 d . . . H4 H 0.3307 0.4792 0.4737 0.027 Uiso 1 1 calc R . . C41 C 0.3115(3) 0.6187(2) 0.40039(15) 0.0202(6) Uani 1 1 d . . . N42 N 0.2257(3) 0.71429(19) 0.39691(12) 0.0211(5) Uani 1 1 d . . . C43 C 0.2430(4) 0.7824(2) 0.33799(16) 0.0255(6) Uani 1 1 d . . . H43 H 0.1827 0.8471 0.3348 0.031 Uiso 1 1 calc R . . C44 C 0.3471(4) 0.7604(3) 0.28176(17) 0.0298(7) Uani 1 1 d . . . H44 H 0.3564 0.8094 0.2413 0.036 Uiso 1 1 calc R . . C45 C 0.4367(4) 0.6650(3) 0.28646(17) 0.0301(7) Uani 1 1 d . . . H45 H 0.5096 0.6495 0.2498 0.036 Uiso 1 1 calc R . . C46 C 0.4174(4) 0.5918(3) 0.34658(16) 0.0259(6) Uani 1 1 d . . . H46 H 0.4751 0.5262 0.3501 0.031 Uiso 1 1 calc R . . N51 N 0.0428(3) 0.89120(19) 0.49108(12) 0.0184(5) Uani 1 1 d . . . C52 C 0.1426(4) 0.9728(2) 0.47396(14) 0.0192(5) Uani 1 1 d . . . H52 H 0.2435 0.9564 0.4558 0.023 Uiso 1 1 calc R . . C56 C -0.0985(3) 0.9191(2) 0.51724(14) 0.0196(6) Uani 1 1 d . . . H56 H -0.1703 0.8644 0.5301 0.024 Uiso 1 1 calc R . . O6 O -0.1518(3) 0.6911(2) 0.42526(12) 0.0254(5) Uani 1 1 d . . . Cl8 Cl 0.51896(11) 0.77703(15) 0.57492(7) 0.0244(3) Uani 0.888(5) 1 d P . . O81 O 0.3554(3) 0.8150(2) 0.57219(14) 0.0386(6) Uani 1 1 d . . . O82 O 0.5242(4) 0.6706(3) 0.6093(2) 0.0648(12) Uani 0.888(5) 1 d P . . O83 O 0.6273(3) 0.8498(2) 0.62112(12) 0.0321(5) Uani 1 1 d . . . O84 O 0.5675(4) 0.7691(4) 0.49843(18) 0.0674(15) Uani 0.888(5) 1 d P . . Cl9 Cl 0.5189(11) 0.8144(9) 0.5602(5) 0.025(2) Uiso 0.112(5) 1 d P . . O91 O 0.512(2) 0.8816(16) 0.4965(11) 0.029(5) Uiso 0.112(5) 1 d P . . O92 O 0.591(2) 0.7074(15) 0.5427(12) 0.025(5) Uiso 0.112(5) 1 d P . . H61 H -0.225(7) 0.709(4) 0.447(3) 0.067(17) Uiso 1 1 d . . . H62 H -0.154(6) 0.630(5) 0.423(3) 0.075(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0273(2) 0.01832(19) 0.01550(17) 0.00149(12) 0.00524(13) 0.00280(14) O1 0.0302(12) 0.0209(10) 0.0176(9) 0.0014(7) 0.0062(8) 0.0042(8) C1 0.0213(15) 0.0208(13) 0.0143(11) -0.0003(9) -0.0015(10) -0.0026(11) C11 0.0233(15) 0.0221(13) 0.0158(12) -0.0023(10) -0.0016(10) -0.0021(11) C12 0.0269(16) 0.0246(14) 0.0177(12) 0.0011(10) -0.0008(11) 0.0000(12) C13 0.0308(17) 0.0338(17) 0.0173(13) -0.0017(11) 0.0043(11) -0.0003(13) C14 0.0392(19) 0.0335(16) 0.0146(12) 0.0027(11) 0.0045(11) -0.0058(14) C15 0.044(2) 0.0249(15) 0.0181(13) 0.0035(11) -0.0008(12) -0.0005(13) C16 0.0369(18) 0.0246(15) 0.0168(12) 0.0000(10) 0.0020(11) 0.0035(13) N2 0.0255(13) 0.0206(11) 0.0162(10) 0.0014(9) 0.0031(9) 0.0014(10) N3 0.0218(13) 0.0205(11) 0.0158(10) -0.0012(8) 0.0026(9) -0.0015(9) C4 0.0255(16) 0.0218(14) 0.0192(12) -0.0008(10) 0.0015(11) 0.0026(12) C41 0.0210(15) 0.0212(13) 0.0182(12) -0.0040(10) 0.0015(10) 0.0007(11) N42 0.0245(13) 0.0236(12) 0.0149(10) -0.0009(8) 0.0011(9) 0.0014(10) C43 0.0316(18) 0.0252(15) 0.0197(13) 0.0010(11) 0.0028(11) -0.0005(12) C44 0.0381(19) 0.0320(16) 0.0197(13) 0.0026(11) 0.0055(12) -0.0012(14) C45 0.0334(18) 0.0382(17) 0.0204(13) -0.0026(12) 0.0108(12) 0.0000(14) C46 0.0279(17) 0.0288(15) 0.0218(13) -0.0038(11) 0.0057(11) 0.0012(13) N51 0.0196(12) 0.0213(11) 0.0142(10) 0.0012(8) 0.0014(8) 0.0005(9) C52 0.0186(14) 0.0235(14) 0.0159(11) 0.0015(10) 0.0034(10) 0.0000(11) C56 0.0219(15) 0.0217(13) 0.0153(11) 0.0020(9) 0.0025(10) -0.0032(11) O6 0.0295(13) 0.0225(11) 0.0243(10) -0.0010(9) 0.0035(9) 0.0005(10) Cl8 0.0208(5) 0.0313(7) 0.0212(4) -0.0061(5) 0.0027(3) 0.0010(4) O81 0.0249(13) 0.0450(14) 0.0450(13) -0.0147(11) -0.0017(10) 0.0076(11) O82 0.059(2) 0.0308(17) 0.096(3) 0.0118(17) -0.031(2) 0.0005(15) O83 0.0277(13) 0.0465(14) 0.0222(10) -0.0074(9) 0.0032(9) -0.0108(10) O84 0.0366(19) 0.134(4) 0.0341(17) -0.045(2) 0.0161(14) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N3 1.924(2) . ? Cu O1 1.9615(19) . ? Cu N51 1.993(2) . ? Cu N42 2.011(2) . ? Cu O6 2.284(2) . ? O1 C1 1.279(3) . ? C1 N2 1.335(3) . ? C1 C11 1.482(4) . ? C11 C12 1.387(4) . ? C11 C16 1.399(4) . ? C12 C13 1.384(4) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 C16 1.383(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N2 N3 1.369(3) . ? N3 C4 1.274(4) . ? C4 C41 1.469(4) . ? C4 H4 0.9300 . ? C41 N42 1.360(4) . ? C41 C46 1.371(4) . ? N42 C43 1.335(4) . ? C43 C44 1.378(4) . ? C43 H43 0.9300 . ? C44 C45 1.375(5) . ? C44 H44 0.9300 . ? C45 C46 1.393(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? N51 C56 1.322(4) . ? N51 C52 1.339(4) . ? C52 C56 1.383(4) 3_576 ? C52 H52 0.9300 . ? C56 C52 1.383(4) 3_576 ? C56 H56 0.9300 . ? O6 H61 0.77(6) . ? O6 H62 0.75(6) . ? Cl8 Cl9 0.524(11) . ? Cl8 O92 1.203(19) . ? Cl8 O81 1.406(2) . ? Cl8 O84 1.422(3) . ? Cl8 O82 1.430(4) . ? Cl8 O83 1.438(2) . ? Cl8 O91 1.861(19) . ? O81 Cl9 1.367(9) . ? O82 O92 1.40(2) . ? O82 Cl9 1.953(13) . ? O83 Cl9 1.376(9) . ? O84 O92 1.079(19) . ? O84 Cl9 1.300(9) . ? O84 O91 1.45(2) . ? Cl9 O91 1.37(2) . ? Cl9 O92 1.48(2) . ? 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 N3 Cu O1 79.27(9) . . ? N3 Cu N51 165.52(9) . . ? O1 Cu N51 93.81(8) . . ? N3 Cu N42 81.32(10) . . ? O1 Cu N42 160.48(9) . . ? N51 Cu N42 104.62(9) . . ? N3 Cu O6 101.18(10) . . ? O1 Cu O6 90.81(9) . . ? N51 Cu O6 91.55(9) . . ? N42 Cu O6 95.03(9) . . ? C1 O1 Cu 110.94(17) . . ? O1 C1 N2 124.6(2) . . ? O1 C1 C11 117.8(2) . . ? N2 C1 C11 117.5(2) . . ? C12 C11 C16 119.6(3) . . ? C12 C11 C1 117.9(2) . . ? C16 C11 C1 122.4(3) . . ? C13 C12 C11 119.7(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 120.3(3) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C1 N2 N3 107.1(2) . . ? C4 N3 N2 123.9(2) . . ? C4 N3 Cu 118.14(19) . . ? N2 N3 Cu 117.89(17) . . ? N3 C4 C41 114.2(2) . . ? N3 C4 H4 122.9 . . ? C41 C4 H4 122.9 . . ? N42 C41 C46 122.1(3) . . ? N42 C41 C4 114.9(2) . . ? C46 C41 C4 123.0(3) . . ? C43 N42 C41 118.5(2) . . ? C43 N42 Cu 130.1(2) . . ? C41 N42 Cu 111.27(18) . . ? N42 C43 C44 122.4(3) . . ? N42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C45 C44 C43 118.9(3) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 119.4(3) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 118.6(3) . . ? C41 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C56 N51 C52 116.8(2) . . ? C56 N51 Cu 117.54(19) . . ? C52 N51 Cu 125.37(19) . . ? N51 C52 C56 121.2(3) . 3_576 ? N51 C52 H52 119.4 . . ? C56 C52 H52 119.4 3_576 . ? N51 C56 C52 122.0(3) . 3_576 ? N51 C56 H56 119.0 . . ? C52 C56 H56 119.0 3_576 . ? Cu O6 H61 114(4) . . ? Cu O6 H62 105(4) . . ? H61 O6 H62 107(5) . . ? O81 Cl8 O84 110.0(2) . . ? O81 Cl8 O82 107.7(2) . . ? O84 Cl8 O82 109.0(3) . . ? O81 Cl8 O83 109.88(16) . . ? O84 Cl8 O83 110.34(19) . . ? O82 Cl8 O83 109.92(19) . . ? O81 Cl9 O91 98.9(11) . . ? O81 Cl9 O83 116.2(6) . . ? O91 Cl9 O83 113.6(11) . . ? O81 Cl9 O92 116.6(11) . . ? O91 Cl9 O92 110.6(13) . . ? O83 Cl9 O92 101.4(10) . . ? 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 N3 Cu O1 C1 -2.91(18) . . . . ? N51 Cu O1 C1 -170.07(19) . . . . ? N42 Cu O1 C1 -9.3(4) . . . . ? O6 Cu O1 C1 98.32(19) . . . . ? Cu O1 C1 N2 3.1(3) . . . . ? Cu O1 C1 C11 -175.57(18) . . . . ? O1 C1 C11 C12 8.9(4) . . . . ? N2 C1 C11 C12 -169.8(2) . . . . ? O1 C1 C11 C16 -173.0(3) . . . . ? N2 C1 C11 C16 8.3(4) . . . . ? C16 C11 C12 C13 -1.0(4) . . . . ? C1 C11 C12 C13 177.2(3) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? C12 C13 C14 C15 2.1(5) . . . . ? C13 C14 C15 C16 -1.3(5) . . . . ? C14 C15 C16 C11 -0.6(5) . . . . ? C12 C11 C16 C15 1.8(4) . . . . ? C1 C11 C16 C15 -176.3(3) . . . . ? O1 C1 N2 N3 -0.9(4) . . . . ? C11 C1 N2 N3 177.7(2) . . . . ? C1 N2 N3 C4 176.4(3) . . . . ? C1 N2 N3 Cu -1.9(3) . . . . ? O1 Cu N3 C4 -175.6(2) . . . . ? N51 Cu N3 C4 -113.2(4) . . . . ? N42 Cu N3 C4 2.2(2) . . . . ? O6 Cu N3 C4 95.7(2) . . . . ? O1 Cu N3 N2 2.74(18) . . . . ? N51 Cu N3 N2 65.1(5) . . . . ? N42 Cu N3 N2 -179.4(2) . . . . ? O6 Cu N3 N2 -85.95(19) . . . . ? N2 N3 C4 C41 -178.6(2) . . . . ? Cu N3 C4 C41 -0.3(3) . . . . ? N3 C4 C41 N42 -2.9(4) . . . . ? N3 C4 C41 C46 176.4(3) . . . . ? C46 C41 N42 C43 1.6(4) . . . . ? C4 C41 N42 C43 -179.0(3) . . . . ? C46 C41 N42 Cu -174.9(2) . . . . ? C4 C41 N42 Cu 4.5(3) . . . . ? N3 Cu N42 C43 -179.6(3) . . . . ? O1 Cu N42 C43 -173.3(3) . . . . ? N51 Cu N42 C43 -13.1(3) . . . . ? O6 Cu N42 C43 79.8(3) . . . . ? N3 Cu N42 C41 -3.65(19) . . . . ? O1 Cu N42 C41 2.7(4) . . . . ? N51 Cu N42 C41 162.86(18) . . . . ? O6 Cu N42 C41 -104.22(19) . . . . ? C41 N42 C43 C44 -1.5(4) . . . . ? Cu N42 C43 C44 174.3(2) . . . . ? N42 C43 C44 C45 -0.1(5) . . . . ? C43 C44 C45 C46 1.6(5) . . . . ? N42 C41 C46 C45 -0.2(4) . . . . ? C4 C41 C46 C45 -179.5(3) . . . . ? C44 C45 C46 C41 -1.4(5) . . . . ? N3 Cu N51 C56 -100.2(4) . . . . ? O1 Cu N51 C56 -39.42(19) . . . . ? N42 Cu N51 C56 147.10(18) . . . . ? O6 Cu N51 C56 51.49(19) . . . . ? N3 Cu N51 C52 73.6(4) . . . . ? O1 Cu N51 C52 134.3(2) . . . . ? N42 Cu N51 C52 -39.1(2) . . . . ? O6 Cu N51 C52 -134.7(2) . . . . ? C56 N51 C52 C56 -0.6(4) . . . 3_576 ? Cu N51 C52 C56 -174.35(18) . . . 3_576 ? C52 N51 C56 C52 0.6(4) . . . 3_576 ? Cu N51 C56 C52 174.86(19) . . . 3_576 ? 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 O6 H61 O84 0.77(6) 2.11(6) 2.883(4) 175(5) 1_455 O6 H61 O92 0.77(6) 2.34(6) 3.07(2) 157(5) 1_455 O6 H62 N2 0.75(6) 2.05(6) 2.804(3) 177(6) 3_566 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.622 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.091 #===END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 643522' ##################################################################### # CHEMICAL INFORMATION # ##################################################################### _chemical_name_systematic ? _chemical_name_common 'Compound 3' _chemical_formula_moiety 'C38 H34 Cu2 N6 O4, 2(Cl O4)' _chemical_formula_sum 'C38 H34 Cl2 Cu2 N6 O12' _chemical_formula_weight 964.72 _chemical_melting_point ? _chemical_compound_source ? ##################################################################### # UNIT CELL INFORMATION # ##################################################################### _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.0479(16) _cell_length_b 16.0303(17) _cell_length_c 19.1499(19) _cell_angle_alpha 72.222(2) _cell_angle_beta 89.242(2) _cell_angle_gamma 65.772(2) _cell_volume 3977.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3872 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 21.80 ##################################################################### # CRYSTAL INFORMATION # ##################################################################### _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_special_details ? ##################################################################### # ABSORPTION CORRECTION # ##################################################################### _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_T_max 0.865 ##################################################################### # DATA COLLECTION # ##################################################################### _diffrn_ambient_temperature 295(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42320 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 14825 _reflns_number_gt 7095 _reflns_threshold_expression I>2\s(I) ##################################################################### # COMPUTING PROGRAMS # ##################################################################### _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELX97-L (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? ##################################################################### # REFINEMENT INFORMATION # ##################################################################### _refine_special_details ; Some C atoms of phenyl rings and O atoms of perchlorato anions showed unreasonably high displacement parameters indicating the presence of positional disorder. Atoms C12-C17, C29-C34, C67-C72, O12, O15, O17, O18 and O24 were therefore split over two positions (called A and B) and refined by allowing two distinct site ocupation factors for the C and O atoms to vary freely. Refined occupancy factors converged to almost equal values of 0.608(7) and 0.63(3) for the major components of the disordered C and O atoms respectively. The anisotropic displacement parameters of the disordered O atoms were restrained to be approximately isotropic, and their Cl-O distances constrained to be equal. The disordered C atoms could not be refined anisotropically. The disordered phenyl rings were modelled with geometries constrained to be regular hexagons (C-C 1.39 \%A). All H atoms were positioned geometrically and refined using the riding-model approximation, with C-H = 0.93-0.96 \%A, N-H = 0.86 \%A, and with U~iso~(H) = 1.2 U~eq~(C, N) or 1.5 U~eq~(C) for methyl H atoms. The poor quality of the crystal and the presence of disorder may account for the rather low observed/unique reflection ratio (48%). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^] 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 14825 _refine_ls_number_parameters 1039 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1333 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_details ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.566 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.081 ##################################################################### # ATOMIC TYPES, COORDINATES AND DISPLACEMENT PARAMETERS # ##################################################################### loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.63195(4) 0.10765(4) 0.94763(3) 0.04315(16) Uani 1 1 d . . . Cu2 Cu 0.64645(4) 0.10058(4) 0.59641(3) 0.04719(17) Uani 1 1 d . . . Cu3 Cu 0.14956(4) 0.09049(4) 0.85225(3) 0.04461(16) Uani 1 1 d . . . Cu4 Cu 0.13068(4) 0.10311(4) 0.49684(3) 0.04404(17) Uani 1 1 d . . . Cl1 Cl 0.81617(12) -0.28375(11) 0.87222(7) 0.0639(4) Uani 1 1 d D . . Cl2 Cl 0.30871(13) -0.28640(11) 0.77316(7) 0.0716(4) Uani 1 1 d D . . Cl3 Cl 0.40040(11) 0.18678(11) 0.64960(8) 0.0648(4) Uani 1 1 d D . . Cl4 Cl -0.09578(10) 0.18692(11) 0.75525(8) 0.0600(4) Uani 1 1 d D . . O1 O 0.63012(19) -0.01413(19) 0.98520(14) 0.0394(7) Uani 1 1 d . . . O2 O 0.6285(2) 0.2357(2) 0.91451(14) 0.0465(8) Uani 1 1 d . B . O3 O 0.6548(2) -0.0255(2) 0.62082(14) 0.0473(8) Uani 1 1 d . . . O4 O 0.6430(2) 0.2292(2) 0.56352(16) 0.0533(9) Uani 1 1 d . B . O5 O 0.1552(2) -0.0344(2) 0.89206(15) 0.0441(8) Uani 1 1 d . . . O6 O 0.1515(2) 0.2169(2) 0.81953(14) 0.0465(8) Uani 1 1 d . . . O7 O 0.1304(2) -0.01858(19) 0.52070(14) 0.0425(8) Uani 1 1 d . . . O8 O 0.1247(2) 0.2319(2) 0.46523(15) 0.0498(8) Uani 1 1 d . B . O9 O 0.8050(4) -0.3684(3) 0.8895(2) 0.1219(17) Uani 1 1 d . A . O10 O 0.8719(4) -0.2799(3) 0.8131(2) 0.1221(16) Uani 1 1 d . A . O11 O 0.8655(3) -0.2849(3) 0.9348(2) 0.1176(16) Uani 1 1 d . A . O12A O 0.7365(12) -0.1919(8) 0.8489(8) 0.104(5) Uani 0.63(3) 1 d PDU A 1 O12B O 0.7082(13) -0.227(2) 0.8589(13) 0.105(8) Uani 0.37(3) 1 d PDU A 2 O13 O 0.3625(4) -0.2890(3) 0.7127(2) 0.1345(19) Uani 1 1 d . A . O14 O 0.3054(3) -0.3747(3) 0.8041(2) 0.1117(15) Uani 1 1 d . A . O15A O 0.2023(10) -0.2227(12) 0.7521(8) 0.107(5) Uani 0.63(3) 1 d PDU A 1 O15B O 0.2383(19) -0.1927(12) 0.7441(12) 0.100(7) Uani 0.37(3) 1 d PDU A 2 O16 O 0.3537(4) -0.2696(4) 0.8276(2) 0.1377(19) Uani 1 1 d . A . O17A O 0.4676(10) 0.1609(18) 0.5997(8) 0.105(6) Uani 0.63(3) 1 d PDU A 1 O18A O 0.4008(8) 0.1011(8) 0.7043(10) 0.111(5) Uani 0.63(3) 1 d PDU A 1 O17B O 0.4613(17) 0.2084(16) 0.5984(12) 0.063(5) Uani 0.37(3) 1 d PDU A 2 O18B O 0.3948(16) 0.1009(14) 0.652(2) 0.116(9) Uani 0.37(3) 1 d PDU A 2 O19 O 0.3072(3) 0.2572(3) 0.6147(2) 0.1045(14) Uani 1 1 d . A . O20 O 0.4346(4) 0.2180(4) 0.6999(2) 0.1409(19) Uani 1 1 d . A . O21 O -0.0577(3) 0.2222(3) 0.6910(2) 0.1128(15) Uani 1 1 d . A . O22 O -0.1002(3) 0.1028(3) 0.7541(3) 0.148(2) Uani 1 1 d . A . O23 O -0.1882(3) 0.2573(3) 0.7569(2) 0.0956(13) Uani 1 1 d . A . O24A O -0.0310(11) 0.1872(15) 0.8084(9) 0.087(5) Uani 0.63(3) 1 d PD A 1 O24B O -0.0318(19) 0.140(2) 0.8227(10) 0.071(6) Uani 0.37(3) 1 d PD A 2 N1 N 0.6162(2) 0.1314(3) 1.03960(18) 0.0379(9) Uani 1 1 d . . . N2 N 0.6123(2) 0.2215(3) 1.03295(19) 0.0435(9) Uani 1 1 d . B . H2N H 0.6056 0.2429 1.0697 0.052 Uiso 1 1 calc R . . N3 N 0.6354(2) 0.1229(3) 0.49322(18) 0.0414(9) Uani 1 1 d . . . N4 N 0.6272(3) 0.2141(3) 0.45376(18) 0.0490(10) Uani 1 1 d . B . H4N H 0.6211 0.2352 0.4062 0.059 Uiso 1 1 calc R . . N5 N 0.1386(2) 0.1131(3) 0.94482(18) 0.0385(9) Uani 1 1 d . . . N6 N 0.1344(2) 0.2035(3) 0.93706(19) 0.0419(9) Uani 1 1 d . . . H6N H 0.1283 0.2249 0.9737 0.050 Uiso 1 1 calc R . . N7 N 0.1135(2) 0.1292(3) 0.39283(17) 0.0388(9) Uani 1 1 d . . . N8 N 0.1076(3) 0.2200(3) 0.35401(18) 0.0461(10) Uani 1 1 d . B . H8N H 0.1000 0.2422 0.3065 0.055 Uiso 1 1 calc R . . N9 N 0.6466(2) 0.0974(3) 0.84582(18) 0.0396(9) Uani 1 1 d . . . N10 N 0.6589(3) 0.0914(3) 0.70310(19) 0.0439(10) Uani 1 1 d . . . N11 N 0.1620(2) 0.0817(3) 0.74973(18) 0.0398(9) Uani 1 1 d . . . N12 N 0.1451(2) 0.0912(3) 0.60342(17) 0.0403(9) Uani 1 1 d . . . C1 C 0.5928(3) -0.1964(3) 1.1335(2) 0.0476(12) Uani 1 1 d . . . H1 H 0.5772 -0.1676 1.1702 0.057 Uiso 1 1 calc R . . C2 C 0.5933(4) -0.2855(4) 1.1456(3) 0.0608(14) Uani 1 1 d . . . H2 H 0.5774 -0.3162 1.1902 0.073 Uiso 1 1 calc R . . C3 C 0.6171(4) -0.3303(4) 1.0924(3) 0.0622(14) Uani 1 1 d . . . H3 H 0.6178 -0.3909 1.1009 0.075 Uiso 1 1 calc R . . C4 C 0.6397(4) -0.2842(4) 1.0271(3) 0.0596(14) Uani 1 1 d . . . H4 H 0.6570 -0.3143 0.9913 0.072 Uiso 1 1 calc R . . C5 C 0.6371(3) -0.1943(3) 1.0135(2) 0.0485(13) Uani 1 1 d . . . H5 H 0.6502 -0.1628 0.9679 0.058 Uiso 1 1 calc R . . C6 C 0.6152(3) -0.1495(3) 1.0675(2) 0.0393(11) Uani 1 1 d . . . C7 C 0.6168(3) -0.0525(3) 1.0517(2) 0.0385(11) Uani 1 1 d . . . C8 C 0.6046(3) -0.0112(3) 1.1070(2) 0.0454(12) Uani 1 1 d . . . H8 H 0.5985 -0.0479 1.1534 0.054 Uiso 1 1 calc R . . C9 C 0.6003(3) 0.0799(3) 1.1007(2) 0.0428(12) Uani 1 1 d . . . C10 C 0.5774(4) 0.1140(4) 1.1668(2) 0.0751(17) Uani 1 1 d . . . H10A H 0.6355 0.1122 1.1886 0.113 Uiso 1 1 calc R . . H10B H 0.5552 0.0725 1.2025 0.113 Uiso 1 1 calc R . . H10C H 0.5269 0.1792 1.1513 0.113 Uiso 1 1 calc R . . C11 C 0.6198(3) 0.2725(3) 0.9656(2) 0.0406(11) Uani 1 1 d . . . C12A C 0.6115(5) 0.3707(4) 0.9496(3) 0.049(7) Uiso 0.608(7) 1 d PG B 1 C13A C 0.5786(5) 0.4349(4) 0.8778(3) 0.047(2) Uiso 0.608(7) 1 d PG B 1 H13A H 0.5593 0.4160 0.8415 0.056 Uiso 0.608(7) 1 calc PR B 1 C14A C 0.5744(5) 0.5273(4) 0.8602(3) 0.065(3) Uiso 0.608(7) 1 d PG B 1 H14A H 0.5524 0.5703 0.8122 0.078 Uiso 0.608(7) 1 calc PR B 1 C15A C 0.6032(5) 0.5555(4) 0.9145(4) 0.073(4) Uiso 0.608(7) 1 d PG B 1 H15A H 0.6005 0.6173 0.9028 0.088 Uiso 0.608(7) 1 calc PR B 1 C16A C 0.6362(5) 0.4913(5) 0.9863(3) 0.067(4) Uiso 0.608(7) 1 d PG B 1 H16A H 0.6554 0.5102 1.0227 0.080 Uiso 0.608(7) 1 calc PR B 1 C17A C 0.6403(5) 0.3989(5) 1.0039(3) 0.052(3) Uiso 0.608(7) 1 d PG B 1 H17A H 0.6623 0.3559 1.0520 0.062 Uiso 0.608(7) 1 calc PR B 1 C12B C 0.6228(8) 0.3662(6) 0.9494(5) 0.044(10) Uiso 0.392(7) 1 d PG B 2 C13B C 0.6422(9) 0.4070(8) 0.8792(5) 0.069(4) Uiso 0.392(7) 1 d PG B 2 H13B H 0.6525 0.3747 0.8448 0.083 Uiso 0.392(7) 1 calc PR B 2 C14B C 0.6461(10) 0.4962(8) 0.8603(5) 0.103(6) Uiso 0.392(7) 1 d PG B 2 H14B H 0.6591 0.5236 0.8133 0.123 Uiso 0.392(7) 1 calc PR B 2 C15B C 0.6307(9) 0.5445(7) 0.9117(6) 0.091(7) Uiso 0.392(7) 1 d PG B 2 H15B H 0.6333 0.6042 0.8990 0.109 Uiso 0.392(7) 1 calc PR B 2 C16B C 0.6113(8) 0.5036(8) 0.9819(6) 0.071(6) Uiso 0.392(7) 1 d PG B 2 H16B H 0.6010 0.5360 1.0163 0.085 Uiso 0.392(7) 1 calc PR B 2 C17B C 0.6074(8) 0.4145(8) 1.0008(4) 0.052(4) Uiso 0.392(7) 1 d PG B 2 H17B H 0.5944 0.3871 1.0478 0.062 Uiso 0.392(7) 1 calc PR B 2 C18 C 0.6280(4) -0.2130(4) 0.5652(3) 0.0627(15) Uani 1 1 d . . . H18 H 0.6206 -0.1876 0.5139 0.075 Uiso 1 1 calc R . . C19 C 0.6248(4) -0.3002(4) 0.5977(3) 0.0742(17) Uani 1 1 d . . . H19 H 0.6155 -0.3334 0.5684 0.089 Uiso 1 1 calc R . . C20 C 0.6350(4) -0.3387(4) 0.6724(3) 0.0779(17) Uani 1 1 d . . . H20 H 0.6329 -0.3981 0.6944 0.093 Uiso 1 1 calc R . . C21 C 0.6486(4) -0.2889(4) 0.7151(3) 0.0767(17) Uani 1 1 d . . . H21 H 0.6563 -0.3150 0.7664 0.092 Uiso 1 1 calc R . . C22 C 0.6509(3) -0.2011(3) 0.6829(2) 0.0553(14) Uani 1 1 d . . . H22 H 0.6586 -0.1677 0.7127 0.066 Uiso 1 1 calc R . . C23 C 0.6421(3) -0.1613(3) 0.6076(2) 0.0430(12) Uani 1 1 d . . . C24 C 0.6440(3) -0.0652(3) 0.5739(2) 0.0399(11) Uani 1 1 d . . . C25 C 0.6362(3) -0.0249(3) 0.4983(2) 0.0456(12) Uani 1 1 d . . . H25 H 0.6353 -0.0634 0.4708 0.055 Uiso 1 1 calc R . . C26 C 0.6297(3) 0.0664(3) 0.4580(2) 0.0421(11) Uani 1 1 d . . . C27 C 0.6167(3) 0.0983(3) 0.3759(2) 0.0553(13) Uani 1 1 d . . . H27A H 0.5574 0.1569 0.3569 0.083 Uiso 1 1 calc R . . H27B H 0.6124 0.0487 0.3598 0.083 Uiso 1 1 calc R . . H27C H 0.6718 0.1099 0.3578 0.083 Uiso 1 1 calc R . . C28 C 0.6295(3) 0.2670(3) 0.4950(3) 0.0491(12) Uani 1 1 d . . . C29A C 0.6051(5) 0.3712(4) 0.4565(4) 0.051(3) Uiso 0.608(7) 1 d PG B 1 C30A C 0.5630(6) 0.4211(5) 0.3832(4) 0.079(3) Uiso 0.608(7) 1 d PG B 1 H30A H 0.5454 0.3901 0.3557 0.095 Uiso 0.608(7) 1 calc PR B 1 C31A C 0.5473(6) 0.5171(5) 0.3511(3) 0.106(4) Uiso 0.608(7) 1 d PG B 1 H31A H 0.5192 0.5504 0.3020 0.127 Uiso 0.608(7) 1 calc PR B 1 C32A C 0.5737(6) 0.5633(4) 0.3922(4) 0.091(3) Uiso 0.608(7) 1 d PG B 1 H32A H 0.5632 0.6276 0.3707 0.110 Uiso 0.608(7) 1 calc PR B 1 C33A C 0.6157(5) 0.5135(5) 0.4655(4) 0.081(3) Uiso 0.608(7) 1 d PG B 1 H33A H 0.6334 0.5445 0.4930 0.097 Uiso 0.608(7) 1 calc PR B 1 C34A C 0.6314(5) 0.4175(5) 0.4976(3) 0.077(3) Uiso 0.608(7) 1 d PG B 1 H34A H 0.6595 0.3841 0.5467 0.092 Uiso 0.608(7) 1 calc PR B 1 C29B C 0.6360(8) 0.3570(6) 0.4664(5) 0.045(4) Uiso 0.392(7) 1 d PG B 2 C30B C 0.6076(8) 0.4120(7) 0.3920(5) 0.057(4) Uiso 0.392(7) 1 d PG B 2 H30B H 0.5906 0.3871 0.3591 0.069 Uiso 0.392(7) 1 calc PR B 2 C31B C 0.6046(8) 0.5042(6) 0.3667(4) 0.081(5) Uiso 0.392(7) 1 d PG B 2 H31B H 0.5856 0.5410 0.3169 0.097 Uiso 0.392(7) 1 calc PR B 2 C32B C 0.6301(8) 0.5415(6) 0.4159(6) 0.070(4) Uiso 0.392(7) 1 d PG B 2 H32B H 0.6281 0.6032 0.3990 0.085 Uiso 0.392(7) 1 calc PR B 2 C33B C 0.6585(9) 0.4865(8) 0.4904(5) 0.120(7) Uiso 0.392(7) 1 d PG B 2 H33B H 0.6755 0.5115 0.5233 0.144 Uiso 0.392(7) 1 calc PR B 2 C34B C 0.6615(9) 0.3943(8) 0.5156(4) 0.086(5) Uiso 0.392(7) 1 d PG B 2 H34B H 0.6805 0.3575 0.5655 0.103 Uiso 0.392(7) 1 calc PR B 2 C35 C 0.6338(3) 0.0284(3) 0.8266(2) 0.0469(12) Uani 1 1 d . . . H35 H 0.6201 -0.0183 0.8614 0.056 Uiso 1 1 calc R . . C36 C 0.6411(3) 0.0275(3) 0.7557(2) 0.0489(13) Uani 1 1 d . . . H36 H 0.6329 -0.0213 0.7440 0.059 Uiso 1 1 calc R . . C37 C 0.6731(4) 0.1574(4) 0.7228(2) 0.0578(14) Uani 1 1 d . . . H37 H 0.6883 0.2027 0.6877 0.069 Uiso 1 1 calc R . . C38 C 0.6663(3) 0.1612(4) 0.7934(2) 0.0551(14) Uani 1 1 d . . . H38 H 0.6757 0.2097 0.8047 0.066 Uiso 1 1 calc R . . C39 C 0.1296(4) -0.2222(4) 1.0439(3) 0.0625(15) Uani 1 1 d . . . H39 H 0.1310 -0.2009 1.0838 0.075 Uiso 1 1 calc R . . C40 C 0.1202(4) -0.3072(4) 1.0556(3) 0.0715(16) Uani 1 1 d . . . H40 H 0.1138 -0.3417 1.1027 0.086 Uiso 1 1 calc R . . C41 C 0.1202(4) -0.3410(4) 0.9980(3) 0.0683(16) Uani 1 1 d . . . H41 H 0.1149 -0.3988 1.0054 0.082 Uiso 1 1 calc R . . C42 C 0.1281(4) -0.2883(4) 0.9301(3) 0.0731(16) Uani 1 1 d . . . H42 H 0.1280 -0.3108 0.8907 0.088 Uiso 1 1 calc R . . C43 C 0.1364(4) -0.2025(3) 0.9172(3) 0.0577(14) Uani 1 1 d . . . H43 H 0.1415 -0.1680 0.8697 0.069 Uiso 1 1 calc R . . C44 C 0.1370(3) -0.1677(3) 0.9748(2) 0.0411(11) Uani 1 1 d . . . C45 C 0.1430(3) -0.0723(3) 0.9587(2) 0.0383(11) Uani 1 1 d . . . C46 C 0.1355(3) -0.0329(3) 1.0147(2) 0.0447(12) Uani 1 1 d . . . H46 H 0.1327 -0.0709 1.0616 0.054 Uiso 1 1 calc R . . C47 C 0.1315(3) 0.0587(3) 1.0086(2) 0.0387(11) Uani 1 1 d . . . C48 C 0.1209(3) 0.0890(3) 1.0751(2) 0.0487(12) Uani 1 1 d . . . H48A H 0.1785 0.0961 1.0873 0.073 Uiso 1 1 calc R . . H48B H 0.1131 0.0409 1.1157 0.073 Uiso 1 1 calc R . . H48C H 0.0643 0.1498 1.0653 0.073 Uiso 1 1 calc R . . C49 C 0.1404(3) 0.2546(3) 0.8704(2) 0.0405(11) Uani 1 1 d . . . C50 C 0.1357(3) 0.3513(3) 0.8535(2) 0.0443(12) Uani 1 1 d . . . C51 C 0.0940(4) 0.4083(4) 0.8982(3) 0.0629(14) Uani 1 1 d . . . H51 H 0.0683 0.3853 0.9404 0.075 Uiso 1 1 calc R . . C52 C 0.0920(5) 0.5001(4) 0.8778(3) 0.0847(19) Uani 1 1 d . . . H52 H 0.0637 0.5391 0.9067 0.102 Uiso 1 1 calc R . . C53 C 0.1300(5) 0.5342(4) 0.8173(4) 0.087(2) Uani 1 1 d . . . H53 H 0.1291 0.5953 0.8056 0.105 Uiso 1 1 calc R . . C54 C 0.1696(4) 0.4791(4) 0.7733(3) 0.0809(18) Uani 1 1 d . . . H54 H 0.1951 0.5030 0.7313 0.097 Uiso 1 1 calc R . . C55 C 0.1721(4) 0.3885(4) 0.7906(3) 0.0609(14) Uani 1 1 d . . . H55 H 0.1983 0.3518 0.7598 0.073 Uiso 1 1 calc R . . C56 C 0.1033(4) -0.2047(3) 0.4652(3) 0.0560(14) Uani 1 1 d . . . H56 H 0.0912 -0.1770 0.4139 0.067 Uiso 1 1 calc R . . C57 C 0.1038(4) -0.2938(4) 0.4971(3) 0.0729(16) Uani 1 1 d . . . H57 H 0.0914 -0.3255 0.4677 0.088 Uiso 1 1 calc R . . C58 C 0.1227(4) -0.3368(4) 0.5729(3) 0.0722(16) Uani 1 1 d . . . H58 H 0.1236 -0.3975 0.5950 0.087 Uiso 1 1 calc R . . C59 C 0.1401(4) -0.2878(4) 0.6152(3) 0.0663(15) Uani 1 1 d . . . H59 H 0.1539 -0.3161 0.6664 0.080 Uiso 1 1 calc R . . C60 C 0.1371(3) -0.1981(3) 0.5822(2) 0.0510(13) Uani 1 1 d . . . H60 H 0.1467 -0.1652 0.6117 0.061 Uiso 1 1 calc R . . C61 C 0.1203(3) -0.1550(3) 0.5067(2) 0.0405(11) Uani 1 1 d . . . C62 C 0.1191(3) -0.0583(3) 0.4729(2) 0.0385(11) Uani 1 1 d . . . C63 C 0.1075(3) -0.0164(3) 0.3981(2) 0.0437(12) Uani 1 1 d . . . H63 H 0.1034 -0.0536 0.3703 0.052 Uiso 1 1 calc R . . C64 C 0.1008(3) 0.0756(3) 0.3576(2) 0.0422(12) Uani 1 1 d . . . C65 C 0.0787(4) 0.1110(3) 0.2750(2) 0.0735(17) Uani 1 1 d . . . H65A H 0.0828 0.0588 0.2586 0.110 Uiso 1 1 calc R . . H65B H 0.1254 0.1345 0.2534 0.110 Uiso 1 1 calc R . . H65C H 0.0136 0.1625 0.2601 0.110 Uiso 1 1 calc R . . C66 C 0.1146(3) 0.2704(3) 0.3962(3) 0.0470(12) Uani 1 1 d . . . C67A C 0.1123(5) 0.3662(4) 0.3654(4) 0.051(5) Uiso 0.608(7) 1 d PGU B 1 C68A C 0.0922(6) 0.4171(6) 0.2900(4) 0.058(3) Uiso 0.608(7) 1 d PGU B 1 H68A H 0.0797 0.3898 0.2570 0.070 Uiso 0.608(7) 1 calc PR B 1 C69A C 0.0906(6) 0.5087(6) 0.2640(3) 0.089(5) Uiso 0.608(7) 1 d PGU B 1 H69A H 0.0772 0.5428 0.2136 0.107 Uiso 0.608(7) 1 calc PR B 1 C70A C 0.1092(6) 0.5494(5) 0.3134(5) 0.127(6) Uiso 0.608(7) 1 d PGU B 1 H70A H 0.1082 0.6107 0.2960 0.152 Uiso 0.608(7) 1 calc PR B 1 C71A C 0.1293(6) 0.4985(6) 0.3888(4) 0.102(4) Uiso 0.608(7) 1 d PGU B 1 H71A H 0.1417 0.5258 0.4218 0.122 Uiso 0.608(7) 1 calc PR B 1 C72A C 0.1308(6) 0.4069(5) 0.4148(3) 0.080(3) Uiso 0.608(7) 1 d PGU B 1 H72A H 0.1443 0.3728 0.4653 0.095 Uiso 0.608(7) 1 calc PR B 1 C67B C 0.1006(9) 0.3685(6) 0.3618(6) 0.063(10) Uiso 0.392(7) 1 d PGU B 2 C68B C 0.1184(9) 0.3993(8) 0.2891(6) 0.064(5) Uiso 0.392(7) 1 d PGU B 2 H68B H 0.1367 0.3570 0.2619 0.076 Uiso 0.392(7) 1 calc PR B 2 C69B C 0.1088(9) 0.4934(9) 0.2570(5) 0.081(7) Uiso 0.392(7) 1 d PGU B 2 H69B H 0.1207 0.5141 0.2083 0.098 Uiso 0.392(7) 1 calc PR B 2 C70B C 0.0814(9) 0.5567(7) 0.2975(6) 0.078(5) Uiso 0.392(7) 1 d PGU B 2 H70B H 0.0750 0.6197 0.2760 0.093 Uiso 0.392(7) 1 calc PR B 2 C71B C 0.0637(8) 0.5259(7) 0.3702(5) 0.072(4) Uiso 0.392(7) 1 d PGU B 2 H71B H 0.0453 0.5682 0.3974 0.087 Uiso 0.392(7) 1 calc PR B 2 C72B C 0.0732(8) 0.4318(8) 0.4023(5) 0.066(4) Uiso 0.392(7) 1 d PGU B 2 H72B H 0.0613 0.4112 0.4510 0.079 Uiso 0.392(7) 1 calc PR B 2 C73 C 0.1417(3) 0.0186(3) 0.7296(2) 0.0491(13) Uani 1 1 d . . . H73 H 0.1329 -0.0303 0.7659 0.059 Uiso 1 1 calc R . . C74 C 0.1333(3) 0.0227(3) 0.6574(2) 0.0436(12) Uani 1 1 d . . . H74 H 0.1191 -0.0233 0.6459 0.052 Uiso 1 1 calc R . . C75 C 0.1672(3) 0.1539(4) 0.6234(2) 0.0564(14) Uani 1 1 d . . . H75 H 0.1782 0.2018 0.5876 0.068 Uiso 1 1 calc R . . C76 C 0.1741(3) 0.1486(4) 0.6963(2) 0.0559(14) Uani 1 1 d . . . H76 H 0.1878 0.1945 0.7081 0.067 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 0.0582(4) 0.0530(4) 0.0333(3) -0.0216(3) 0.0101(3) -0.0328(3) Cu2 0.0656(4) 0.0611(4) 0.0336(3) -0.0233(3) 0.0121(3) -0.0395(3) Cu3 0.0629(4) 0.0559(4) 0.0327(3) -0.0226(3) 0.0113(3) -0.0367(3) Cu4 0.0656(4) 0.0493(4) 0.0310(3) -0.0175(3) 0.0096(3) -0.0347(3) Cl1 0.1021(12) 0.0644(10) 0.0395(8) -0.0227(7) 0.0109(8) -0.0451(10) Cl2 0.1271(15) 0.0670(11) 0.0397(8) -0.0210(8) 0.0158(9) -0.0571(11) Cl3 0.0695(10) 0.0739(11) 0.0641(9) -0.0299(9) 0.0194(8) -0.0384(9) Cl4 0.0661(10) 0.0689(10) 0.0612(9) -0.0306(8) 0.0101(8) -0.0377(9) O1 0.054(2) 0.0434(19) 0.0264(16) -0.0137(14) 0.0083(14) -0.0244(16) O2 0.069(2) 0.053(2) 0.0306(17) -0.0182(15) 0.0080(15) -0.0354(18) O3 0.069(2) 0.059(2) 0.0276(16) -0.0195(16) 0.0078(15) -0.0373(18) O4 0.083(2) 0.064(2) 0.0367(19) -0.0255(17) 0.0212(17) -0.048(2) O5 0.067(2) 0.055(2) 0.0307(17) -0.0224(16) 0.0144(15) -0.0391(18) O6 0.066(2) 0.052(2) 0.0345(17) -0.0189(16) 0.0098(15) -0.0338(18) O7 0.061(2) 0.0439(19) 0.0315(16) -0.0148(15) 0.0065(15) -0.0288(17) O8 0.078(2) 0.052(2) 0.0342(18) -0.0187(16) 0.0114(16) -0.0392(18) O9 0.187(5) 0.116(4) 0.130(4) -0.050(3) 0.044(3) -0.122(4) O10 0.188(5) 0.142(4) 0.070(3) -0.037(3) 0.062(3) -0.102(4) O11 0.180(5) 0.138(4) 0.070(3) -0.045(3) -0.011(3) -0.093(4) O12A 0.118(9) 0.059(6) 0.085(6) -0.016(5) -0.031(6) 0.004(6) O12B 0.126(14) 0.126(18) 0.061(9) -0.058(11) 0.020(9) -0.033(12) O13 0.226(6) 0.165(5) 0.067(3) -0.053(3) 0.078(3) -0.126(4) O14 0.163(4) 0.095(3) 0.116(3) -0.031(3) 0.033(3) -0.096(3) O15A 0.138(9) 0.099(8) 0.067(6) -0.043(6) -0.005(6) -0.023(7) O15B 0.116(15) 0.056(10) 0.091(10) 0.001(8) -0.001(10) -0.019(9) O16 0.230(6) 0.184(5) 0.081(3) -0.069(3) 0.017(3) -0.148(5) O17A 0.070(6) 0.196(17) 0.068(6) -0.088(10) 0.018(5) -0.042(9) O18A 0.135(7) 0.061(6) 0.109(10) 0.016(6) 0.022(7) -0.047(5) O17B 0.073(9) 0.089(12) 0.055(8) -0.033(7) 0.027(6) -0.054(9) O18B 0.166(14) 0.082(10) 0.18(2) -0.073(13) 0.092(15) -0.106(10) O19 0.070(3) 0.085(3) 0.143(4) -0.016(3) 0.005(3) -0.033(3) O20 0.185(5) 0.158(5) 0.081(3) -0.071(3) 0.006(3) -0.051(4) O21 0.139(4) 0.139(4) 0.067(3) -0.041(3) 0.027(3) -0.061(3) O22 0.137(4) 0.070(3) 0.263(6) -0.067(4) 0.012(4) -0.061(3) O23 0.065(3) 0.076(3) 0.154(4) -0.050(3) 0.013(3) -0.030(2) O24A 0.069(6) 0.155(14) 0.078(8) -0.076(8) 0.015(6) -0.061(9) O24B 0.073(9) 0.105(16) 0.029(6) -0.015(8) 0.000(6) -0.037(10) N1 0.043(2) 0.046(2) 0.036(2) -0.0209(19) 0.0099(18) -0.024(2) N2 0.061(3) 0.048(3) 0.035(2) -0.023(2) 0.0100(19) -0.030(2) N3 0.048(2) 0.047(3) 0.034(2) -0.010(2) 0.0099(18) -0.028(2) N4 0.067(3) 0.060(3) 0.026(2) -0.009(2) 0.0124(19) -0.036(2) N5 0.043(2) 0.049(3) 0.036(2) -0.023(2) 0.0070(18) -0.026(2) N6 0.057(3) 0.047(3) 0.036(2) -0.025(2) 0.0085(19) -0.029(2) N7 0.049(2) 0.044(2) 0.028(2) -0.0105(19) 0.0041(17) -0.025(2) N8 0.069(3) 0.045(3) 0.032(2) -0.009(2) 0.0047(19) -0.034(2) N9 0.044(2) 0.051(3) 0.035(2) -0.021(2) 0.0112(18) -0.027(2) N10 0.048(2) 0.058(3) 0.045(2) -0.023(2) 0.0071(19) -0.036(2) N11 0.049(2) 0.056(3) 0.034(2) -0.022(2) 0.0124(18) -0.036(2) N12 0.052(2) 0.055(3) 0.029(2) -0.018(2) 0.0121(18) -0.035(2) C1 0.059(3) 0.044(3) 0.048(3) -0.020(3) 0.017(2) -0.028(3) C2 0.071(4) 0.066(4) 0.054(3) -0.019(3) 0.015(3) -0.038(3) C3 0.067(4) 0.067(4) 0.071(4) -0.030(3) 0.013(3) -0.042(3) C4 0.075(4) 0.054(4) 0.067(4) -0.034(3) 0.010(3) -0.034(3) C5 0.067(3) 0.053(3) 0.040(3) -0.027(3) 0.017(2) -0.032(3) C6 0.033(3) 0.043(3) 0.046(3) -0.016(2) 0.001(2) -0.019(2) C7 0.035(3) 0.049(3) 0.034(3) -0.018(2) 0.002(2) -0.018(2) C8 0.061(3) 0.055(3) 0.034(3) -0.021(2) 0.013(2) -0.033(3) C9 0.054(3) 0.058(3) 0.033(3) -0.023(2) 0.011(2) -0.034(3) C10 0.133(5) 0.079(4) 0.048(3) -0.038(3) 0.034(3) -0.066(4) C11 0.040(3) 0.047(3) 0.043(3) -0.022(3) 0.003(2) -0.022(2) C18 0.096(4) 0.062(4) 0.043(3) -0.018(3) 0.005(3) -0.045(3) C19 0.108(5) 0.076(4) 0.066(4) -0.032(3) 0.010(3) -0.059(4) C20 0.101(5) 0.075(4) 0.073(4) -0.017(4) 0.005(4) -0.057(4) C21 0.112(5) 0.084(4) 0.050(3) -0.010(3) 0.004(3) -0.064(4) C22 0.079(4) 0.058(4) 0.036(3) -0.007(3) -0.005(3) -0.043(3) C23 0.049(3) 0.054(3) 0.039(3) -0.017(2) 0.005(2) -0.033(3) C24 0.043(3) 0.055(3) 0.031(3) -0.017(2) 0.010(2) -0.027(2) C25 0.062(3) 0.046(3) 0.036(3) -0.019(2) 0.007(2) -0.027(3) C26 0.045(3) 0.052(3) 0.033(3) -0.017(2) 0.006(2) -0.022(3) C27 0.071(4) 0.055(3) 0.036(3) -0.014(2) 0.008(2) -0.024(3) C28 0.058(3) 0.053(3) 0.052(3) -0.026(3) 0.020(3) -0.034(3) C35 0.058(3) 0.051(3) 0.046(3) -0.023(3) 0.010(2) -0.031(3) C36 0.068(3) 0.060(3) 0.029(3) -0.020(3) 0.006(2) -0.034(3) C37 0.089(4) 0.087(4) 0.037(3) -0.027(3) 0.023(3) -0.070(3) C38 0.077(4) 0.078(4) 0.045(3) -0.033(3) 0.018(3) -0.057(3) C39 0.099(4) 0.072(4) 0.049(3) -0.031(3) 0.030(3) -0.060(4) C40 0.097(5) 0.078(4) 0.066(4) -0.029(3) 0.035(3) -0.060(4) C41 0.084(4) 0.071(4) 0.080(4) -0.040(4) 0.032(3) -0.051(3) C42 0.096(5) 0.074(4) 0.078(4) -0.047(4) 0.024(3) -0.048(4) C43 0.086(4) 0.057(3) 0.056(3) -0.034(3) 0.026(3) -0.044(3) C44 0.037(3) 0.051(3) 0.048(3) -0.025(3) 0.010(2) -0.024(2) C45 0.040(3) 0.049(3) 0.038(3) -0.021(2) 0.007(2) -0.026(2) C46 0.056(3) 0.050(3) 0.035(3) -0.018(2) 0.008(2) -0.026(3) C47 0.036(3) 0.054(3) 0.037(3) -0.025(2) 0.005(2) -0.022(2) C48 0.055(3) 0.052(3) 0.041(3) -0.024(2) 0.009(2) -0.019(3) C49 0.040(3) 0.048(3) 0.040(3) -0.021(3) 0.002(2) -0.020(2) C50 0.054(3) 0.042(3) 0.039(3) -0.014(2) -0.004(2) -0.022(3) C51 0.082(4) 0.058(4) 0.059(3) -0.027(3) 0.007(3) -0.034(3) C52 0.122(6) 0.056(4) 0.085(5) -0.039(4) -0.003(4) -0.034(4) C53 0.131(6) 0.064(4) 0.080(5) -0.016(4) -0.006(4) -0.059(4) C54 0.120(5) 0.067(4) 0.064(4) -0.012(3) 0.013(4) -0.055(4) C55 0.075(4) 0.055(4) 0.062(3) -0.020(3) 0.007(3) -0.036(3) C56 0.087(4) 0.044(3) 0.046(3) -0.012(3) -0.003(3) -0.039(3) C57 0.101(5) 0.065(4) 0.073(4) -0.026(3) 0.000(3) -0.052(4) C58 0.088(4) 0.054(4) 0.084(4) -0.013(3) 0.007(3) -0.046(3) C59 0.086(4) 0.055(4) 0.055(3) -0.012(3) 0.000(3) -0.032(3) C60 0.076(4) 0.041(3) 0.040(3) -0.013(2) 0.000(3) -0.029(3) C61 0.040(3) 0.045(3) 0.038(3) -0.011(2) 0.005(2) -0.022(2) C62 0.042(3) 0.045(3) 0.034(3) -0.014(2) 0.008(2) -0.024(2) C63 0.062(3) 0.045(3) 0.037(3) -0.021(2) 0.007(2) -0.030(3) C64 0.059(3) 0.054(3) 0.025(2) -0.015(2) 0.010(2) -0.033(3) C65 0.135(5) 0.070(4) 0.036(3) -0.014(3) 0.003(3) -0.065(4) C66 0.058(3) 0.038(3) 0.043(3) -0.007(2) 0.005(2) -0.022(3) C73 0.081(4) 0.052(3) 0.030(3) -0.015(2) 0.015(2) -0.043(3) C74 0.067(3) 0.049(3) 0.031(3) -0.019(2) 0.011(2) -0.036(3) C75 0.088(4) 0.077(4) 0.044(3) -0.033(3) 0.028(3) -0.065(3) C76 0.087(4) 0.078(4) 0.037(3) -0.028(3) 0.021(3) -0.060(3) ##################################################################### # MOLECULAR GEOMETRY # ##################################################################### 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 1.875(3) . ? Cu1 N1 1.905(3) . ? Cu1 O2 1.933(3) . ? Cu1 N9 2.008(3) . ? Cu2 O3 1.881(3) . ? Cu2 N3 1.894(3) . ? Cu2 O4 1.941(3) . ? Cu2 N10 2.009(3) . ? Cu3 O5 1.877(3) . ? Cu3 N5 1.907(3) . ? Cu3 O6 1.942(3) . ? Cu3 N11 2.012(3) . ? Cu4 O7 1.864(3) . ? Cu4 N7 1.904(3) . ? Cu4 O8 1.930(3) . ? Cu4 N12 1.997(3) . ? Cl1 O9 1.375(4) . ? Cl1 O10 1.401(4) . ? Cl1 O12A 1.403(10) . ? Cl1 O11 1.410(3) . ? Cl1 O12B 1.480(16) . ? Cl2 O15B 1.374(15) . ? Cl2 O14 1.379(4) . ? Cl2 O16 1.398(4) . ? Cl2 O13 1.406(4) . ? Cl2 O15A 1.481(11) . ? Cl3 O17B 1.396(15) . ? Cl3 O19 1.397(4) . ? Cl3 O18B 1.400(11) . ? Cl3 O20 1.400(4) . ? Cl3 O17A 1.407(10) . ? Cl3 O18A 1.449(7) . ? Cl4 O22 1.384(4) . ? Cl4 O23 1.392(4) . ? Cl4 O21 1.408(4) . ? Cl4 O24B 1.417(15) . ? Cl4 O24A 1.422(10) . ? O1 C7 1.287(4) . ? O2 C11 1.269(4) . ? O3 C24 1.295(4) . ? O4 C28 1.245(5) . ? O5 C45 1.282(4) . ? O6 C49 1.271(4) . ? O7 C62 1.312(4) . ? O8 C66 1.258(5) . ? N1 C9 1.294(5) . ? N1 N2 1.388(4) . ? N2 C11 1.331(5) . ? N2 H2N 0.8600 . ? N3 C26 1.312(5) . ? N3 N4 1.379(4) . ? N4 C28 1.334(5) . ? N4 H4N 0.8600 . ? N5 C47 1.298(5) . ? N5 N6 1.386(4) . ? N6 C49 1.314(5) . ? N6 H6N 0.8600 . ? N7 C64 1.313(5) . ? N7 N8 1.383(4) . ? N8 C66 1.336(5) . ? N8 H8N 0.8600 . ? N9 C38 1.325(5) . ? N9 C35 1.351(5) . ? N10 C36 1.313(5) . ? N10 C37 1.318(5) . ? N11 C76 1.310(5) . ? N11 C73 1.327(5) . ? N12 C74 1.329(5) . ? N12 C75 1.336(5) . ? C1 C2 1.372(6) . ? C1 C6 1.377(5) . ? C1 H1 0.9300 . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.360(6) . ? C3 H3 0.9300 . ? C4 C5 1.369(6) . ? C4 H4 0.9300 . ? C5 C6 1.393(5) . ? C5 H5 0.9300 . ? C6 C7 1.501(6) . ? C7 C8 1.385(5) . ? C8 C9 1.403(5) . ? C8 H8 0.9300 . ? C9 C10 1.509(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12B 1.457(9) . ? C11 C12A 1.459(6) . ? C12A C13A 1.3900 . ? C12A C17A 1.3900 . ? C13A C14A 1.3900 . ? C13A H13A 0.9300 . ? C14A C15A 1.3900 . ? C14A H14A 0.9300 . ? C15A C16A 1.3900 . ? C15A H15A 0.9300 . ? C16A C17A 1.3900 . ? C16A H16A 0.9300 . ? C17A H17A 0.9300 . ? C12B C13B 1.3900 . ? C12B C17B 1.3900 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? C16B C17B 1.3900 . ? C16B H16B 0.9300 . ? C17B H17B 0.9300 . ? C18 C19 1.365(6) . ? C18 C23 1.396(5) . ? C18 H18 0.9300 . ? C19 C20 1.356(6) . ? C19 H19 0.9300 . ? C20 C21 1.373(6) . ? C20 H20 0.9300 . ? C21 C22 1.368(6) . ? C21 H21 0.9300 . ? C22 C23 1.370(5) . ? C22 H22 0.9300 . ? C23 C24 1.490(6) . ? C24 C25 1.377(5) . ? C25 C26 1.395(5) . ? C25 H25 0.9300 . ? C26 C27 1.486(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29B 1.423(8) . ? C28 C29A 1.490(7) . ? C29A C30A 1.3900 . ? C29A C34A 1.3900 . ? C30A C31A 1.3900 . ? C30A H30A 0.9300 . ? C31A C32A 1.3900 . ? C31A H31A 0.9300 . ? C32A C33A 1.3900 . ? C32A H32A 0.9300 . ? C33A C34A 1.3900 . ? C33A H33A 0.9300 . ? C34A H34A 0.9300 . ? C29B C30B 1.3900 . ? C29B C34B 1.3900 . ? C30B C31B 1.3900 . ? C30B H30B 0.9300 . ? C31B C32B 1.3900 . ? C31B H31B 0.9300 . ? C32B C33B 1.3900 . ? C32B H32B 0.9300 . ? C33B C34B 1.3900 . ? C33B H33B 0.9300 . ? C34B H34B 0.9300 . ? C35 C36 1.363(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.373(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.376(6) . ? C39 C40 1.379(6) . ? C39 H39 0.9300 . ? C40 C41 1.371(6) . ? C40 H40 0.9300 . ? C41 C42 1.351(6) . ? C41 H41 0.9300 . ? C42 C43 1.379(6) . ? C42 H42 0.9300 . ? C43 C44 1.382(5) . ? C43 H43 0.9300 . ? C44 C45 1.505(6) . ? C45 C46 1.385(5) . ? C46 C47 1.412(5) . ? C46 H46 0.9300 . ? C47 C48 1.481(5) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.456(6) . ? C50 C55 1.385(6) . ? C50 C51 1.396(6) . ? C51 C52 1.391(6) . ? C51 H51 0.9300 . ? C52 C53 1.350(7) . ? C52 H52 0.9300 . ? C53 C54 1.362(7) . ? C53 H53 0.9300 . ? C54 C55 1.372(6) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.369(6) . ? C56 C61 1.376(5) . ? C56 H56 0.9300 . ? C57 C58 1.378(6) . ? C57 H57 0.9300 . ? C58 C59 1.380(6) . ? C58 H58 0.9300 . ? C59 C60 1.364(6) . ? C59 H59 0.9300 . ? C60 C61 1.375(5) . ? C60 H60 0.9300 . ? C61 C62 1.478(5) . ? C62 C63 1.362(5) . ? C63 C64 1.403(5) . ? C63 H63 0.9300 . ? C64 C65 1.498(5) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C67B 1.432(9) . ? C66 C67A 1.452(7) . ? C67A C68A 1.3900 . ? C67A C72A 1.3900 . ? C68A C69A 1.3900 . ? C68A H68A 0.9300 . ? C69A C70A 1.3900 . ? C69A H69A 0.9300 . ? C70A C71A 1.3900 . ? C70A H70A 0.9300 . ? C71A C72A 1.3900 . ? C71A H71A 0.9300 . ? C72A H72A 0.9300 . ? C67B C68B 1.3900 . ? C67B C72B 1.3900 . ? C68B C69B 1.3900 . ? C68B H68B 0.9300 . ? C69B C70B 1.3900 . ? C69B H69B 0.9300 . ? C70B C71B 1.3900 . ? C70B H70B 0.9300 . ? C71B C72B 1.3900 . ? C71B H71B 0.9300 . ? C72B H72B 0.9300 . ? C73 C74 1.370(5) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C76 1.374(5) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? 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 N1 94.07(14) . . ? O1 Cu1 O2 175.87(12) . . ? N1 Cu1 O2 82.19(13) . . ? O1 Cu1 N9 92.04(13) . . ? N1 Cu1 N9 173.82(16) . . ? O2 Cu1 N9 91.67(13) . . ? O3 Cu2 N3 93.95(14) . . ? O3 Cu2 O4 175.01(12) . . ? N3 Cu2 O4 81.67(14) . . ? O3 Cu2 N10 92.49(13) . . ? N3 Cu2 N10 173.53(16) . . ? O4 Cu2 N10 91.87(14) . . ? O5 Cu3 N5 93.80(14) . . ? O5 Cu3 O6 174.57(12) . . ? N5 Cu3 O6 82.03(13) . . ? O5 Cu3 N11 92.90(13) . . ? N5 Cu3 N11 173.27(16) . . ? O6 Cu3 N11 91.24(13) . . ? O7 Cu4 N7 94.45(13) . . ? O7 Cu4 O8 175.64(12) . . ? N7 Cu4 O8 81.71(13) . . ? O7 Cu4 N12 91.68(13) . . ? N7 Cu4 N12 173.70(15) . . ? O8 Cu4 N12 92.11(13) . . ? O9 Cl1 O10 107.8(3) . . ? O9 Cl1 O12A 122.9(9) . . ? O10 Cl1 O12A 102.8(8) . . ? O9 Cl1 O11 108.5(3) . . ? O10 Cl1 O11 110.5(3) . . ? O12A Cl1 O11 103.9(7) . . ? O9 Cl1 O12B 90.4(14) . . ? O10 Cl1 O12B 120.2(10) . . ? O11 Cl1 O12B 116.6(9) . . ? O15B Cl2 O14 133.9(13) . . ? O15B Cl2 O16 95.3(13) . . ? O14 Cl2 O16 107.9(3) . . ? O15B Cl2 O13 98.1(10) . . ? O14 Cl2 O13 109.2(3) . . ? O16 Cl2 O13 110.9(3) . . ? O14 Cl2 O15A 99.8(9) . . ? O16 Cl2 O15A 114.4(6) . . ? O13 Cl2 O15A 113.8(7) . . ? O17B Cl3 O19 102.2(11) . . ? O17B Cl3 O18B 111.3(8) . . ? O19 Cl3 O18B 102.3(13) . . ? O17B Cl3 O20 92.4(10) . . ? O19 Cl3 O20 109.2(3) . . ? O18B Cl3 O20 135.3(17) . . ? O19 Cl3 O17A 113.3(8) . . ? O18B Cl3 O17A 81.7(7) . . ? O20 Cl3 O17A 112.3(8) . . ? O17B Cl3 O18A 136.9(9) . . ? O19 Cl3 O18A 114.6(5) . . ? O20 Cl3 O18A 95.7(9) . . ? O17A Cl3 O18A 110.5(7) . . ? O22 Cl4 O23 111.6(3) . . ? O22 Cl4 O21 108.0(3) . . ? O23 Cl4 O21 109.3(3) . . ? O22 Cl4 O24B 93.6(12) . . ? O23 Cl4 O24B 115.7(12) . . ? O21 Cl4 O24B 117.3(11) . . ? O22 Cl4 O24A 122.4(9) . . ? O23 Cl4 O24A 105.8(8) . . ? O21 Cl4 O24A 98.6(8) . . ? C7 O1 Cu1 125.3(3) . . ? C11 O2 Cu1 113.4(3) . . ? C24 O3 Cu2 125.3(3) . . ? C28 O4 Cu2 113.5(3) . . ? C45 O5 Cu3 125.1(3) . . ? C49 O6 Cu3 113.0(3) . . ? C62 O7 Cu4 125.4(3) . . ? C66 O8 Cu4 114.1(3) . . ? C9 N1 N2 120.2(3) . . ? C9 N1 Cu1 128.4(3) . . ? N2 N1 Cu1 111.1(2) . . ? C11 N2 N1 115.2(3) . . ? C11 N2 H2N 122.4 . . ? N1 N2 H2N 122.4 . . ? C26 N3 N4 119.8(4) . . ? C26 N3 Cu2 128.6(3) . . ? N4 N3 Cu2 111.5(3) . . ? C28 N4 N3 114.8(4) . . ? C28 N4 H4N 122.6 . . ? N3 N4 H4N 122.6 . . ? C47 N5 N6 120.0(3) . . ? C47 N5 Cu3 129.3(3) . . ? N6 N5 Cu3 110.6(3) . . ? C49 N6 N5 116.1(3) . . ? C49 N6 H6N 121.9 . . ? N5 N6 H6N 121.9 . . ? C64 N7 N8 120.3(3) . . ? C64 N7 Cu4 127.9(3) . . ? N8 N7 Cu4 111.6(2) . . ? C66 N8 N7 114.7(3) . . ? C66 N8 H8N 122.6 . . ? N7 N8 H8N 122.6 . . ? C38 N9 C35 116.9(4) . . ? C38 N9 Cu1 120.7(3) . . ? C35 N9 Cu1 122.4(3) . . ? C36 N10 C37 116.0(4) . . ? C36 N10 Cu2 122.3(3) . . ? C37 N10 Cu2 121.2(3) . . ? C76 N11 C73 116.0(4) . . ? C76 N11 Cu3 121.1(3) . . ? C73 N11 Cu3 121.9(3) . . ? C74 N12 C75 116.8(4) . . ? C74 N12 Cu4 123.1(3) . . ? C75 N12 Cu4 120.1(3) . . ? C2 C1 C6 120.3(4) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? C1 C2 C3 121.0(5) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 118.9(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.9(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 118.4(4) . . ? C1 C6 C7 122.5(4) . . ? C5 C6 C7 119.1(4) . . ? O1 C7 C8 125.0(4) . . ? O1 C7 C6 115.0(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 127.0(4) . . ? C7 C8 H8 116.5 . . ? C9 C8 H8 116.5 . . ? N1 C9 C8 119.8(4) . . ? N1 C9 C10 122.3(4) . . ? C8 C9 C10 117.9(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 N2 118.1(4) . . ? O2 C11 C12B 119.1(6) . . ? N2 C11 C12B 122.7(5) . . ? O2 C11 C12A 120.7(4) . . ? N2 C11 C12A 121.1(4) . . ? C13A C12A C17A 120.0 . . ? C13A C12A C11 118.8(4) . . ? C17A C12A C11 121.1(4) . . ? C12A C13A C14A 120.0 . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C15A C14A C13A 120.0 . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C17A C12A 120.0 . . ? C16A C17A H17A 120.0 . . ? C12A C17A H17A 120.0 . . ? C13B C12B C17B 120.0 . . ? C17B C12B C11 122.8(7) . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C15B C16B C17B 120.0 . . ? C15B C16B H16B 120.0 . . ? C17B C16B H16B 120.0 . . ? C16B C17B C12B 120.0 . . ? C16B C17B H17B 120.0 . . ? C12B C17B H17B 120.0 . . ? C19 C18 C23 121.2(5) . . ? C19 C18 H18 119.4 . . ? C23 C18 H18 119.4 . . ? C20 C19 C18 120.6(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.2(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.5(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 121.4(5) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 117.1(4) . . ? C22 C23 C24 120.3(4) . . ? C18 C23 C24 122.6(4) . . ? O3 C24 C25 124.3(4) . . ? O3 C24 C23 114.8(4) . . ? C25 C24 C23 120.8(4) . . ? C24 C25 C26 128.0(4) . . ? C24 C25 H25 116.0 . . ? C26 C25 H25 116.0 . . ? N3 C26 C25 119.4(4) . . ? N3 C26 C27 121.0(4) . . ? C25 C26 C27 119.6(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 N4 118.3(4) . . ? O4 C28 C29B 116.8(6) . . ? N4 C28 C29B 123.8(6) . . ? O4 C28 C29A 123.6(5) . . ? N4 C28 C29A 117.8(5) . . ? C30A C29A C34A 120.0 . . ? C30A C29A C28 124.2(5) . . ? C34A C29A C28 115.7(5) . . ? C29A C30A C31A 120.0 . . ? C29A C30A H30A 120.0 . . ? C31A C30A H30A 120.0 . . ? C32A C31A C30A 120.0 . . ? C32A C31A H31A 120.0 . . ? C30A C31A H31A 120.0 . . ? C31A C32A C33A 120.0 . . ? C31A C32A H32A 120.0 . . ? C33A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33A C34A C29A 120.0 . . ? C33A C34A H34A 120.0 . . ? C29A C34A H34A 120.0 . . ? C30B C29B C34B 120.0 . . ? C30B C29B C28 121.0(7) . . ? C34B C29B C28 118.7(7) . . ? C31B C30B C29B 120.0 . . ? C31B C30B H30B 120.0 . . ? C29B C30B H30B 120.0 . . ? C30B C31B C32B 120.0 . . ? C30B C31B H31B 120.0 . . ? C32B C31B H31B 120.0 . . ? C33B C32B C31B 120.0 . . ? C33B C32B H32B 120.0 . . ? C31B C32B H32B 120.0 . . ? C32B C33B C34B 120.0 . . ? C32B C33B H33B 120.0 . . ? C34B C33B H33B 120.0 . . ? C33B C34B C29B 120.0 . . ? C33B C34B H34B 120.0 . . ? C29B C34B H34B 120.0 . . ? N9 C35 C36 119.5(4) . . ? N9 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? N10 C36 C35 124.0(4) . . ? N10 C36 H36 118.0 . . ? C35 C36 H36 118.0 . . ? N10 C37 C38 122.1(4) . . ? N10 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? N9 C38 C37 121.5(4) . . ? N9 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C44 C39 C40 121.9(5) . . ? C44 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C41 C40 C39 120.0(5) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 118.3(5) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C41 C42 C43 122.4(5) . . ? C41 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C42 C43 C44 120.0(5) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C39 C44 C43 117.3(4) . . ? C39 C44 C45 123.8(4) . . ? C43 C44 C45 118.8(4) . . ? O5 C45 C46 125.4(4) . . ? O5 C45 C44 115.3(4) . . ? C46 C45 C44 119.3(4) . . ? C45 C46 C47 127.2(4) . . ? C45 C46 H46 116.4 . . ? C47 C46 H46 116.4 . . ? N5 C47 C46 118.8(4) . . ? N5 C47 C48 122.1(4) . . ? C46 C47 C48 119.1(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O6 C49 N6 118.1(4) . . ? O6 C49 C50 119.5(4) . . ? N6 C49 C50 122.4(4) . . ? C55 C50 C51 119.2(4) . . ? C55 C50 C49 118.9(4) . . ? C51 C50 C49 121.9(4) . . ? C52 C51 C50 118.2(5) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? C53 C52 C51 121.8(6) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 120.0(6) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 120.3(5) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C50 120.5(5) . . ? C54 C55 H55 119.7 . . ? C50 C55 H55 119.7 . . ? C57 C56 C61 121.8(5) . . ? C57 C56 H56 119.1 . . ? C61 C56 H56 119.1 . . ? C56 C57 C58 120.1(5) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C57 C58 C59 118.7(5) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? C60 C59 C58 120.1(5) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 122.0(4) . . ? C59 C60 H60 119.0 . . ? C61 C60 H60 119.0 . . ? C60 C61 C56 117.2(4) . . ? C60 C61 C62 120.4(4) . . ? C56 C61 C62 122.4(4) . . ? O7 C62 C63 124.4(4) . . ? O7 C62 C61 114.3(4) . . ? C63 C62 C61 121.3(4) . . ? C62 C63 C64 128.3(4) . . ? C62 C63 H63 115.8 . . ? C64 C63 H63 115.8 . . ? N7 C64 C63 119.3(4) . . ? N7 C64 C65 121.3(4) . . ? C63 C64 C65 119.4(4) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O8 C66 N8 117.9(4) . . ? O8 C66 C67B 122.5(6) . . ? N8 C66 C67B 119.3(6) . . ? O8 C66 C67A 119.4(5) . . ? N8 C66 C67A 122.7(5) . . ? C68A C67A C72A 120.0 . . ? C68A C67A C66 122.7(5) . . ? C72A C67A C66 117.3(5) . . ? C69A C68A C67A 120.0 . . ? C69A C68A H68A 120.0 . . ? C67A C68A H68A 120.0 . . ? C68A C69A C70A 120.0 . . ? C68A C69A H69A 120.0 . . ? C70A C69A H69A 120.0 . . ? C69A C70A C71A 120.0 . . ? C69A C70A H70A 120.0 . . ? C71A C70A H70A 120.0 . . ? C72A C71A C70A 120.0 . . ? C72A C71A H71A 120.0 . . ? C70A C71A H71A 120.0 . . ? C71A C72A C67A 120.0 . . ? C71A C72A H72A 120.0 . . ? C67A C72A H72A 120.0 . . ? C68B C67B C72B 120.0 . . ? C68B C67B C66 120.2(8) . . ? C72B C67B C66 119.8(8) . . ? C67B C68B C69B 120.0 . . ? C67B C68B H68B 120.0 . . ? C69B C68B H68B 120.0 . . ? C70B C69B C68B 120.0 . . ? C70B C69B H69B 120.0 . . ? C68B C69B H69B 120.0 . . ? C69B C70B C71B 120.0 . . ? C69B C70B H70B 120.0 . . ? C71B C70B H70B 120.0 . . ? C72B C71B C70B 120.0 . . ? C72B C71B H71B 120.0 . . ? C70B C71B H71B 120.0 . . ? C71B C72B C67B 120.0 . . ? C71B C72B H72B 120.0 . . ? C67B C72B H72B 120.0 . . ? N11 C73 C74 122.5(4) . . ? N11 C73 H73 118.8 . . ? C74 C73 H73 118.8 . . ? N12 C74 C73 121.1(4) . . ? N12 C74 H74 119.5 . . ? C73 C74 H74 119.5 . . ? N12 C75 C76 120.7(4) . . ? N12 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? N11 C76 C75 122.9(4) . . ? N11 C76 H76 118.5 . . ? C75 C76 H76 118.5 . . ? #===END ##################################################################### # AUTHOR DATA # ##################################################################### _audit_creation_date 26/06/2007 _audit_creation_method 'ModiCIF v2.00' _audit_update_record ? _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori G. & Spagna, R. (1999) J. Appl. Cryst., 32, 115-119. Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _publ_section_exptl_refinement ; All H atoms were positioned geometrically and treated as riding, with C---H = 0.93-0.97 \%A and with U~iso~(H) = 1.2 U~eq~(C) or 1.5 U~eq~(C) for methyl groups. ; #===END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 651330' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_melting_point ? _chemical_formula_structural "[{Cu(PhCO=NN=CHPy)(OClO3)}2(4,4'-bipy)]" _chemical_formula_moiety 'C36 H28 Cl2 Cu2 N8 O10' _chemical_formula_sum 'C36 H28 Cl2 Cu2 N8 O10' _chemical_formula_weight 930.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n 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 12.3678(12) _cell_length_b 12.8964(11) _cell_length_c 12.9157(12) _cell_angle_alpha 90.00 _cell_angle_beta 115.200(9) _cell_angle_gamma 90.00 _cell_volume 1864.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square plate' _exptl_crystal_colour brown-grey _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.998 _exptl_absorpt_correction_T_max 1.002 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 14513 _diffrn_reflns_av_R_equivalents 0.1151 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2418 _reflns_number_gt 1750 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0355P)^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 2418 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Cu Cu 0.67578(7) 0.41252(6) 0.56235(6) 0.0285(3) Uani 1 1 d . . . O1 O 0.5562(4) 0.3400(3) 0.5996(3) 0.0304(11) Uani 1 1 d . . . C1 C 0.4635(5) 0.3194(5) 0.5075(5) 0.0281(16) Uani 1 1 d . . . C11 C 0.3659(5) 0.2575(5) 0.5154(5) 0.0270(16) Uani 1 1 d . . . C12 C 0.3800(6) 0.2186(5) 0.6205(6) 0.0385(18) Uani 1 1 d . . . H12 H 0.4495 0.2326 0.6858 0.046 Uiso 1 1 calc R . . C13 C 0.2908(7) 0.1589(5) 0.6284(7) 0.050(2) Uani 1 1 d . . . H13 H 0.3000 0.1332 0.6990 0.060 Uiso 1 1 calc R . . C14 C 0.1886(7) 0.1379(5) 0.5315(8) 0.051(2) Uani 1 1 d . . . H14 H 0.1288 0.0975 0.5367 0.061 Uiso 1 1 calc R . . C15 C 0.1742(6) 0.1759(5) 0.4276(7) 0.045(2) Uani 1 1 d . . . H15 H 0.1047 0.1614 0.3625 0.054 Uiso 1 1 calc R . . C16 C 0.2621(6) 0.2353(5) 0.4193(6) 0.0374(18) Uani 1 1 d . . . H16 H 0.2519 0.2608 0.3484 0.045 Uiso 1 1 calc R . . N2 N 0.4469(4) 0.3495(4) 0.4031(4) 0.0303(14) Uani 1 1 d . . . N3 N 0.5461(4) 0.4017(4) 0.4136(4) 0.0253(12) Uani 1 1 d . . . C4 C 0.5620(5) 0.4393(5) 0.3308(5) 0.0288(17) Uani 1 1 d . . . H4 H 0.5055 0.4315 0.2555 0.035 Uiso 1 1 calc R . . C41 C 0.6720(6) 0.4949(5) 0.3586(5) 0.0285(16) Uani 1 1 d . . . N42 N 0.7451(4) 0.4950(4) 0.4724(4) 0.0277(13) Uani 1 1 d . . . C43 C 0.8472(6) 0.5458(5) 0.5086(6) 0.0367(18) Uani 1 1 d . . . H43 H 0.8975 0.5453 0.5864 0.044 Uiso 1 1 calc R . . C44 C 0.8830(6) 0.5997(5) 0.4361(6) 0.0416(18) Uani 1 1 d . . . H44 H 0.9551 0.6355 0.4643 0.050 Uiso 1 1 calc R . . C45 C 0.8094(6) 0.5988(5) 0.3220(6) 0.0431(18) Uani 1 1 d . . . H45 H 0.8315 0.6336 0.2709 0.052 Uiso 1 1 calc R . . C46 C 0.7027(6) 0.5466(5) 0.2824(6) 0.0375(18) Uani 1 1 d . . . H46 H 0.6518 0.5463 0.2048 0.045 Uiso 1 1 calc R . . N51 N 0.7964(4) 0.4397(4) 0.7183(4) 0.0253(13) Uani 1 1 d . . . C52 C 0.7754(6) 0.5160(5) 0.7766(5) 0.044(2) Uani 1 1 d . . . H52 H 0.7050 0.5539 0.7416 0.053 Uiso 1 1 calc R . . C53 C 0.8532(6) 0.5407(6) 0.8860(5) 0.046(2) Uani 1 1 d . . . H53 H 0.8347 0.5941 0.9241 0.056 Uiso 1 1 calc R . . C54 C 0.9583(5) 0.4875(5) 0.9399(5) 0.0202(14) Uani 1 1 d . . . C55 C 0.9812(5) 0.4113(5) 0.8780(5) 0.0344(17) Uani 1 1 d . . . H55 H 1.0524 0.3742 0.9097 0.041 Uiso 1 1 calc R . . C56 C 0.8986(6) 0.3901(5) 0.7691(5) 0.0386(19) Uani 1 1 d . . . H56 H 0.9157 0.3378 0.7287 0.046 Uiso 1 1 calc R . . Cl6 Cl 0.84209(15) 0.21341(13) 0.50481(14) 0.0317(4) Uani 1 1 d . . . O61 O 0.7520(4) 0.2507(3) 0.5395(3) 0.0356(11) Uani 1 1 d . . . O62 O 0.8442(4) 0.2766(4) 0.4164(3) 0.0514(14) Uani 1 1 d . . . O63 O 0.8156(5) 0.1103(4) 0.4686(5) 0.0729(17) Uani 1 1 d . . . O64 O 0.9543(4) 0.2200(4) 0.6014(4) 0.0530(14) 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 Cu 0.0259(4) 0.0353(5) 0.0204(4) -0.0015(4) 0.0060(3) -0.0043(5) O1 0.029(3) 0.038(3) 0.021(2) 0.001(2) 0.008(2) -0.002(2) C1 0.022(4) 0.035(4) 0.028(4) -0.002(3) 0.011(3) 0.003(3) C11 0.028(4) 0.028(4) 0.034(4) -0.005(3) 0.021(3) -0.001(3) C12 0.045(5) 0.037(4) 0.038(4) -0.006(4) 0.021(4) -0.002(4) C13 0.067(6) 0.040(5) 0.063(6) 0.002(4) 0.047(5) -0.007(4) C14 0.042(5) 0.033(5) 0.090(7) -0.003(5) 0.040(5) -0.014(4) C15 0.034(4) 0.035(5) 0.058(5) -0.006(4) 0.013(4) 0.000(4) C16 0.036(4) 0.027(4) 0.051(5) -0.008(4) 0.021(4) -0.012(4) N2 0.026(3) 0.041(4) 0.023(3) 0.000(3) 0.009(2) -0.004(3) N3 0.025(3) 0.029(3) 0.024(3) 0.004(3) 0.013(2) -0.002(3) C4 0.033(4) 0.026(4) 0.022(4) -0.002(3) 0.007(3) -0.001(3) C41 0.034(4) 0.025(4) 0.029(4) 0.000(3) 0.015(3) 0.003(3) N42 0.032(3) 0.026(3) 0.025(3) -0.006(3) 0.012(3) -0.004(3) C43 0.032(4) 0.040(4) 0.035(4) -0.007(4) 0.011(3) -0.001(4) C44 0.038(4) 0.022(4) 0.068(5) 0.003(4) 0.026(4) -0.009(4) C45 0.053(5) 0.034(5) 0.055(5) 0.008(4) 0.035(4) 0.000(4) C46 0.051(5) 0.035(4) 0.029(4) 0.007(3) 0.019(4) 0.004(4) N51 0.017(3) 0.030(4) 0.024(3) -0.002(3) 0.005(2) -0.002(3) C52 0.032(4) 0.052(5) 0.035(4) -0.008(4) 0.002(4) 0.023(4) C53 0.042(5) 0.053(5) 0.029(4) -0.024(4) 0.000(4) 0.015(4) C54 0.016(3) 0.021(4) 0.020(3) -0.001(3) 0.005(3) 0.001(3) C55 0.024(4) 0.043(4) 0.031(4) -0.012(4) 0.006(3) 0.012(4) C56 0.033(4) 0.050(5) 0.031(4) -0.018(4) 0.012(3) 0.003(4) Cl6 0.0388(11) 0.0284(10) 0.0323(10) -0.0025(9) 0.0193(8) -0.0059(9) O61 0.035(3) 0.032(3) 0.048(3) -0.004(2) 0.026(2) 0.001(2) O62 0.068(4) 0.054(3) 0.035(3) 0.011(3) 0.025(3) -0.006(3) O63 0.127(5) 0.031(3) 0.107(4) -0.028(3) 0.094(4) -0.023(3) O64 0.033(3) 0.085(4) 0.040(3) 0.014(3) 0.015(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N3 1.912(5) . ? Cu N51 1.961(4) . ? Cu O1 1.975(4) . ? Cu N42 2.016(5) . ? Cu O61 2.360(4) . ? O1 C1 1.281(6) . ? C1 N2 1.332(7) . ? C1 C11 1.487(8) . ? C11 C16 1.383(8) . ? C11 C12 1.387(8) . ? C12 C13 1.384(9) . ? C12 H12 0.9300 . ? C13 C14 1.375(10) . ? C13 H13 0.9300 . ? C14 C15 1.368(9) . ? C14 H14 0.9300 . ? C15 C16 1.372(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N2 N3 1.355(6) . ? N3 C4 1.264(7) . ? C4 C41 1.441(8) . ? C4 H4 0.9300 . ? C41 N42 1.359(7) . ? C41 C46 1.369(8) . ? N42 C43 1.320(7) . ? C43 C44 1.381(9) . ? C43 H43 0.9300 . ? C44 C45 1.363(8) . ? C44 H44 0.9300 . ? C45 C46 1.371(9) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? N51 C56 1.315(7) . ? N51 C52 1.331(7) . ? C52 C53 1.366(8) . ? C52 H52 0.9300 . ? C53 C54 1.370(8) . ? C53 H53 0.9300 . ? C54 C55 1.370(8) . ? C54 C54 1.488(10) 3_767 ? C55 C56 1.368(8) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? Cl6 O63 1.401(5) . ? Cl6 O62 1.412(4) . ? Cl6 O64 1.420(4) . ? Cl6 O61 1.448(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 N3 Cu N51 172.0(2) . . ? N3 Cu O1 79.39(19) . . ? N51 Cu O1 98.95(18) . . ? N3 Cu N42 80.8(2) . . ? N51 Cu N42 100.0(2) . . ? O1 Cu N42 159.52(18) . . ? N3 Cu O61 91.07(18) . . ? N51 Cu O61 96.71(18) . . ? O1 Cu O61 89.55(16) . . ? N42 Cu O61 95.96(17) . . ? C1 O1 Cu 109.8(4) . . ? O1 C1 N2 124.9(6) . . ? O1 C1 C11 118.6(6) . . ? N2 C1 C11 116.5(5) . . ? C16 C11 C12 119.1(6) . . ? C16 C11 C1 121.3(6) . . ? C12 C11 C1 119.6(6) . . ? C13 C12 C11 120.1(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 119.7(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.5(7) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.1(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.6(7) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C1 N2 N3 107.5(5) . . ? C4 N3 N2 124.5(5) . . ? C4 N3 Cu 117.1(4) . . ? N2 N3 Cu 118.2(4) . . ? N3 C4 C41 116.8(5) . . ? N3 C4 H4 121.6 . . ? C41 C4 H4 121.6 . . ? N42 C41 C46 121.1(6) . . ? N42 C41 C4 113.1(6) . . ? C46 C41 C4 125.7(6) . . ? C43 N42 C41 118.6(6) . . ? C43 N42 Cu 129.5(4) . . ? C41 N42 Cu 111.9(4) . . ? N42 C43 C44 123.0(6) . . ? N42 C43 H43 118.5 . . ? C44 C43 H43 118.5 . . ? C45 C44 C43 118.0(7) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 C46 120.1(7) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 119.2(6) . . ? C41 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C56 N51 C52 117.1(5) . . ? C56 N51 Cu 125.1(4) . . ? C52 N51 Cu 117.8(4) . . ? N51 C52 C53 122.4(6) . . ? N51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C52 C53 C54 120.5(6) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C55 116.7(5) . . ? C53 C54 C54 120.5(7) . 3_767 ? C55 C54 C54 122.7(7) . 3_767 ? C56 C55 C54 119.6(6) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? N51 C56 C55 123.6(6) . . ? N51 C56 H56 118.2 . . ? C55 C56 H56 118.2 . . ? O63 Cl6 O62 111.1(3) . . ? O63 Cl6 O64 110.6(3) . . ? O62 Cl6 O64 109.1(3) . . ? O63 Cl6 O61 108.5(3) . . ? O62 Cl6 O61 109.9(3) . . ? O64 Cl6 O61 107.5(3) . . ? Cl6 O61 Cu 137.2(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.342 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.073 data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 655720' ##################################################################### # CHEMICAL INFORMATION # ##################################################################### _chemical_name_systematic ? _chemical_name_common 'Compound 4' _chemical_formula_moiety 'C46 H40 Cu2 N6 O4' _chemical_formula_sum 'C46 H40 Cu2 N6 O4' _chemical_formula_weight 867.92 _chemical_melting_point ? _chemical_compound_source ? ##################################################################### # UNIT CELL INFORMATION # ##################################################################### _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,-y,z+1/2 x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x,-y,-z x-1/2,y,-z-1/2 -x-1/2,y-1/2,z x,-y-1/2,z-1/2 _cell_length_a 20.978(2) _cell_length_b 15.6254(15) _cell_length_c 24.649(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8079.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.50 _cell_measurement_theta_max 18.36 ##################################################################### # CRYSTAL INFORMATION # ##################################################################### _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_special_details ? ##################################################################### # ABSORPTION CORRECTION # ##################################################################### _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.917 _exptl_absorpt_correction_T_max 0.960 ##################################################################### # DATA COLLECTION # ##################################################################### _diffrn_ambient_temperature 295(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44759 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7095 _reflns_number_gt 2789 _reflns_threshold_expression I>2\s(I) ##################################################################### # COMPUTING PROGRAMS # ##################################################################### _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELX97-L (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? ##################################################################### # REFINEMENT INFORMATION # ##################################################################### _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 'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^] 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 7095 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2212 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_details ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.652 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.046 _publ_section_exptl_refinement ? ##################################################################### # ATOMIC TYPES, COORDINATES AND DISPLACEMENT PARAMETERS # ##################################################################### loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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 0.47764(3) 0.13879(4) 0.35109(2) 0.0576(2) Uani 1 1 d . . . Cu2 Cu 0.51114(3) 0.13131(4) 0.88982(2) 0.0623(2) Uani 1 1 d . . . N1 N 0.4720(2) 0.1495(3) 0.27365(16) 0.0565(13) Uani 1 1 d . . . N2 N 0.5289(2) 0.1792(3) 0.24987(16) 0.0568(13) Uani 1 1 d . . . N3 N 0.5090(3) 0.1282(3) 0.9673(2) 0.0892(19) Uani 1 1 d . . . N4 N 0.4510(3) 0.1614(3) 0.9918(2) 0.0786(18) Uani 1 1 d . . . N5 N 0.4922(2) 0.1283(3) 0.43149(15) 0.0481(12) Uani 1 1 d . . . N6 N 0.4952(2) 0.1202(3) 0.81024(15) 0.0487(13) Uani 1 1 d . . . O1 O 0.39740(15) 0.0859(2) 0.35672(13) 0.0558(10) Uani 1 1 d . . . O2 O 0.56156(15) 0.1832(2) 0.33896(14) 0.0697(12) Uani 1 1 d . . . O3 O 0.59250(17) 0.0845(2) 0.88398(15) 0.0736(13) Uani 1 1 d . . . O4 O 0.43094(16) 0.1880(2) 0.90095(15) 0.0765(13) Uani 1 1 d . . . C1 C 0.2371(3) 0.0616(3) 0.3092(2) 0.0664(17) Uani 1 1 d . . . H1 H 0.2378 0.0983 0.2796 0.080 Uiso 1 1 calc R . . C2 C 0.1793(3) 0.0260(4) 0.3257(3) 0.082(2) Uani 1 1 d . . . H2 H 0.1419 0.0381 0.3070 0.099 Uiso 1 1 calc R . . C3 C 0.1788(3) -0.0266(4) 0.3695(3) 0.078(2) Uani 1 1 d . . . H3 H 0.1405 -0.0504 0.3810 0.093 Uiso 1 1 calc R . . C4 C 0.2336(4) -0.0452(4) 0.3972(3) 0.078(2) Uani 1 1 d . . . H4 H 0.2327 -0.0812 0.4272 0.094 Uiso 1 1 calc R . . C5 C 0.2901(3) -0.0098(4) 0.3797(2) 0.0671(19) Uani 1 1 d . . . H5 H 0.3274 -0.0227 0.3984 0.081 Uiso 1 1 calc R . . C6 C 0.2933(3) 0.0436(4) 0.3358(2) 0.0511(16) Uani 1 1 d . . . C7 C 0.3548(3) 0.0797(3) 0.3187(2) 0.0489(15) Uani 1 1 d . . . C8 C 0.3659(2) 0.1023(3) 0.2655(2) 0.0588(17) Uani 1 1 d . . . H8 H 0.3319 0.0961 0.2416 0.071 Uiso 1 1 calc R . . C9 C 0.4238(3) 0.1341(4) 0.2434(2) 0.0537(15) Uani 1 1 d . . . C10 C 0.4287(2) 0.1436(3) 0.18229(17) 0.0862(19) Uani 1 1 d . . . H10A H 0.4701 0.1656 0.1730 0.129 Uiso 1 1 calc R . . H10B H 0.3965 0.1825 0.1698 0.129 Uiso 1 1 calc R . . H10C H 0.4228 0.0889 0.1654 0.129 Uiso 1 1 calc R . . C11 C 0.5710(3) 0.1958(4) 0.2872(3) 0.0582(17) Uani 1 1 d . . . C12 C 0.6323(3) 0.2311(3) 0.2690(3) 0.0572(17) Uani 1 1 d . . . C13 C 0.6795(3) 0.2463(4) 0.3054(3) 0.077(2) Uani 1 1 d . . . H13 H 0.6729 0.2333 0.3418 0.093 Uiso 1 1 calc R . . C14 C 0.7377(3) 0.2810(4) 0.2893(3) 0.108(3) Uani 1 1 d . . . H14 H 0.7701 0.2895 0.3145 0.130 Uiso 1 1 calc R . . C15 C 0.7469(3) 0.3023(4) 0.2364(3) 0.102(3) Uani 1 1 d . . . H15 H 0.7854 0.3261 0.2255 0.123 Uiso 1 1 calc R . . C16 C 0.6998(3) 0.2891(4) 0.1993(3) 0.089(2) Uani 1 1 d . . . H16 H 0.7059 0.3044 0.1632 0.107 Uiso 1 1 calc R . . C17 C 0.6431(3) 0.2531(3) 0.2156(3) 0.071(2) Uani 1 1 d . . . H17 H 0.6113 0.2434 0.1901 0.086 Uiso 1 1 calc R . . C18 C 0.7330(4) -0.0047(4) 0.9486(3) 0.121(3) Uani 1 1 d . . . H18 H 0.7210 -0.0054 0.9849 0.145 Uiso 1 1 calc R . . C19 C 0.7933(4) -0.0343(5) 0.9362(3) 0.132(3) Uani 1 1 d . . . H19 H 0.8204 -0.0524 0.9637 0.159 Uiso 1 1 calc R . . C20 C 0.8123(3) -0.0368(4) 0.8847(4) 0.095(3) Uani 1 1 d . . . H20 H 0.8520 -0.0588 0.8754 0.114 Uiso 1 1 calc R . . C21 C 0.7728(4) -0.0070(5) 0.8469(3) 0.116(3) Uani 1 1 d . . . H21 H 0.7855 -0.0069 0.8108 0.139 Uiso 1 1 calc R . . C22 C 0.7119(3) 0.0245(4) 0.8608(3) 0.104(3) Uani 1 1 d . . . H22 H 0.6856 0.0455 0.8335 0.125 Uiso 1 1 calc R . . C23 C 0.6904(3) 0.0250(4) 0.9127(3) 0.0615(19) Uani 1 1 d . . . C24 C 0.6259(3) 0.0606(3) 0.9242(3) 0.0570(17) Uani 1 1 d . . . C25 C 0.6070(3) 0.0654(3) 0.9767(3) 0.0709(19) Uani 1 1 d . . . H25 H 0.6360 0.0442 1.0019 0.085 Uiso 1 1 calc R . . C26 C 0.5481(4) 0.0990(4) 0.9993(3) 0.079(2) Uani 1 1 d . . . C27 C 0.5394(2) 0.0969(3) 1.06002(19) 0.083(2) Uani 1 1 d . . . H27A H 0.4984 0.1202 1.0692 0.124 Uiso 1 1 calc R . . H27B H 0.5722 0.1302 1.0770 0.124 Uiso 1 1 calc R . . H27C H 0.5419 0.0388 1.0726 0.124 Uiso 1 1 calc R . . C28 C 0.4144(3) 0.1903(4) 0.9523(3) 0.0671(19) Uani 1 1 d . . . C29 C 0.3521(3) 0.2234(4) 0.9685(3) 0.0638(18) Uani 1 1 d . . . C30 C 0.3141(4) 0.2609(4) 0.9310(3) 0.080(2) Uani 1 1 d . . . H30 H 0.3285 0.2650 0.8954 0.096 Uiso 1 1 calc R . . C31 C 0.2548(4) 0.2934(4) 0.9437(3) 0.100(3) Uani 1 1 d . . . H31 H 0.2302 0.3204 0.9174 0.120 Uiso 1 1 calc R . . C32 C 0.2332(4) 0.2855(5) 0.9944(4) 0.118(3) Uani 1 1 d . . . H32 H 0.1926 0.3053 1.0031 0.141 Uiso 1 1 calc R . . C33 C 0.2695(4) 0.2492(5) 1.0331(3) 0.134(4) Uani 1 1 d . . . H33 H 0.2541 0.2455 1.0684 0.160 Uiso 1 1 calc R . . C34 C 0.3301(3) 0.2168(4) 1.0208(3) 0.106(3) Uani 1 1 d . . . H34 H 0.3549 0.1914 1.0476 0.127 Uiso 1 1 calc R . . C35 C 0.5461(2) 0.1552(3) 0.4553(2) 0.0564(18) Uani 1 1 d . . . H35 H 0.5793 0.1742 0.4334 0.068 Uiso 1 1 calc R . . C36 C 0.5546(2) 0.1559(3) 0.5106(2) 0.0604(18) Uani 1 1 d . . . H36 H 0.5924 0.1762 0.5254 0.072 Uiso 1 1 calc R . . C37 C 0.5068(3) 0.1264(3) 0.5439(2) 0.0557(16) Uani 1 1 d . . . C38 C 0.4526(3) 0.0970(3) 0.5202(2) 0.0668(19) Uani 1 1 d . . . H38 H 0.4200 0.0752 0.5416 0.080 Uiso 1 1 calc R . . C39 C 0.4457(2) 0.0993(3) 0.4645(2) 0.0587(17) Uani 1 1 d . . . H39 H 0.4078 0.0801 0.4492 0.070 Uiso 1 1 calc R . . C40 C 0.5158(2) 0.1285(4) 0.60518(18) 0.0880(18) Uani 1 1 d . . . H40A H 0.5540 0.0963 0.6139 0.106 Uiso 1 1 calc R . . H40B H 0.5233 0.1873 0.6159 0.106 Uiso 1 1 calc R . . C41 C 0.4636(2) 0.0948(3) 0.63806(18) 0.0777(19) Uani 1 1 d . . . H41A H 0.4574 0.0349 0.6292 0.093 Uiso 1 1 calc R . . H41B H 0.4247 0.1250 0.6287 0.093 Uiso 1 1 calc R . . C42 C 0.4746(3) 0.1028(3) 0.6988(2) 0.0563(16) Uani 1 1 d . . . C43 C 0.4285(2) 0.1340(4) 0.7330(2) 0.0637(17) Uani 1 1 d . . . H43 H 0.3891 0.1501 0.7191 0.076 Uiso 1 1 calc R . . C44 C 0.4406(2) 0.1417(4) 0.7883(2) 0.0645(17) Uani 1 1 d . . . H44 H 0.4085 0.1629 0.8107 0.077 Uiso 1 1 calc R . . C45 C 0.5389(2) 0.0873(3) 0.7779(2) 0.0588(17) Uani 1 1 d . . . H45 H 0.5772 0.0691 0.7932 0.071 Uiso 1 1 calc R . . C46 C 0.5306(3) 0.0785(3) 0.7222(2) 0.0626(17) Uani 1 1 d . . . H46 H 0.5633 0.0562 0.7010 0.075 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 0.0570(4) 0.0743(5) 0.0416(4) 0.0099(4) 0.0038(4) 0.0000(5) Cu2 0.0696(6) 0.0746(5) 0.0427(5) -0.0071(4) 0.0005(4) -0.0071(5) N1 0.061(3) 0.071(3) 0.037(3) 0.009(3) 0.001(3) -0.006(3) N2 0.055(3) 0.067(4) 0.049(3) 0.009(3) 0.018(3) -0.010(3) N3 0.135(6) 0.081(4) 0.052(4) 0.000(4) -0.003(4) -0.022(4) N4 0.069(4) 0.096(5) 0.070(4) -0.017(4) 0.030(3) 0.000(3) N5 0.050(3) 0.051(3) 0.043(3) 0.013(3) 0.004(3) 0.008(3) N6 0.053(3) 0.056(3) 0.037(3) -0.002(2) 0.002(3) 0.012(3) O1 0.057(2) 0.075(3) 0.035(2) 0.005(2) -0.002(2) -0.009(2) O2 0.049(2) 0.117(4) 0.043(3) 0.026(2) 0.007(2) -0.004(2) O3 0.066(3) 0.096(3) 0.059(3) 0.011(2) -0.021(2) 0.016(2) O4 0.064(3) 0.107(3) 0.059(3) -0.030(3) 0.021(2) -0.006(2) C1 0.066(4) 0.079(5) 0.055(4) -0.004(3) 0.010(4) -0.019(4) C2 0.068(5) 0.101(6) 0.078(6) -0.013(4) 0.008(4) -0.011(5) C3 0.070(6) 0.089(6) 0.075(6) -0.023(5) 0.033(4) -0.042(5) C4 0.095(6) 0.082(5) 0.057(5) -0.014(4) 0.022(5) -0.033(5) C5 0.073(5) 0.073(5) 0.055(5) -0.005(4) 0.023(4) -0.017(4) C6 0.048(4) 0.063(5) 0.042(4) -0.004(3) 0.005(3) -0.010(4) C7 0.053(4) 0.051(4) 0.042(4) 0.000(3) 0.014(3) -0.005(3) C8 0.051(4) 0.080(5) 0.045(4) 0.003(3) 0.002(3) -0.007(3) C9 0.060(4) 0.063(4) 0.038(4) -0.001(4) 0.002(3) 0.004(4) C10 0.102(5) 0.125(5) 0.031(3) 0.010(4) 0.000(3) -0.026(4) C11 0.047(4) 0.065(5) 0.062(5) 0.003(4) 0.005(4) 0.007(4) C12 0.045(4) 0.063(4) 0.064(5) 0.015(4) 0.014(4) 0.008(4) C13 0.049(5) 0.112(6) 0.071(5) 0.012(4) 0.007(4) -0.011(4) C14 0.067(6) 0.162(7) 0.097(7) 0.011(6) 0.003(5) -0.031(5) C15 0.069(6) 0.122(6) 0.117(8) 0.032(6) 0.024(5) -0.025(5) C16 0.079(6) 0.101(6) 0.088(6) 0.029(5) 0.024(5) -0.010(5) C17 0.054(5) 0.091(5) 0.069(5) 0.020(4) 0.016(4) 0.001(4) C18 0.092(6) 0.193(9) 0.078(6) 0.036(5) 0.022(5) 0.062(6) C19 0.113(8) 0.175(8) 0.108(8) 0.040(6) 0.008(6) 0.073(6) C20 0.081(6) 0.092(6) 0.113(8) -0.012(6) 0.014(6) 0.017(5) C21 0.092(6) 0.177(9) 0.078(7) -0.021(6) 0.001(6) 0.006(6) C22 0.079(6) 0.162(7) 0.072(6) -0.014(6) -0.022(5) 0.013(5) C23 0.084(6) 0.061(5) 0.039(4) -0.001(4) -0.011(4) -0.001(4) C24 0.043(4) 0.054(4) 0.074(5) -0.010(4) 0.001(4) 0.008(3) C25 0.055(4) 0.081(5) 0.077(5) -0.011(4) -0.004(4) 0.003(4) C26 0.103(6) 0.076(6) 0.056(5) 0.016(4) -0.028(5) -0.025(5) C27 0.104(5) 0.101(5) 0.045(4) 0.004(4) -0.006(4) -0.005(4) C28 0.062(5) 0.064(5) 0.075(6) -0.022(4) 0.009(5) -0.020(4) C29 0.049(5) 0.073(5) 0.069(5) -0.015(4) 0.011(4) -0.003(4) C30 0.078(6) 0.063(5) 0.099(7) 0.001(4) 0.017(5) -0.001(4) C31 0.098(7) 0.086(6) 0.115(8) 0.005(5) -0.003(6) 0.015(5) C32 0.084(7) 0.133(8) 0.136(10) -0.016(7) 0.021(7) 0.007(6) C33 0.117(9) 0.199(10) 0.085(8) -0.018(6) 0.050(7) 0.023(7) C34 0.090(6) 0.165(7) 0.063(6) -0.011(5) 0.020(5) 0.017(5) C35 0.038(4) 0.085(5) 0.047(4) 0.004(4) -0.003(3) -0.001(4) C36 0.056(4) 0.083(5) 0.043(4) -0.003(4) -0.002(3) -0.001(4) C37 0.062(4) 0.070(4) 0.035(3) -0.002(4) 0.004(3) -0.008(4) C38 0.065(4) 0.091(5) 0.045(4) 0.015(4) 0.000(3) -0.011(4) C39 0.055(4) 0.071(5) 0.050(4) 0.012(4) 0.002(3) -0.006(3) C40 0.087(4) 0.145(5) 0.033(3) 0.002(4) -0.001(4) -0.015(5) C41 0.085(5) 0.112(5) 0.036(4) 0.001(3) -0.002(3) 0.011(4) C42 0.064(4) 0.073(5) 0.032(4) 0.002(3) 0.001(4) -0.002(4) C43 0.048(4) 0.098(5) 0.045(4) 0.013(4) -0.002(3) 0.000(4) C44 0.050(4) 0.096(5) 0.048(4) 0.012(4) 0.005(3) 0.004(4) C45 0.062(4) 0.073(4) 0.042(4) -0.014(3) -0.004(3) 0.022(3) C46 0.078(5) 0.072(4) 0.038(4) -0.006(3) 0.003(4) 0.032(4) ##################################################################### # MOLECULAR GEOMETRY # ##################################################################### 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 1.880(3) . ? Cu1 O2 1.916(3) . ? Cu1 N1 1.920(4) . ? Cu1 N5 2.012(4) . ? Cu2 O3 1.862(4) . ? Cu2 N3 1.912(5) . ? Cu2 O4 1.921(3) . ? Cu2 N6 1.998(4) . ? N1 C9 1.281(5) . ? N1 N2 1.409(5) . ? N2 C11 1.301(6) . ? N3 C26 1.226(6) . ? N3 N4 1.453(6) . ? N4 C28 1.319(6) . ? N5 C35 1.341(5) . ? N5 C39 1.348(5) . ? N6 C44 1.309(5) . ? N6 C45 1.319(5) . ? O1 C7 1.299(5) . ? O2 C11 1.306(6) . ? O3 C24 1.271(6) . ? O4 C28 1.313(6) . ? C1 C6 1.378(6) . ? C1 C2 1.395(6) . ? C1 H1 0.9300 . ? C2 C3 1.358(7) . ? C2 H2 0.9300 . ? C3 C4 1.368(7) . ? C3 H3 0.9300 . ? C4 C5 1.377(7) . ? C4 H4 0.9300 . ? C5 C6 1.368(6) . ? C5 H5 0.9300 . ? C6 C7 1.469(6) . ? C7 C8 1.378(6) . ? C8 C9 1.421(6) . ? C8 H8 0.9300 . ? C9 C10 1.516(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.470(7) . ? C12 C13 1.357(7) . ? C12 C17 1.378(7) . ? C13 C14 1.394(7) . ? C13 H13 0.9300 . ? C14 C15 1.358(8) . ? C14 H14 0.9300 . ? C15 C16 1.361(7) . ? C15 H15 0.9300 . ? C16 C17 1.376(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.341(7) . ? C18 C19 1.380(8) . ? C18 H18 0.9300 . ? C19 C20 1.331(8) . ? C19 H19 0.9300 . ? C20 C21 1.330(8) . ? C20 H20 0.9300 . ? C21 C22 1.412(8) . ? C21 H21 0.9300 . ? C22 C23 1.355(8) . ? C22 H22 0.9300 . ? C23 C24 1.490(7) . ? C24 C25 1.355(7) . ? C25 C26 1.455(8) . ? C25 H25 0.9300 . ? C26 C27 1.507(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.461(7) . ? C29 C30 1.355(7) . ? C29 C34 1.374(8) . ? C30 C31 1.380(8) . ? C30 H30 0.9300 . ? C31 C32 1.335(8) . ? C31 H31 0.9300 . ? C32 C33 1.347(9) . ? C32 H32 0.9300 . ? C33 C34 1.401(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.374(6) . ? C35 H35 0.9300 . ? C36 C37 1.375(6) . ? C36 H36 0.9300 . ? C37 C38 1.357(6) . ? C37 C40 1.523(6) . ? C38 C39 1.381(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.461(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.519(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C46 1.363(6) . ? C42 C43 1.372(6) . ? C43 C44 1.393(6) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.392(6) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? 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 173.40(15) . . ? O1 Cu1 N1 93.24(17) . . ? O2 Cu1 N1 82.51(17) . . ? O1 Cu1 N5 91.59(17) . . ? O2 Cu1 N5 92.49(17) . . ? N1 Cu1 N5 174.76(19) . . ? O3 Cu2 N3 95.1(2) . . ? O3 Cu2 O4 174.08(16) . . ? N3 Cu2 O4 81.3(2) . . ? O3 Cu2 N6 92.51(17) . . ? N3 Cu2 N6 167.2(2) . . ? O4 Cu2 N6 91.91(17) . . ? C9 N1 N2 119.3(4) . . ? C9 N1 Cu1 127.7(4) . . ? N2 N1 Cu1 113.0(3) . . ? C11 N2 N1 110.3(4) . . ? C26 N3 N4 115.2(6) . . ? C26 N3 Cu2 129.6(6) . . ? N4 N3 Cu2 115.2(4) . . ? C28 N4 N3 107.7(5) . . ? C35 N5 C39 116.8(4) . . ? C35 N5 Cu1 122.3(4) . . ? C39 N5 Cu1 120.8(4) . . ? C44 N6 C45 117.4(5) . . ? C44 N6 Cu2 122.0(4) . . ? C45 N6 Cu2 120.6(4) . . ? C7 O1 Cu1 126.6(3) . . ? C11 O2 Cu1 110.3(4) . . ? C24 O3 Cu2 124.1(4) . . ? C28 O4 Cu2 112.4(4) . . ? C6 C1 C2 121.7(6) . . ? C6 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 118.7(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 121.2(7) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 118.9(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 122.3(6) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 117.3(5) . . ? C5 C6 C7 120.3(6) . . ? C1 C6 C7 122.4(6) . . ? O1 C7 C8 123.5(5) . . ? O1 C7 C6 115.2(5) . . ? C8 C7 C6 121.3(5) . . ? C7 C8 C9 126.8(5) . . ? C7 C8 H8 116.6 . . ? C9 C8 H8 116.6 . . ? N1 C9 C8 121.1(5) . . ? N1 C9 C10 120.4(5) . . ? C8 C9 C10 118.3(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 O2 123.9(5) . . ? N2 C11 C12 116.9(6) . . ? O2 C11 C12 119.2(5) . . ? C13 C12 C17 117.9(6) . . ? C13 C12 C11 120.2(6) . . ? C17 C12 C11 121.9(6) . . ? C12 C13 C14 121.2(6) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 119.5(7) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.3(7) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.6(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C12 121.5(6) . . ? C16 C17 H17 119.3 . . ? C12 C17 H17 119.3 . . ? C23 C18 C19 125.4(7) . . ? C23 C18 H18 117.3 . . ? C19 C18 H18 117.3 . . ? C20 C19 C18 119.7(8) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 118.0(8) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 C22 121.1(8) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 122.1(7) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C18 C23 C22 113.5(7) . . ? C18 C23 C24 127.4(7) . . ? C22 C23 C24 118.9(7) . . ? O3 C24 C25 124.6(6) . . ? O3 C24 C23 117.5(6) . . ? C25 C24 C23 118.0(6) . . ? C24 C25 C26 129.4(6) . . ? C24 C25 H25 115.3 . . ? C26 C25 H25 115.3 . . ? N3 C26 C25 117.1(7) . . ? N3 C26 C27 124.4(7) . . ? C25 C26 C27 118.4(6) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 N4 123.2(6) . . ? O4 C28 C29 120.6(6) . . ? N4 C28 C29 116.2(7) . . ? C30 C29 C34 118.4(7) . . ? C30 C29 C28 119.6(7) . . ? C34 C29 C28 122.1(7) . . ? C29 C30 C31 122.3(7) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C32 C31 C30 119.1(8) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 120.7(10) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 120.8(9) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C29 C34 C33 118.8(7) . . ? C29 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N5 C35 C36 123.1(5) . . ? N5 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C37 119.7(5) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 117.8(5) . . ? C38 C37 C40 122.6(5) . . ? C36 C37 C40 119.6(5) . . ? C37 C38 C39 120.5(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? N5 C39 C38 122.2(5) . . ? N5 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C41 C40 C37 116.7(4) . . ? C41 C40 H40A 108.1 . . ? C37 C40 H40A 108.1 . . ? C41 C40 H40B 108.1 . . ? C37 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? C40 C41 C42 113.7(4) . . ? C40 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? C40 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C46 C42 C43 116.5(5) . . ? C46 C42 C41 121.7(5) . . ? C43 C42 C41 121.8(5) . . ? C42 C43 C44 120.3(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? N6 C44 C43 122.7(5) . . ? N6 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? N6 C45 C46 123.2(5) . . ? N6 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C42 C46 C45 119.9(5) . . ? C42 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? #===END