Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Gajda, Tamas' 'Jancso, Attila' 'Lonnberg, Harri' 'Mikkola, Satu' 'Sirges, Holger' _publ_contact_author_name 'Prof Tamas Gajda' _publ_contact_author_address ; Inorganic and Analytical Chemistry University of Szeged Dóm tér 7. Szeged H-6720 HUNGARY ; _publ_contact_author_phone 'xx36 62 544054' _publ_contact_author_fax 'xx36 62 420505' _publ_contact_author_email tamas.gajda@chem.u-szeged.hu _publ_requested_journal 'Journal of Chemical Society, Dalton Transaction' _publ_section_title ; Crystal structure, solution properties and hydrolytic activity of an alkoxo-bridged dinuclear copper(II) complex, as a ribonuclease model ; data_[Cu(bpdpo)(ClO4)2] _database_code_CSD 163302 _chemical_name_systematic ; N,N'-bis(2-pyridylmethyl)-1,3-diaminopropan-2-ol copper(II) diperchlorate ; _chemical_name_common '[Cu(hbdpo)(ClO4)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Cl2 Cu N4 O9' _chemical_formula_weight 534.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.714(2) _cell_length_b 12.817(3) _cell_length_c 27.364(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.77(3) _cell_angle_gamma 90.00 _cell_volume 4108.0(14) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.01 _exptl_crystal_description plate _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IDPS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 181 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9079 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.1351 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.01 _reflns_number_total 8674 _reflns_number_gt 4084 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8674 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1496 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.53991(6) 0.75067(7) 0.40134(3) 0.0309(2) Uani 1 1 d . . . N1 N 0.5941(4) 0.7121(4) 0.33435(18) 0.0302(13) Uani 1 1 d . . . N2 N 0.3837(4) 0.7415(5) 0.36944(18) 0.0324(13) Uani 1 1 d . . . H2A H 0.3562 0.6749 0.3758 0.039 Uiso 1 1 calc R . . N3 N 0.4727(5) 0.7474(5) 0.46946(19) 0.0423(15) Uani 1 1 d . . . H3A H 0.4430 0.6807 0.4736 0.051 Uiso 1 1 calc R . . N4 N 0.6776(4) 0.8107(4) 0.43456(17) 0.0305(13) Uani 1 1 d . . . O2 O 0.6169(5) 0.5775(5) 0.4275(2) 0.0689(18) Uani 1 1 d . . . Cu1A Cu 1.03675(7) 0.32881(7) 0.35302(3) 0.0362(2) Uani 1 1 d . . . N4A N 1.0853(5) 0.3637(5) 0.42206(19) 0.0339(14) Uani 1 1 d . . . N3A N 0.9039(5) 0.2560(7) 0.3847(2) 0.059(2) Uani 1 1 d . . . H3AA H 0.9013 0.1897 0.3709 0.071 Uiso 1 1 calc R . . N2A N 0.9540(5) 0.3291(5) 0.2874(2) 0.0401(15) Uani 1 1 d . . . H2AA H 0.9562 0.2608 0.2760 0.048 Uiso 1 1 calc R . . N1A N 1.1728(5) 0.3667(5) 0.31346(19) 0.0346(13) Uani 1 1 d . . . O2A O 1.1404(6) 0.1566(5) 0.3610(3) 0.078(2) Uani 1 1 d . . . Cl1 Cl 0.55417(18) 0.48364(17) 0.41706(7) 0.0491(5) Uani 1 1 d . . . Cl1A Cl 1.10263(15) 0.05179(15) 0.35430(6) 0.0382(4) Uani 1 1 d . . . Cl2 Cl 0.54282(18) 1.04845(16) 0.38349(6) 0.0477(5) Uani 1 1 d . . . Cl2A Cl 1.03566(14) 0.63146(14) 0.34244(6) 0.0356(4) Uani 1 1 d . . . O1 O 0.2386(4) 0.6973(4) 0.45308(19) 0.0511(14) Uani 1 1 d . . . H1A H 0.2140 0.6699 0.4271 0.077 Uiso 1 1 calc R . . O1A O 0.7623(6) 0.1936(5) 0.3042(2) 0.0750(19) Uani 1 1 d . . . H1AA H 0.7322 0.1541 0.3249 0.112 Uiso 1 1 calc R . . O3 O 0.5844(7) 0.4603(7) 0.3656(3) 0.123(3) Uani 1 1 d . . . O3A O 1.1710(5) -0.0021(5) 0.31924(19) 0.0652(18) Uani 1 1 d . . . O4 O 0.5914(7) 0.4040(6) 0.4463(3) 0.119(3) Uani 1 1 d . . . O5A O 0.9835(5) 0.0499(5) 0.3395(2) 0.0619(17) Uani 1 1 d . . . O5 O 0.4362(5) 0.5075(6) 0.4156(3) 0.095(2) Uani 1 1 d . . . O4A O 1.1126(4) -0.0040(4) 0.40006(17) 0.0500(14) Uani 1 1 d . . . O7A O 0.9690(4) 0.5399(4) 0.35396(19) 0.0525(14) Uani 1 1 d . . . O7 O 0.5211(6) 0.9542(5) 0.3563(2) 0.085(2) Uani 1 1 d . . . O6A O 1.1535(5) 0.6125(5) 0.3530(3) 0.078(2) Uani 1 1 d . . . O8A O 0.9973(6) 0.7195(5) 0.3697(3) 0.081(2) Uani 1 1 d . . . O9A O 1.0232(6) 0.6520(5) 0.2918(2) 0.081(2) Uani 1 1 d . . . O6 O 0.5331(7) 1.0263(5) 0.4337(2) 0.088(2) Uani 1 1 d . . . O8 O 0.4808(10) 1.1358(8) 0.3699(3) 0.147(4) Uani 1 1 d . . . O9 O 0.6628(8) 1.0705(7) 0.3759(4) 0.132(3) Uani 1 1 d . . . C1 C 0.7003(6) 0.6785(6) 0.3225(2) 0.0351(17) Uani 1 1 d . . . H1B H 0.7590 0.6786 0.3468 0.042 Uiso 1 1 calc R . . C15A C 1.1690(6) 0.4311(6) 0.4368(2) 0.0366(17) Uani 1 1 d . . . H15C H 1.2130 0.4657 0.4128 0.044 Uiso 1 1 calc R . . C2 C 0.7250(6) 0.6439(6) 0.2758(2) 0.0372(17) Uani 1 1 d . . . H2B H 0.8006 0.6238 0.2680 0.045 Uiso 1 1 calc R . . C14A C 1.1915(6) 0.4506(6) 0.4855(3) 0.0430(19) Uani 1 1 d . . . H14C H 1.2507 0.4973 0.4949 0.052 Uiso 1 1 calc R . . C3 C 0.6391(6) 0.6390(6) 0.2409(2) 0.0412(19) Uani 1 1 d . . . H3B H 0.6544 0.6135 0.2090 0.049 Uiso 1 1 calc R . . C13A C 1.1262(6) 0.4007(6) 0.5208(2) 0.0423(19) Uani 1 1 d . . . H13C H 1.1413 0.4123 0.5545 0.051 Uiso 1 1 calc R . . C4 C 0.5296(6) 0.6721(6) 0.2530(2) 0.0357(17) Uani 1 1 d . . . H4B H 0.4690 0.6693 0.2296 0.043 Uiso 1 1 calc R . . C12A C 1.0403(6) 0.3348(7) 0.5062(2) 0.046(2) Uani 1 1 d . . . H12C H 0.9939 0.3018 0.5299 0.055 Uiso 1 1 calc R . . C5 C 0.5107(6) 0.7096(5) 0.3005(2) 0.0327(16) Uani 1 1 d . . . C11A C 1.0209(6) 0.3164(6) 0.4562(2) 0.0394(18) Uani 1 1 d . . . C6 C 0.3964(5) 0.7494(6) 0.3159(2) 0.0350(16) Uani 1 1 d . . . H6B H 0.3878 0.8231 0.3057 0.042 Uiso 1 1 calc R . . H6C H 0.3354 0.7083 0.2995 0.042 Uiso 1 1 calc R . . C10A C 0.9328(7) 0.2394(8) 0.4374(3) 0.063(3) Uani 1 1 d . . . H10D H 0.9624 0.1676 0.4420 0.076 Uiso 1 1 calc R . . H10E H 0.8626 0.2462 0.4569 0.076 Uiso 1 1 calc R . . C7 C 0.2989(6) 0.8159(6) 0.3888(2) 0.0367(17) Uani 1 1 d . . . H7B H 0.2262 0.8076 0.3704 0.044 Uiso 1 1 calc R . . H7C H 0.3265 0.8880 0.3834 0.044 Uiso 1 1 calc R . . C9A C 0.7975(7) 0.3000(8) 0.3750(3) 0.058(2) Uani 1 1 d . . . H9D H 0.7987 0.3732 0.3864 0.070 Uiso 1 1 calc R . . H9E H 0.7398 0.2623 0.3944 0.070 Uiso 1 1 calc R . . C8 C 0.2766(6) 0.8005(6) 0.4432(2) 0.0396(18) Uani 1 1 d . . . H8B H 0.2140 0.8494 0.4525 0.047 Uiso 1 1 calc R . . C8A C 0.7593(7) 0.2988(6) 0.3214(3) 0.0446(19) Uani 1 1 d . . . H8C H 0.6793 0.3256 0.3188 0.054 Uiso 1 1 calc R . . C9 C 0.3765(6) 0.8207(6) 0.4771(2) 0.0395(18) Uani 1 1 d . . . H9B H 0.4038 0.8929 0.4721 0.047 Uiso 1 1 calc R . . H9C H 0.3508 0.8147 0.5113 0.047 Uiso 1 1 calc R . . C7A C 0.8323(7) 0.3591(8) 0.2882(3) 0.069(3) Uani 1 1 d . . . H7D H 0.8275 0.4336 0.2975 0.083 Uiso 1 1 calc R . . H7E H 0.8006 0.3524 0.2547 0.083 Uiso 1 1 calc R . . C10 C 0.5686(6) 0.7572(6) 0.5051(2) 0.0383(17) Uani 1 1 d . . . H10A H 0.5952 0.6867 0.5146 0.046 Uiso 1 1 calc R . . H10B H 0.5413 0.7927 0.5348 0.046 Uiso 1 1 calc R . . C6A C 1.0207(6) 0.3922(6) 0.2528(2) 0.0405(18) Uani 1 1 d . . . H6D H 0.9891 0.4638 0.2515 0.049 Uiso 1 1 calc R . . H6E H 1.0132 0.3616 0.2197 0.049 Uiso 1 1 calc R . . C11 C 0.6679(6) 0.8182(6) 0.4843(2) 0.0310(16) Uani 1 1 d . . . C5A C 1.1454(6) 0.3974(5) 0.2670(2) 0.0343(17) Uani 1 1 d . . . C12 C 0.7446(6) 0.8718(6) 0.5127(3) 0.0441(19) Uani 1 1 d . . . H12A H 0.7349 0.8764 0.5470 0.053 Uiso 1 1 calc R . . C4A C 1.2265(7) 0.4324(6) 0.2351(2) 0.0404(18) Uani 1 1 d . . . H4C H 1.2055 0.4535 0.2029 0.049 Uiso 1 1 calc R . . C13 C 0.8369(6) 0.9196(7) 0.4907(3) 0.048(2) Uani 1 1 d . . . H13A H 0.8911 0.9576 0.5097 0.057 Uiso 1 1 calc R . . C3A C 1.3388(7) 0.4363(7) 0.2505(3) 0.054(2) Uani 1 1 d . . . H3C H 1.3961 0.4613 0.2293 0.065 Uiso 1 1 calc R . . C14 C 0.8485(6) 0.9111(6) 0.4411(3) 0.044(2) Uani 1 1 d . . . H14A H 0.9124 0.9414 0.4254 0.053 Uiso 1 1 calc R . . C2A C 1.3671(7) 0.4038(6) 0.2968(3) 0.052(2) Uani 1 1 d . . . H2C H 1.4442 0.4061 0.3080 0.063 Uiso 1 1 calc R . . C15 C 0.7664(6) 0.8581(6) 0.4139(2) 0.0390(18) Uani 1 1 d . . . H15A H 0.7736 0.8552 0.3794 0.047 Uiso 1 1 calc R . . C1A C 1.2817(6) 0.3675(6) 0.3272(2) 0.0421(18) Uani 1 1 d . . . H1C H 1.3020 0.3425 0.3588 0.051 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 0.0249(4) 0.0486(5) 0.0195(4) -0.0030(4) 0.0057(3) 0.0010(4) N1 0.023(3) 0.045(4) 0.022(3) 0.004(2) 0.004(2) -0.001(3) N2 0.030(3) 0.041(4) 0.026(3) -0.001(3) 0.004(2) 0.000(3) N3 0.031(3) 0.068(4) 0.028(3) -0.003(3) 0.010(2) -0.004(3) N4 0.029(3) 0.042(4) 0.020(3) 0.000(2) 0.007(2) -0.003(3) O2 0.072(4) 0.070(4) 0.064(4) 0.033(3) -0.008(3) -0.023(4) Cu1A 0.0308(5) 0.0534(6) 0.0246(4) 0.0090(4) 0.0046(3) -0.0038(4) N4A 0.031(3) 0.043(4) 0.028(3) 0.009(3) 0.012(2) 0.002(3) N3A 0.034(3) 0.110(6) 0.035(3) 0.022(4) 0.004(3) -0.017(4) N2A 0.043(4) 0.042(4) 0.035(3) 0.007(3) 0.001(3) -0.001(3) N1A 0.036(3) 0.040(4) 0.028(3) 0.000(3) 0.006(2) -0.006(3) O2A 0.081(5) 0.041(4) 0.110(5) 0.014(4) 0.001(4) -0.010(3) Cl1 0.0530(12) 0.0452(12) 0.0490(11) -0.0109(10) 0.0015(9) 0.0008(10) Cl1A 0.0410(10) 0.0466(12) 0.0272(8) 0.0007(8) 0.0029(7) -0.0006(9) Cl2 0.0648(13) 0.0451(12) 0.0336(9) -0.0027(9) 0.0092(9) -0.0096(11) Cl2A 0.0372(9) 0.0381(10) 0.0315(9) 0.0005(8) 0.0033(7) -0.0024(8) O1 0.049(3) 0.055(4) 0.050(3) 0.002(3) 0.009(3) -0.011(3) O1A 0.076(5) 0.071(5) 0.078(4) 0.003(4) 0.012(4) -0.007(4) O3 0.131(7) 0.145(8) 0.091(6) -0.056(5) -0.016(5) 0.048(6) O3A 0.052(3) 0.103(5) 0.041(3) -0.006(3) 0.025(3) 0.004(4) O4 0.107(6) 0.074(5) 0.175(9) 0.064(6) 0.025(6) -0.007(5) O5A 0.050(3) 0.071(4) 0.065(4) -0.027(3) -0.012(3) 0.016(3) O5 0.048(4) 0.098(6) 0.138(7) -0.028(5) 0.005(4) 0.006(4) O4A 0.059(3) 0.058(4) 0.033(3) 0.009(3) 0.007(2) 0.007(3) O7A 0.048(3) 0.048(4) 0.062(3) 0.010(3) 0.004(3) -0.015(3) O7 0.106(5) 0.091(5) 0.060(4) -0.038(4) 0.030(4) -0.046(4) O6A 0.044(4) 0.048(4) 0.142(6) 0.007(4) -0.012(4) -0.004(3) O8A 0.087(5) 0.058(4) 0.098(5) -0.038(4) 0.040(4) -0.006(4) O9A 0.115(6) 0.092(5) 0.038(3) 0.023(3) -0.005(3) -0.023(4) O6 0.172(7) 0.058(4) 0.035(3) 0.006(3) 0.015(4) 0.012(5) O8 0.229(11) 0.133(8) 0.079(5) -0.007(5) -0.045(6) 0.093(8) O9 0.115(7) 0.112(7) 0.170(9) 0.012(6) 0.044(6) -0.053(6) C1 0.031(4) 0.046(5) 0.029(3) 0.000(3) 0.006(3) -0.002(3) C15A 0.040(4) 0.041(4) 0.029(3) 0.003(3) 0.008(3) -0.001(4) C2 0.034(4) 0.048(5) 0.030(4) 0.001(3) 0.015(3) 0.007(4) C14A 0.040(4) 0.047(5) 0.042(4) -0.004(4) 0.006(3) -0.003(4) C3 0.051(4) 0.051(5) 0.021(3) -0.009(3) 0.016(3) -0.003(4) C13A 0.043(4) 0.063(6) 0.020(3) 0.000(3) 0.002(3) 0.010(4) C4 0.039(4) 0.045(5) 0.023(3) -0.004(3) -0.001(3) -0.008(3) C12A 0.033(4) 0.074(6) 0.031(4) 0.010(4) 0.013(3) 0.006(4) C5 0.040(4) 0.037(4) 0.022(3) -0.003(3) 0.007(3) -0.002(3) C11A 0.031(4) 0.055(5) 0.033(4) 0.014(4) 0.007(3) -0.002(4) C6 0.034(4) 0.047(4) 0.024(3) 0.002(3) -0.004(3) -0.001(4) C10A 0.048(5) 0.109(8) 0.033(4) 0.017(5) 0.000(3) -0.027(5) C7 0.033(4) 0.041(5) 0.037(4) 0.002(3) 0.004(3) 0.015(3) C9A 0.037(5) 0.087(7) 0.051(5) 0.008(5) 0.005(4) 0.009(5) C8 0.028(4) 0.055(5) 0.036(4) 0.004(4) 0.015(3) 0.000(4) C8A 0.039(4) 0.044(5) 0.051(5) -0.009(4) -0.004(4) -0.004(4) C9 0.037(4) 0.049(5) 0.033(4) -0.005(3) 0.011(3) 0.006(4) C7A 0.050(5) 0.096(8) 0.061(6) 0.024(5) -0.014(4) -0.018(5) C10 0.036(4) 0.056(5) 0.023(3) -0.002(3) 0.004(3) -0.002(4) C6A 0.052(5) 0.043(5) 0.026(3) 0.000(3) -0.003(3) -0.012(4) C11 0.032(4) 0.040(4) 0.021(3) -0.001(3) 0.003(3) 0.002(3) C5A 0.050(4) 0.031(4) 0.022(3) -0.005(3) 0.006(3) -0.010(3) C12 0.043(4) 0.062(5) 0.027(4) -0.003(4) 0.005(3) 0.001(4) C4A 0.059(5) 0.038(4) 0.025(3) 0.001(3) 0.015(3) -0.015(4) C13 0.037(4) 0.065(6) 0.041(4) -0.015(4) 0.002(3) -0.018(4) C3A 0.067(6) 0.064(6) 0.033(4) -0.008(4) 0.021(4) -0.018(5) C14 0.042(4) 0.052(5) 0.040(4) 0.000(4) 0.008(3) -0.016(4) C2A 0.043(5) 0.067(6) 0.048(5) -0.007(4) 0.016(4) -0.011(4) C15 0.039(4) 0.046(5) 0.032(4) 0.003(3) 0.010(3) -0.010(4) C1A 0.043(4) 0.054(5) 0.029(4) -0.006(4) 0.004(3) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.995(5) . ? Cu1 N1 2.010(5) . ? Cu1 N2 2.020(5) . ? Cu1 N3 2.034(5) . ? Cu1 O2 2.498(6) . ? Cu1 O7 2.891(7) . ? N1 C5 1.337(8) . ? N1 C1 1.360(8) . ? N2 C6 1.478(7) . ? N2 C7 1.480(8) . ? N3 C10 1.483(8) . ? N3 C9 1.483(9) . ? N4 C15 1.337(8) . ? N4 C11 1.372(7) . ? O2 Cl1 1.436(6) . ? Cu1A N1A 1.999(5) . ? Cu1A N4A 2.016(5) . ? Cu1A N3A 2.021(6) . ? Cu1A N2A 2.028(6) . ? Cu1A O2A 2.527(6) . ? Cu1A O7A 2.819(6) . ? N4A C11A 1.353(8) . ? N4A C15A 1.364(9) . ? N3A C9A 1.390(9) . ? N3A C10A 1.492(9) . ? N2A C7A 1.476(10) . ? N2A C6A 1.479(8) . ? N1A C1A 1.325(9) . ? N1A C5A 1.365(8) . ? O2A Cl1A 1.425(6) . ? Cl1 O4 1.365(7) . ? Cl1 O5 1.415(6) . ? Cl1 O3 1.487(8) . ? Cl1A O3A 1.435(5) . ? Cl1A O4A 1.445(5) . ? Cl1A O5A 1.448(5) . ? Cl2 O8 1.384(8) . ? Cl2 O6 1.410(6) . ? Cl2 O7 1.440(6) . ? Cl2 O9 1.451(8) . ? Cl2A O9A 1.416(5) . ? Cl2A O6A 1.427(6) . ? Cl2A O8A 1.429(6) . ? Cl2A O7A 1.447(5) . ? O1 C8 1.423(8) . ? O1A C8A 1.429(9) . ? C1 C2 1.385(9) . ? C15A C14A 1.377(9) . ? C2 C3 1.380(9) . ? C14A C13A 1.395(10) . ? C3 C4 1.396(9) . ? C13A C12A 1.369(10) . ? C4 C5 1.407(8) . ? C12A C11A 1.404(9) . ? C5 C6 1.499(9) . ? C11A C10A 1.513(11) . ? C7 C8 1.529(9) . ? C9A C8A 1.528(10) . ? C8 C9 1.505(10) . ? C8A C7A 1.474(11) . ? C10 C11 1.518(9) . ? C6A C5A 1.508(9) . ? C11 C12 1.365(10) . ? C5A C4A 1.375(9) . ? C12 C13 1.386(10) . ? C4A C3A 1.378(11) . ? C13 C14 1.371(10) . ? C3A C2A 1.369(11) . ? C14 C15 1.386(9) . ? C2A C1A 1.390(10) . ? 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 N4 Cu1 N1 104.3(2) . . ? N4 Cu1 N2 160.2(2) . . ? N1 Cu1 N2 83.5(2) . . ? N4 Cu1 N3 84.9(2) . . ? N1 Cu1 N3 164.2(3) . . ? N2 Cu1 N3 92.0(2) . . ? N4 Cu1 O2 85.7(2) . . ? N1 Cu1 O2 85.7(2) . . ? N2 Cu1 O2 113.2(2) . . ? N3 Cu1 O2 82.0(2) . . ? N4 Cu1 O7 84.4(2) . . ? N1 Cu1 O7 81.74(19) . . ? N2 Cu1 O7 78.8(2) . . ? N3 Cu1 O7 112.4(2) . . ? O2 Cu1 O7 161.64(19) . . ? C5 N1 C1 119.3(6) . . ? C5 N1 Cu1 113.6(4) . . ? C1 N1 Cu1 126.7(4) . . ? C6 N2 C7 112.8(5) . . ? C6 N2 Cu1 108.8(4) . . ? C7 N2 Cu1 114.6(4) . . ? C10 N3 C9 115.1(6) . . ? C10 N3 Cu1 107.5(4) . . ? C9 N3 Cu1 114.9(4) . . ? C15 N4 C11 117.6(6) . . ? C15 N4 Cu1 127.7(4) . . ? C11 N4 Cu1 113.7(4) . . ? Cl1 O2 Cu1 120.3(3) . . ? N1A Cu1A N4A 103.7(2) . . ? N1A Cu1A N3A 165.8(3) . . ? N4A Cu1A N3A 84.8(2) . . ? N1A Cu1A N2A 84.0(2) . . ? N4A Cu1A N2A 162.6(2) . . ? N3A Cu1A N2A 91.1(2) . . ? N1A Cu1A O2A 82.7(2) . . ? N4A Cu1A O2A 89.1(2) . . ? N3A Cu1A O2A 86.1(3) . . ? N2A Cu1A O2A 107.5(2) . . ? N1A Cu1A O7A 89.9(2) . . ? N4A Cu1A O7A 81.6(2) . . ? N3A Cu1A O7A 102.7(3) . . ? N2A Cu1A O7A 82.8(2) . . ? O2A Cu1A O7A 166.46(18) . . ? C11A N4A C15A 119.0(6) . . ? C11A N4A Cu1A 113.3(5) . . ? C15A N4A Cu1A 127.7(4) . . ? C9A N3A C10A 115.7(6) . . ? C9A N3A Cu1A 115.1(6) . . ? C10A N3A Cu1A 108.3(5) . . ? C7A N2A C6A 112.7(6) . . ? C7A N2A Cu1A 115.9(5) . . ? C6A N2A Cu1A 108.5(4) . . ? C1A N1A C5A 118.4(6) . . ? C1A N1A Cu1A 128.3(5) . . ? C5A N1A Cu1A 113.3(4) . . ? Cl1A O2A Cu1A 131.6(4) . . ? O4 Cl1 O5 118.8(5) . . ? O4 Cl1 O2 110.5(5) . . ? O5 Cl1 O2 108.7(4) . . ? O4 Cl1 O3 109.1(5) . . ? O5 Cl1 O3 105.2(5) . . ? O2 Cl1 O3 103.3(5) . . ? O2A Cl1A O3A 111.4(4) . . ? O2A Cl1A O4A 109.5(4) . . ? O3A Cl1A O4A 107.6(3) . . ? O2A Cl1A O5A 110.4(4) . . ? O3A Cl1A O5A 110.5(3) . . ? O4A Cl1A O5A 107.4(3) . . ? O8 Cl2 O6 112.1(5) . . ? O8 Cl2 O7 116.9(5) . . ? O6 Cl2 O7 108.6(4) . . ? O8 Cl2 O9 108.1(7) . . ? O6 Cl2 O9 105.7(5) . . ? O7 Cl2 O9 104.7(5) . . ? O9A Cl2A O6A 108.4(4) . . ? O9A Cl2A O8A 109.6(4) . . ? O6A Cl2A O8A 109.8(4) . . ? O9A Cl2A O7A 108.4(4) . . ? O6A Cl2A O7A 110.0(3) . . ? O8A Cl2A O7A 110.7(4) . . ? Cl2A O7A Cu1A 128.6(3) . . ? Cl2 O7 Cu1 121.7(4) . . ? N1 C1 C2 121.6(6) . . ? N4A C15A C14A 121.9(6) . . ? C3 C2 C1 119.7(6) . . ? C15A C14A C13A 119.2(7) . . ? C2 C3 C4 119.0(6) . . ? C12A C13A C14A 119.3(7) . . ? C3 C4 C5 118.7(6) . . ? C13A C12A C11A 119.7(6) . . ? N1 C5 C4 121.7(6) . . ? N1 C5 C6 116.4(5) . . ? C4 C5 C6 121.9(6) . . ? N4A C11A C12A 120.9(7) . . ? N4A C11A C10A 116.2(6) . . ? C12A C11A C10A 122.8(6) . . ? N2 C6 C5 110.9(5) . . ? N3A C10A C11A 112.4(6) . . ? N2 C7 C8 113.0(5) . . ? N3A C9A C8A 115.5(7) . . ? O1 C8 C9 106.6(6) . . ? O1 C8 C7 111.2(6) . . ? C9 C8 C7 115.9(6) . . ? O1A C8A C7A 105.9(7) . . ? O1A C8A C9A 108.5(7) . . ? C7A C8A C9A 114.9(7) . . ? N3 C9 C8 113.0(6) . . ? C8A C7A N2A 116.2(7) . . ? N3 C10 C11 112.1(5) . . ? N2A C6A C5A 112.1(6) . . ? C12 C11 N4 122.5(6) . . ? C12 C11 C10 123.3(6) . . ? N4 C11 C10 114.2(6) . . ? N1A C5A C4A 122.0(7) . . ? N1A C5A C6A 116.3(6) . . ? C4A C5A C6A 121.7(6) . . ? C11 C12 C13 119.1(6) . . ? C5A C4A C3A 118.8(7) . . ? C14 C13 C12 118.9(7) . . ? C2A C3A C4A 119.4(7) . . ? C13 C14 C15 119.6(7) . . ? C3A C2A C1A 119.2(8) . . ? N4 C15 C14 122.3(6) . . ? N1A C1A C2A 122.1(7) . . ? 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 N4 Cu1 N1 C5 -155.0(5) . . . . ? N2 Cu1 N1 C5 6.6(5) . . . . ? N3 Cu1 N1 C5 80.9(10) . . . . ? O2 Cu1 N1 C5 120.5(5) . . . . ? O7 Cu1 N1 C5 -72.9(5) . . . . ? N4 Cu1 N1 C1 32.9(6) . . . . ? N2 Cu1 N1 C1 -165.5(6) . . . . ? N3 Cu1 N1 C1 -91.2(10) . . . . ? O2 Cu1 N1 C1 -51.6(6) . . . . ? O7 Cu1 N1 C1 115.0(6) . . . . ? N4 Cu1 N2 C6 95.6(7) . . . . ? N1 Cu1 N2 C6 -19.2(5) . . . . ? N3 Cu1 N2 C6 176.0(5) . . . . ? O2 Cu1 N2 C6 -101.7(5) . . . . ? O7 Cu1 N2 C6 63.6(4) . . . . ? N4 Cu1 N2 C7 -31.8(8) . . . . ? N1 Cu1 N2 C7 -146.5(5) . . . . ? N3 Cu1 N2 C7 48.7(5) . . . . ? O2 Cu1 N2 C7 130.9(4) . . . . ? O7 Cu1 N2 C7 -63.7(4) . . . . ? N4 Cu1 N3 C10 -17.4(5) . . . . ? N1 Cu1 N3 C10 108.9(8) . . . . ? N2 Cu1 N3 C10 -177.9(5) . . . . ? O2 Cu1 N3 C10 68.9(5) . . . . ? O7 Cu1 N3 C10 -99.2(5) . . . . ? N4 Cu1 N3 C9 112.1(5) . . . . ? N1 Cu1 N3 C9 -121.5(8) . . . . ? N2 Cu1 N3 C9 -48.4(5) . . . . ? O2 Cu1 N3 C9 -161.5(5) . . . . ? O7 Cu1 N3 C9 30.3(5) . . . . ? N1 Cu1 N4 C15 27.0(6) . . . . ? N2 Cu1 N4 C15 -84.4(8) . . . . ? N3 Cu1 N4 C15 -166.1(6) . . . . ? O2 Cu1 N4 C15 111.6(6) . . . . ? O7 Cu1 N4 C15 -52.9(6) . . . . ? N1 Cu1 N4 C11 -164.5(5) . . . . ? N2 Cu1 N4 C11 84.1(8) . . . . ? N3 Cu1 N4 C11 2.4(5) . . . . ? O2 Cu1 N4 C11 -80.0(5) . . . . ? O7 Cu1 N4 C11 115.5(5) . . . . ? N4 Cu1 O2 Cl1 177.6(4) . . . . ? N1 Cu1 O2 Cl1 -77.7(4) . . . . ? N2 Cu1 O2 Cl1 3.4(5) . . . . ? N3 Cu1 O2 Cl1 92.1(4) . . . . ? O7 Cu1 O2 Cl1 -124.8(5) . . . . ? N1A Cu1A N4A C11A -161.4(5) . . . . ? N3A Cu1A N4A C11A 7.0(5) . . . . ? N2A Cu1A N4A C11A 83.9(9) . . . . ? O2A Cu1A N4A C11A -79.1(5) . . . . ? O7A Cu1A N4A C11A 110.8(5) . . . . ? N1A Cu1A N4A C15A 22.0(6) . . . . ? N3A Cu1A N4A C15A -169.6(6) . . . . ? N2A Cu1A N4A C15A -92.7(9) . . . . ? O2A Cu1A N4A C15A 104.3(6) . . . . ? O7A Cu1A N4A C15A -65.9(6) . . . . ? N1A Cu1A N3A C9A -118.4(11) . . . . ? N4A Cu1A N3A C9A 114.1(6) . . . . ? N2A Cu1A N3A C9A -48.9(6) . . . . ? O2A Cu1A N3A C9A -156.5(6) . . . . ? O7A Cu1A N3A C9A 33.9(6) . . . . ? N1A Cu1A N3A C10A 110.3(10) . . . . ? N4A Cu1A N3A C10A -17.2(6) . . . . ? N2A Cu1A N3A C10A 179.7(6) . . . . ? O2A Cu1A N3A C10A 72.2(6) . . . . ? O7A Cu1A N3A C10A -97.4(6) . . . . ? N1A Cu1A N2A C7A -149.1(6) . . . . ? N4A Cu1A N2A C7A -31.7(11) . . . . ? N3A Cu1A N2A C7A 44.3(6) . . . . ? O2A Cu1A N2A C7A 130.5(6) . . . . ? O7A Cu1A N2A C7A -58.4(6) . . . . ? N1A Cu1A N2A C6A -21.1(5) . . . . ? N4A Cu1A N2A C6A 96.4(9) . . . . ? N3A Cu1A N2A C6A 172.3(5) . . . . ? O2A Cu1A N2A C6A -101.5(5) . . . . ? O7A Cu1A N2A C6A 69.6(5) . . . . ? N4A Cu1A N1A C1A 28.1(7) . . . . ? N3A Cu1A N1A C1A -97.5(11) . . . . ? N2A Cu1A N1A C1A -167.8(7) . . . . ? O2A Cu1A N1A C1A -59.2(7) . . . . ? O7A Cu1A N1A C1A 109.4(7) . . . . ? N4A Cu1A N1A C5A -150.3(5) . . . . ? N3A Cu1A N1A C5A 84.2(11) . . . . ? N2A Cu1A N1A C5A 13.9(5) . . . . ? O2A Cu1A N1A C5A 122.5(5) . . . . ? O7A Cu1A N1A C5A -68.9(5) . . . . ? N1A Cu1A O2A Cl1A -131.5(6) . . . . ? N4A Cu1A O2A Cl1A 124.5(6) . . . . ? N3A Cu1A O2A Cl1A 39.7(6) . . . . ? N2A Cu1A O2A Cl1A -50.2(6) . . . . ? O7A Cu1A O2A Cl1A 170.9(5) . . . . ? Cu1 O2 Cl1 O4 -161.6(5) . . . . ? Cu1 O2 Cl1 O5 -29.5(5) . . . . ? Cu1 O2 Cl1 O3 81.9(5) . . . . ? Cu1A O2A Cl1A O3A 124.3(5) . . . . ? Cu1A O2A Cl1A O4A -116.9(5) . . . . ? Cu1A O2A Cl1A O5A 1.2(6) . . . . ? O9A Cl2A O7A Cu1A 89.9(5) . . . . ? O6A Cl2A O7A Cu1A -28.5(5) . . . . ? O8A Cl2A O7A Cu1A -150.0(4) . . . . ? N1A Cu1A O7A Cl2A -16.2(4) . . . . ? N4A Cu1A O7A Cl2A 87.7(4) . . . . ? N3A Cu1A O7A Cl2A 170.4(4) . . . . ? N2A Cu1A O7A Cl2A -100.2(4) . . . . ? O2A Cu1A O7A Cl2A 40.6(10) . . . . ? O8 Cl2 O7 Cu1 -148.1(6) . . . . ? O6 Cl2 O7 Cu1 -20.1(6) . . . . ? O9 Cl2 O7 Cu1 92.4(5) . . . . ? N4 Cu1 O7 Cl2 -40.5(4) . . . . ? N1 Cu1 O7 Cl2 -145.9(5) . . . . ? N2 Cu1 O7 Cl2 129.2(5) . . . . ? N3 Cu1 O7 Cl2 41.6(5) . . . . ? O2 Cu1 O7 Cl2 -98.3(7) . . . . ? C5 N1 C1 C2 1.6(10) . . . . ? Cu1 N1 C1 C2 173.3(5) . . . . ? C11A N4A C15A C14A 1.5(10) . . . . ? Cu1A N4A C15A C14A 178.0(5) . . . . ? N1 C1 C2 C3 -2.9(11) . . . . ? N4A C15A C14A C13A -0.6(11) . . . . ? C1 C2 C3 C4 1.9(11) . . . . ? C15A C14A C13A C12A -1.0(11) . . . . ? C2 C3 C4 C5 0.2(11) . . . . ? C14A C13A C12A C11A 1.6(11) . . . . ? C1 N1 C5 C4 0.6(10) . . . . ? Cu1 N1 C5 C4 -172.2(5) . . . . ? C1 N1 C5 C6 -179.1(6) . . . . ? Cu1 N1 C5 C6 8.1(8) . . . . ? C3 C4 C5 N1 -1.5(11) . . . . ? C3 C4 C5 C6 178.2(7) . . . . ? C15A N4A C11A C12A -0.8(10) . . . . ? Cu1A N4A C11A C12A -177.7(6) . . . . ? C15A N4A C11A C10A -177.7(7) . . . . ? Cu1A N4A C11A C10A 5.3(8) . . . . ? C13A C12A C11A N4A -0.8(11) . . . . ? C13A C12A C11A C10A 175.9(8) . . . . ? C7 N2 C6 C5 156.2(6) . . . . ? Cu1 N2 C6 C5 27.8(7) . . . . ? N1 C5 C6 N2 -24.5(9) . . . . ? C4 C5 C6 N2 155.8(6) . . . . ? C9A N3A C10A C11A -106.8(9) . . . . ? Cu1A N3A C10A C11A 24.1(9) . . . . ? N4A C11A C10A N3A -20.2(11) . . . . ? C12A C11A C10A N3A 163.0(7) . . . . ? C6 N2 C7 C8 174.1(6) . . . . ? Cu1 N2 C7 C8 -60.6(7) . . . . ? C10A N3A C9A C8A -169.4(7) . . . . ? Cu1A N3A C9A C8A 62.9(9) . . . . ? N2 C7 C8 O1 -57.7(8) . . . . ? N2 C7 C8 C9 64.3(9) . . . . ? N3A C9A C8A O1A 55.7(10) . . . . ? N3A C9A C8A C7A -62.6(11) . . . . ? C10 N3 C9 C8 -174.3(6) . . . . ? Cu1 N3 C9 C8 60.0(7) . . . . ? O1 C8 C9 N3 60.6(7) . . . . ? C7 C8 C9 N3 -63.8(9) . . . . ? O1A C8A C7A N2A -62.4(9) . . . . ? C9A C8A C7A N2A 57.4(11) . . . . ? C6A N2A C7A C8A 179.2(7) . . . . ? Cu1A N2A C7A C8A -54.9(10) . . . . ? C9 N3 C10 C11 -100.6(7) . . . . ? Cu1 N3 C10 C11 28.8(7) . . . . ? C7A N2A C6A C5A 154.4(7) . . . . ? Cu1A N2A C6A C5A 24.6(7) . . . . ? C15 N4 C11 C12 0.3(10) . . . . ? Cu1 N4 C11 C12 -169.4(6) . . . . ? C15 N4 C11 C10 -176.7(6) . . . . ? Cu1 N4 C11 C10 13.6(7) . . . . ? N3 C10 C11 C12 154.1(7) . . . . ? N3 C10 C11 N4 -28.9(9) . . . . ? C1A N1A C5A C4A -2.4(10) . . . . ? Cu1A N1A C5A C4A 176.1(5) . . . . ? C1A N1A C5A C6A 178.4(7) . . . . ? Cu1A N1A C5A C6A -3.1(8) . . . . ? N2A C6A C5A N1A -14.8(9) . . . . ? N2A C6A C5A C4A 165.9(6) . . . . ? N4 C11 C12 C13 -0.9(12) . . . . ? C10 C11 C12 C13 175.8(7) . . . . ? N1A C5A C4A C3A 0.1(11) . . . . ? C6A C5A C4A C3A 179.3(7) . . . . ? C11 C12 C13 C14 -0.3(12) . . . . ? C5A C4A C3A C2A 1.1(12) . . . . ? C12 C13 C14 C15 2.0(12) . . . . ? C4A C3A C2A C1A 0.0(12) . . . . ? C11 N4 C15 C14 1.5(11) . . . . ? Cu1 N4 C15 C14 169.6(6) . . . . ? C13 C14 C15 N4 -2.7(12) . . . . ? C5A N1A C1A C2A 3.6(11) . . . . ? Cu1A N1A C1A C2A -174.7(6) . . . . ? C3A C2A C1A N1A -2.4(12) . . . . ? 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 N3A H3AA O5A 0.93 2.21 3.068(10) 152.3 . N2A H2AA O9A 0.93 2.34 3.153(8) 146.4 2_745 O1 H1A O6A 0.84 2.26 3.099(9) 173.7 1_455 O1A H1AA O9 0.84 1.95 2.786(10) 176.1 1_545 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.350 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.116 data_[Cu2(H-1bpdpo)(DPP)(CH3OH)(ClO4)]ClO4 _database_code_CSD 163303 _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu(1,1)-(N,N'-bis(2-pyridylmethyl)-1,3-diaminopropane-2-alkoxo) mu(1,3)-diphenilphosphato dicopper(II) diperchlorate ; _chemical_name_common '[Cu2(H-1bpdpo)(DPP)(CH3OH)(ClO4)]ClO4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H33 Cl2 Cu2 N4 O14 P' _chemical_formula_weight 878.53 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' 'P' 'P' 0.1023 0.0942 '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 P21/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 7.2856(15) _cell_length_b 32.789(7) _cell_length_c 15.008(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.70(3) _cell_angle_gamma 90.00 _cell_volume 3583.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.27 _cell_measurement_theta_max 25.6 _exptl_crystal_description needles _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IDPS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 270 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27024 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.60 _reflns_number_total 6583 _reflns_number_gt 5117 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0605P)^2^+8.2874P] 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 6583 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.22607(8) 0.561100(19) 0.22640(3) 0.04611(18) Uani 1 1 d . . . Cu2 Cu 0.33672(8) 0.626881(18) 0.40359(4) 0.04607(18) Uani 1 1 d . . . N1 N 0.2319(6) 0.53261(15) 0.1097(3) 0.0548(11) Uani 1 1 d . . . N2 N 0.2115(6) 0.50442(13) 0.2728(3) 0.0550(10) Uani 1 1 d . . . H2B H 0.0889 0.4967 0.2742 0.066 Uiso 1 1 calc R . . N3 N 0.3558(6) 0.59482(13) 0.5159(3) 0.0508(10) Uani 1 1 d . . . H3B H 0.2473 0.5983 0.5460 0.061 Uiso 1 1 calc R . . N4 N 0.4443(6) 0.67023(13) 0.4805(3) 0.0572(11) Uani 1 1 d . . . O1 O 0.2635(4) 0.57700(10) 0.3483(2) 0.0460(7) Uani 1 1 d . . . P1 P 0.3085(2) 0.65410(4) 0.20220(9) 0.0616(4) Uani 1 1 d . . . O2 O 0.2252(5) 0.61537(12) 0.1728(2) 0.0601(9) Uani 1 1 d . . . O3 O 0.3566(6) 0.66039(11) 0.2979(2) 0.0620(10) Uani 1 1 d . . . O4 O 0.4911(7) 0.66259(13) 0.1505(3) 0.0841(14) Uani 1 1 d . . . O5 O 0.1946(12) 0.6917(2) 0.1672(3) 0.152(3) Uani 1 1 d . . . C1 C 0.2056(8) 0.5487(2) 0.0282(3) 0.0666(15) Uani 1 1 d . . . H1A H 0.1773 0.5769 0.0230 0.080 Uiso 1 1 calc R . . C2 C 0.2181(9) 0.5257(3) -0.0486(4) 0.083(2) Uani 1 1 d . . . H2A H 0.1983 0.5378 -0.1056 0.100 Uiso 1 1 calc R . . C3 C 0.2590(10) 0.4859(3) -0.0407(5) 0.095(3) Uani 1 1 d . . . H3A H 0.2689 0.4697 -0.0928 0.114 Uiso 1 1 calc R . . C4 C 0.2868(9) 0.4683(2) 0.0422(5) 0.082(2) Uani 1 1 d . . . H4A H 0.3154 0.4401 0.0480 0.098 Uiso 1 1 calc R . . C5 C 0.2718(7) 0.4929(2) 0.1168(4) 0.0622(14) Uani 1 1 d . . . C6 C 0.3079(8) 0.47732(18) 0.2106(4) 0.0654(14) Uani 1 1 d . . . H6A H 0.2620 0.4490 0.2161 0.079 Uiso 1 1 calc R . . H6B H 0.4414 0.4774 0.2250 0.079 Uiso 1 1 calc R . . C7 C 0.2905(8) 0.50433(16) 0.3652(3) 0.0581(13) Uani 1 1 d . . . H7B H 0.4257 0.5013 0.3641 0.070 Uiso 1 1 calc R . . H7C H 0.2405 0.4811 0.3990 0.070 Uiso 1 1 calc R . . C8 C 0.2410(7) 0.54442(16) 0.4100(3) 0.0506(11) Uani 1 1 d . . . H8A H 0.1108 0.5435 0.4291 0.061 Uiso 1 1 calc R . . C9 C 0.3691(7) 0.55167(15) 0.4908(3) 0.0509(12) Uani 1 1 d . . . H9A H 0.3328 0.5341 0.5410 0.061 Uiso 1 1 calc R . . H9B H 0.4970 0.5449 0.4759 0.061 Uiso 1 1 calc R . . C10 C 0.5060(8) 0.61142(17) 0.5715(4) 0.0591(13) Uani 1 1 d . . . H10A H 0.6243 0.5994 0.5539 0.071 Uiso 1 1 calc R . . H10B H 0.4871 0.6047 0.6349 0.071 Uiso 1 1 calc R . . C11 C 0.5099(8) 0.65690(17) 0.5593(4) 0.0581(13) Uani 1 1 d . . . C12 C 0.5823(10) 0.6844(2) 0.6218(5) 0.0822(19) Uani 1 1 d . . . H12A H 0.6290 0.6750 0.6779 0.099 Uiso 1 1 calc R . . C13 C 0.5856(13) 0.7250(2) 0.6016(6) 0.098(2) Uani 1 1 d . . . H13A H 0.6330 0.7441 0.6439 0.117 Uiso 1 1 calc R . . C14 C 0.5206(13) 0.7379(2) 0.5206(6) 0.096(2) Uani 1 1 d . . . H14A H 0.5252 0.7660 0.5050 0.116 Uiso 1 1 calc R . . C15 C 0.4487(10) 0.70998(18) 0.4620(4) 0.0757(17) Uani 1 1 d . . . H15A H 0.4000 0.7192 0.4061 0.091 Uiso 1 1 calc R . . C16 C 0.5208(11) 0.65436(16) 0.0610(4) 0.0723(19) Uani 1 1 d . . . C17 C 0.3826(12) 0.6546(2) -0.0029(4) 0.085(2) Uani 1 1 d . . . H17A H 0.2589 0.6589 0.0129 0.102 Uiso 1 1 calc R . . C18 C 0.4266(15) 0.6483(2) -0.0913(5) 0.100(3) Uani 1 1 d . . . H18A H 0.3328 0.6485 -0.1366 0.120 Uiso 1 1 calc R . . C19 C 0.6043(16) 0.6417(2) -0.1129(5) 0.104(3) Uani 1 1 d . . . H19A H 0.6341 0.6375 -0.1734 0.125 Uiso 1 1 calc R . . C20 C 0.7401(15) 0.6413(3) -0.0482(6) 0.110(3) Uani 1 1 d . . . H20A H 0.8635 0.6365 -0.0642 0.132 Uiso 1 1 calc R . . C21 C 0.7006(12) 0.6475(2) 0.0391(5) 0.086(2) Uani 1 1 d . . . H21A H 0.7954 0.6472 0.0839 0.104 Uiso 1 1 calc R . . C22 C 0.0709(8) 0.71357(15) 0.2150(3) 0.0561(13) Uani 1 1 d . . . C23 C -0.0732(12) 0.6951(3) 0.2458(5) 0.095(2) Uani 1 1 d . . . H23A H -0.0835 0.6665 0.2359 0.115 Uiso 1 1 calc R . . C24 C -0.2040(14) 0.7128(3) 0.2890(6) 0.110(3) Uani 1 1 d . . . H24A H -0.3108 0.6986 0.3063 0.132 Uiso 1 1 calc R . . C25 C -0.1776(15) 0.7533(3) 0.3078(6) 0.106(3) Uani 1 1 d . . . H25A H -0.2682 0.7662 0.3423 0.127 Uiso 1 1 calc R . . C26 C -0.0361(15) 0.7768(3) 0.2825(6) 0.112(3) Uani 1 1 d . . . H26A H -0.0240 0.8048 0.2981 0.135 Uiso 1 1 calc R . . C27 C 0.0979(14) 0.7549(3) 0.2283(7) 0.121(3) Uani 1 1 d . . . H27A H 0.1990 0.7687 0.2034 0.145 Uiso 1 1 calc R . . C28 C -0.0296(13) 0.6732(3) 0.4868(6) 0.123(3) Uani 1 1 d . . . H28A H -0.1638 0.6721 0.4888 0.185 Uiso 1 1 calc R . . H28B H 0.0078 0.6992 0.4608 0.185 Uiso 1 1 calc R . . H28C H 0.0233 0.6708 0.5474 0.185 Uiso 1 1 calc R . . Cl1 Cl -0.25845(16) 0.56539(4) 0.28645(9) 0.0582(3) Uani 1 1 d . . . O7 O -0.4178(5) 0.55991(16) 0.2301(3) 0.0836(14) Uani 1 1 d . . . O6 O -0.2226(8) 0.53160(18) 0.3376(5) 0.123(2) Uani 1 1 d . . . O8 O -0.1068(6) 0.5742(2) 0.2324(3) 0.1092(19) Uani 1 1 d . . . O9 O -0.2861(7) 0.59892(17) 0.3454(4) 0.1040(17) Uani 1 1 d . . . O10 O 0.0323(6) 0.64154(15) 0.4352(3) 0.0838(13) Uani 1 1 d . . . H4C H -0.0577 0.6299 0.4099 0.101 Uiso 1 1 calc R . . Cl2 Cl 0.0473(2) 0.59879(6) 0.70966(11) 0.0795(5) Uani 1 1 d . . . O11 O 0.1760(8) 0.6291(2) 0.6904(4) 0.116(2) Uani 1 1 d . A . O13 O 0.051(2) 0.5896(13) 0.7976(14) 0.193(18) Uani 0.51(2) 1 d P A 1 O14 O -0.1366(14) 0.6143(5) 0.6995(12) 0.106(6) Uani 0.51(2) 1 d P A 1 O12 O 0.065(5) 0.5665(8) 0.662(3) 0.22(2) Uani 0.51(2) 1 d P A 1 O12A O 0.130(4) 0.5649(8) 0.738(2) 0.189(13) Uani 0.49(2) 1 d P A 2 O13A O -0.056(7) 0.6109(7) 0.772(3) 0.28(3) Uani 0.49(2) 1 d P A 2 O14A O -0.020(3) 0.5837(9) 0.6264(12) 0.154(12) Uani 0.49(2) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0371(3) 0.0629(4) 0.0381(3) 0.0049(2) -0.0012(2) -0.0043(3) Cu2 0.0500(4) 0.0491(3) 0.0394(3) 0.0031(2) 0.0042(2) 0.0082(3) N1 0.040(2) 0.077(3) 0.047(2) -0.001(2) -0.0029(17) -0.014(2) N2 0.050(3) 0.063(3) 0.051(2) -0.0003(19) -0.0028(18) -0.015(2) N3 0.049(2) 0.063(3) 0.040(2) 0.0029(18) -0.0002(17) -0.0002(19) N4 0.062(3) 0.054(3) 0.056(2) -0.005(2) 0.010(2) 0.005(2) O1 0.0440(19) 0.0546(19) 0.0395(16) 0.0096(14) 0.0003(13) 0.0019(14) P1 0.0884(11) 0.0556(8) 0.0417(7) 0.0099(6) 0.0172(7) 0.0258(7) O2 0.053(2) 0.082(3) 0.0450(18) 0.0225(17) -0.0010(15) -0.0010(18) O3 0.089(3) 0.049(2) 0.0485(19) 0.0013(15) 0.0133(18) 0.0133(18) O4 0.130(4) 0.076(3) 0.048(2) -0.0134(19) 0.030(2) -0.041(3) O5 0.242(8) 0.157(6) 0.057(3) 0.018(3) 0.015(4) 0.141(6) C1 0.054(3) 0.100(5) 0.045(3) 0.002(3) -0.008(2) -0.016(3) C2 0.062(4) 0.138(7) 0.050(3) -0.004(4) -0.005(3) -0.017(4) C3 0.064(4) 0.156(8) 0.066(4) -0.042(5) 0.004(3) -0.025(5) C4 0.070(4) 0.100(5) 0.076(4) -0.034(4) 0.005(3) -0.022(4) C5 0.043(3) 0.084(4) 0.060(3) -0.010(3) 0.001(2) -0.021(3) C6 0.060(4) 0.064(3) 0.073(4) -0.007(3) 0.005(3) -0.012(3) C7 0.067(4) 0.055(3) 0.051(3) 0.009(2) -0.013(2) -0.013(3) C8 0.046(3) 0.060(3) 0.046(3) 0.012(2) 0.002(2) -0.007(2) C9 0.055(3) 0.055(3) 0.043(2) 0.011(2) -0.008(2) -0.002(2) C10 0.055(3) 0.072(3) 0.051(3) -0.001(2) -0.008(2) 0.000(3) C11 0.055(3) 0.063(3) 0.057(3) -0.007(2) 0.007(2) -0.006(2) C12 0.091(5) 0.087(5) 0.068(4) -0.020(3) -0.003(3) -0.002(4) C13 0.123(7) 0.073(5) 0.098(6) -0.035(4) 0.007(5) -0.007(4) C14 0.139(7) 0.054(4) 0.097(6) -0.021(4) 0.015(5) 0.000(4) C15 0.101(5) 0.056(3) 0.070(4) -0.008(3) 0.010(3) 0.010(3) C16 0.128(6) 0.047(3) 0.043(3) -0.003(2) 0.029(3) -0.030(3) C17 0.118(6) 0.079(4) 0.059(4) 0.001(3) 0.016(4) -0.016(4) C18 0.169(9) 0.080(5) 0.051(4) 0.010(3) 0.007(4) -0.024(5) C19 0.166(9) 0.088(5) 0.060(4) -0.002(4) 0.049(5) -0.017(5) C20 0.140(8) 0.112(6) 0.081(5) -0.014(5) 0.052(6) -0.016(6) C21 0.110(6) 0.082(4) 0.068(4) -0.005(3) 0.029(4) -0.026(4) C22 0.073(4) 0.043(3) 0.052(3) 0.009(2) 0.004(2) 0.013(2) C23 0.083(5) 0.115(6) 0.088(5) 0.042(5) -0.006(4) 0.001(5) C24 0.101(7) 0.113(7) 0.115(7) 0.025(5) 0.001(5) 0.019(5) C25 0.141(8) 0.077(5) 0.102(6) 0.015(4) 0.033(5) 0.025(5) C26 0.141(9) 0.081(5) 0.114(6) -0.005(5) 0.001(6) 0.055(6) C27 0.110(7) 0.118(7) 0.133(8) 0.049(6) -0.023(6) -0.021(6) C28 0.093(6) 0.173(9) 0.106(6) 0.006(6) 0.024(5) 0.065(6) Cl1 0.0306(6) 0.0771(9) 0.0669(8) -0.0105(6) 0.0010(5) -0.0025(5) O7 0.028(2) 0.145(4) 0.078(3) -0.036(3) -0.0018(17) -0.006(2) O6 0.088(4) 0.101(4) 0.179(6) 0.051(4) -0.015(4) -0.002(3) O8 0.032(2) 0.198(6) 0.098(4) 0.002(4) 0.010(2) -0.009(3) O9 0.076(3) 0.107(4) 0.128(4) -0.050(3) -0.014(3) -0.004(3) O10 0.057(3) 0.104(3) 0.091(3) -0.015(3) 0.005(2) 0.020(2) Cl2 0.0778(11) 0.0991(12) 0.0626(9) 0.0140(8) 0.0171(8) -0.0172(9) O11 0.099(4) 0.148(5) 0.104(4) -0.011(4) 0.033(3) -0.057(4) O13 0.089(11) 0.39(4) 0.101(13) 0.14(2) -0.024(10) -0.042(16) O14 0.039(6) 0.149(12) 0.130(12) 0.035(10) 0.006(6) 0.011(6) O12 0.19(3) 0.124(17) 0.36(4) -0.14(2) 0.19(3) -0.086(17) O12A 0.24(3) 0.19(2) 0.131(18) 0.000(15) -0.043(19) 0.093(19) O13A 0.42(5) 0.124(16) 0.33(4) -0.10(2) 0.34(4) -0.08(2) O14A 0.126(17) 0.24(3) 0.091(10) 0.008(13) -0.038(11) -0.058(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.914(3) . ? Cu1 O2 1.953(4) . ? Cu1 N1 1.987(4) . ? Cu1 N2 1.989(4) . ? Cu1 O8 2.468(4) . ? Cu1 O7 2.594(4) 1_655 ? Cu1 Cu2 3.4996(10) . ? Cu2 O1 1.903(3) . ? Cu2 O3 1.938(3) . ? Cu2 N4 1.978(5) . ? Cu2 N3 1.987(4) . ? Cu2 O10 2.332(4) . ? N1 C5 1.338(8) . ? N1 C1 1.340(7) . ? N2 C6 1.480(7) . ? N2 C7 1.486(6) . ? N3 C10 1.462(6) . ? N3 C9 1.468(6) . ? N4 C15 1.333(7) . ? N4 C11 1.336(7) . ? O1 C8 1.426(5) . ? P1 O2 1.470(4) . ? P1 O3 1.483(4) . ? P1 O5 1.567(5) . ? P1 O4 1.585(5) . ? O4 C16 1.393(6) . ? O5 C22 1.371(7) . ? C1 C2 1.381(9) . ? C2 C3 1.345(11) . ? C3 C4 1.382(11) . ? C4 C5 1.387(8) . ? C5 C6 1.514(8) . ? C7 C8 1.524(8) . ? C8 C9 1.527(7) . ? C10 C11 1.503(8) . ? C11 C12 1.394(8) . ? C12 C13 1.367(10) . ? C13 C14 1.359(11) . ? C14 C15 1.363(10) . ? C16 C17 1.370(10) . ? C16 C21 1.378(10) . ? C17 C18 1.389(9) . ? C18 C19 1.360(13) . ? C19 C20 1.365(13) . ? C20 C21 1.366(10) . ? C22 C23 1.309(9) . ? C22 C27 1.383(11) . ? C23 C24 1.306(11) . ? C24 C25 1.369(12) . ? C25 C26 1.350(13) . ? C26 C27 1.476(13) . ? C28 O10 1.378(9) . ? Cl1 O6 1.369(6) . ? Cl1 O8 1.419(5) . ? Cl1 O7 1.427(4) . ? Cl1 O9 1.429(5) . ? Cl2 O12 1.283(15) . ? Cl2 O13A 1.284(13) . ? Cl2 O12A 1.33(2) . ? Cl2 O13 1.354(15) . ? Cl2 O11 1.403(5) . ? Cl2 O14A 1.419(18) . ? Cl2 O14 1.437(11) . ? 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 98.28(15) . . ? O1 Cu1 N1 164.72(17) . . ? O2 Cu1 N1 93.75(18) . . ? O1 Cu1 N2 85.84(15) . . ? O2 Cu1 N2 175.10(16) . . ? N1 Cu1 N2 82.65(18) . . ? O1 Cu1 O8 91.70(16) . . ? O2 Cu1 O8 82.23(19) . . ? N1 Cu1 O8 99.27(18) . . ? N2 Cu1 O8 95.0(2) . . ? O1 Cu1 O7 82.49(13) . 1_655 ? O2 Cu1 O7 90.79(17) . 1_655 ? N1 Cu1 O7 87.98(15) . 1_655 ? N2 Cu1 O7 92.40(18) . 1_655 ? O8 Cu1 O7 170.21(19) . 1_655 ? O1 Cu1 Cu2 23.47(10) . . ? O2 Cu1 Cu2 75.47(11) . . ? N1 Cu1 Cu2 161.69(12) . . ? N2 Cu1 Cu2 108.87(12) . . ? O8 Cu1 Cu2 93.96(14) . . ? O7 Cu1 Cu2 77.59(10) 1_655 . ? O1 Cu2 O3 99.04(14) . . ? O1 Cu2 N4 166.65(16) . . ? O3 Cu2 N4 91.84(18) . . ? O1 Cu2 N3 85.80(15) . . ? O3 Cu2 N3 171.31(18) . . ? N4 Cu2 N3 82.47(18) . . ? O1 Cu2 O10 90.57(16) . . ? O3 Cu2 O10 98.29(17) . . ? N4 Cu2 O10 95.51(18) . . ? N3 Cu2 O10 88.82(18) . . ? O1 Cu2 Cu1 23.61(9) . . ? O3 Cu2 Cu1 75.45(11) . . ? N4 Cu2 Cu1 164.70(13) . . ? N3 Cu2 Cu1 109.09(12) . . ? O10 Cu2 Cu1 94.74(12) . . ? C5 N1 C1 118.7(5) . . ? C5 N1 Cu1 113.4(3) . . ? C1 N1 Cu1 127.8(4) . . ? C6 N2 C7 114.2(5) . . ? C6 N2 Cu1 108.0(3) . . ? C7 N2 Cu1 107.8(3) . . ? C10 N3 C9 116.8(4) . . ? C10 N3 Cu2 108.7(3) . . ? C9 N3 Cu2 107.2(3) . . ? C15 N4 C11 119.6(5) . . ? C15 N4 Cu2 126.4(4) . . ? C11 N4 Cu2 114.0(4) . . ? C8 O1 Cu2 113.4(3) . . ? C8 O1 Cu1 113.6(3) . . ? Cu2 O1 Cu1 132.92(17) . . ? O2 P1 O3 119.6(2) . . ? O2 P1 O5 111.7(4) . . ? O3 P1 O5 108.8(3) . . ? O2 P1 O4 110.5(2) . . ? O3 P1 O4 105.8(3) . . ? O5 P1 O4 98.2(4) . . ? P1 O2 Cu1 131.9(2) . . ? P1 O3 Cu2 133.8(2) . . ? C16 O4 P1 126.5(4) . . ? C22 O5 P1 125.9(4) . . ? N1 C1 C2 122.4(7) . . ? C3 C2 C1 118.4(7) . . ? C2 C3 C4 120.8(7) . . ? C3 C4 C5 118.0(7) . . ? N1 C5 C4 121.6(6) . . ? N1 C5 C6 115.7(5) . . ? C4 C5 C6 122.6(6) . . ? N2 C6 C5 108.2(5) . . ? N2 C7 C8 108.6(4) . . ? O1 C8 C7 109.1(4) . . ? O1 C8 C9 108.6(4) . . ? C7 C8 C9 109.7(4) . . ? N3 C9 C8 108.1(4) . . ? N3 C10 C11 108.4(4) . . ? N4 C11 C12 120.2(6) . . ? N4 C11 C10 115.2(5) . . ? C12 C11 C10 124.6(6) . . ? C13 C12 C11 119.3(7) . . ? C14 C13 C12 119.6(7) . . ? C13 C14 C15 119.1(7) . . ? N4 C15 C14 122.3(7) . . ? C17 C16 C21 121.2(6) . . ? C17 C16 O4 122.8(7) . . ? C21 C16 O4 115.9(7) . . ? C16 C17 C18 118.8(8) . . ? C19 C18 C17 119.9(9) . . ? C18 C19 C20 120.5(7) . . ? C19 C20 C21 120.8(9) . . ? C20 C21 C16 118.8(8) . . ? C23 C22 O5 119.2(7) . . ? C23 C22 C27 121.0(8) . . ? O5 C22 C27 119.7(8) . . ? C24 C23 C22 125.0(9) . . ? C23 C24 C25 115.8(10) . . ? C26 C25 C24 126.8(9) . . ? C25 C26 C27 113.6(8) . . ? C22 C27 C26 117.6(8) . . ? O6 Cl1 O8 110.3(4) . . ? O6 Cl1 O7 111.6(4) . . ? O8 Cl1 O7 108.7(3) . . ? O6 Cl1 O9 107.7(4) . . ? O8 Cl1 O9 108.8(4) . . ? O7 Cl1 O9 109.6(3) . . ? Cl1 O8 Cu1 140.2(4) . . ? C28 O10 Cu2 126.8(5) . . ? O12 Cl2 O13A 137.0(13) . . ? O12 Cl2 O12A 55(2) . . ? O13A Cl2 O12A 107(2) . . ? O12 Cl2 O13 111(2) . . ? O13A Cl2 O13 50(2) . . ? O12A Cl2 O13 60.5(13) . . ? O12 Cl2 O11 113.0(9) . . ? O13A Cl2 O11 110.0(11) . . ? O12A Cl2 O11 111.1(16) . . ? O13 Cl2 O11 111.5(12) . . ? O12 Cl2 O14A 43(2) . . ? O13A Cl2 O14A 124(3) . . ? O12A Cl2 O14A 97.5(14) . . ? O13 Cl2 O14A 141.0(17) . . ? O11 Cl2 O14A 106.4(10) . . ? O12 Cl2 O14 110.1(19) . . ? O13A Cl2 O14 53(3) . . ? O12A Cl2 O14 137.9(17) . . ? O13 Cl2 O14 100.0(11) . . ? O11 Cl2 O14 110.8(7) . . ? O14A Cl2 O14 74.4(12) . . ? 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 N2 H2B O12 0.93 2.55 3.247(19) 131.6 3_566 N2 H2B O12A 0.93 2.57 3.37(3) 143.7 3_566 N3 H3B O14A 0.93 2.37 3.27(3) 161.1 . N3 H3B O12 0.93 2.46 3.23(2) 141.1 . O10 H4C O9 0.84 2.15 2.995(7) 179.0 . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.253 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.077