Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email YMEEKIM@EWHA.AC.KR _publ_contact_author_name 'Prof Youngmee Kim' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name Y.Kim C.Kim S.Yim S.-K.Yoo data_Cu(OAc)2(btp)2 _database_code_CSD 196738 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Cu N14 O6' _chemical_formula_weight 644.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.867(3) _cell_length_b 9.304(2) _cell_length_c 10.935(4) _cell_angle_alpha 93.40(2) _cell_angle_beta 102.42(3) _cell_angle_gamma 97.11(2) _cell_volume 674.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.11 _cell_measurement_theta_max 12.71 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 331 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4 Mach-3 diffractometer' _diffrn_measurement_method 2\q-\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% negligible _diffrn_reflns_number 2882 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2647 _reflns_number_gt 2216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_reduction 'XCAD-4 (Harms, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.2530P] 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 2647 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 1.0000 0.5000 0.02869(17) Uani 1 d S . . O1 O 0.5137(3) 1.0134(2) 0.67976(17) 0.0356(4) Uani 1 d . . . O2 O 0.8065(3) 0.9434(3) 0.6809(2) 0.0515(6) Uani 1 d . . . C1 C 0.6845(5) 0.9846(3) 0.7373(3) 0.0376(7) Uani 1 d . . . C2 C 0.7283(6) 1.0058(5) 0.8782(3) 0.0603(10) Uani 1 d . . . H2A H 0.8448 0.9615 0.9127 0.090 Uiso 1 calc R . . H2B H 0.6148 0.9614 0.9073 0.090 Uiso 1 calc R . . H2C H 0.7534 1.1079 0.9047 0.090 Uiso 1 calc R . . N1 N 0.3855(3) 0.7913(2) 0.4850(2) 0.0315(5) Uani 1 d . . . C3 C 0.3407(4) 0.6906(3) 0.3840(3) 0.0344(6) Uani 1 d . . . H3 H 0.3522 0.7137 0.3041 0.041 Uiso 1 calc R . . N2 N 0.2807(4) 0.5599(3) 0.4082(2) 0.0352(5) Uani 1 d . . . N3 N 0.2850(3) 0.5767(2) 0.53333(19) 0.0292(5) Uani 1 d . . . C4 C 0.3471(4) 0.7148(3) 0.5774(2) 0.0315(6) Uani 1 d . . . H4 H 0.3613 0.7518 0.6602 0.038 Uiso 1 calc R . . C5 C 0.2329(4) 0.4591(3) 0.6020(2) 0.0300(5) Uani 1 d . . . C6 C 0.1705(4) 0.3211(3) 0.5443(3) 0.0343(6) Uani 1 d . . . H6 H 0.1566 0.3005 0.4584 0.041 Uiso 1 calc R . . C7 C 0.1296(5) 0.2148(3) 0.6214(3) 0.0411(7) Uani 1 d . . . H7 H 0.0876 0.1191 0.5873 0.049 Uiso 1 calc R . . C8 C 0.1502(5) 0.2483(3) 0.7469(3) 0.0398(7) Uani 1 d . . . H8 H 0.1242 0.1773 0.7999 0.048 Uiso 1 calc R . . C9 C 0.2116(4) 0.3926(3) 0.7921(2) 0.0322(6) Uani 1 d . . . N4 N 0.2542(3) 0.4973(2) 0.7227(2) 0.0313(5) Uani 1 d . . . N5 N 0.2340(4) 0.4382(3) 0.9205(2) 0.0363(5) Uani 1 d . . . N6 N 0.2233(5) 0.3413(3) 1.0078(3) 0.0512(7) Uani 1 d . . . C10 C 0.2474(6) 0.4276(4) 1.1098(3) 0.0556(9) Uani 1 d . . . H10 H 0.2500 0.3921 1.1877 0.067 Uiso 1 calc R . . N7 N 0.2685(5) 0.5709(3) 1.0959(2) 0.0546(7) Uani 1 d . . . C11 C 0.2601(5) 0.5735(4) 0.9752(3) 0.0439(7) Uani 1 d . . . H11 H 0.2707 0.6574 0.9336 0.053 Uiso 1 calc R . . O3 O 0.8073(6) 1.1234(4) 1.2000(3) 0.0674(8) Uani 1 d . . . H31 H 0.770(14) 1.065(10) 1.237(8) 0.20(4) Uiso 1 d . . . H32 H 0.942(10) 1.126(6) 1.235(5) 0.11(2) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0328(3) 0.0300(3) 0.0210(2) 0.00166(17) 0.00297(18) 0.00120(18) O1 0.0434(12) 0.0352(10) 0.0263(9) 0.0031(8) 0.0061(8) 0.0015(9) O2 0.0430(13) 0.0594(15) 0.0492(13) -0.0026(11) 0.0075(10) 0.0042(11) C1 0.0488(18) 0.0287(14) 0.0285(14) 0.0033(11) 0.0012(13) -0.0082(12) C2 0.073(3) 0.074(2) 0.0259(15) 0.0063(15) -0.0022(15) 0.001(2) N1 0.0373(13) 0.0303(12) 0.0245(11) -0.0001(9) 0.0031(9) 0.0029(10) C3 0.0379(15) 0.0363(15) 0.0274(13) 0.0008(11) 0.0056(11) 0.0022(12) N2 0.0453(14) 0.0342(12) 0.0239(11) -0.0032(9) 0.0062(10) 0.0031(10) N3 0.0341(12) 0.0290(11) 0.0231(10) -0.0004(8) 0.0049(9) 0.0027(9) C4 0.0376(15) 0.0303(13) 0.0241(12) -0.0004(10) 0.0043(11) 0.0013(11) C5 0.0267(13) 0.0311(13) 0.0313(13) 0.0020(10) 0.0048(10) 0.0040(10) C6 0.0350(15) 0.0338(14) 0.0322(14) -0.0055(11) 0.0070(11) 0.0025(11) C7 0.0424(17) 0.0284(14) 0.0487(17) -0.0047(12) 0.0074(14) -0.0008(12) C8 0.0474(18) 0.0300(14) 0.0418(16) 0.0059(12) 0.0116(13) 0.0005(12) C9 0.0319(14) 0.0318(14) 0.0313(13) 0.0030(11) 0.0044(11) 0.0037(11) N4 0.0355(12) 0.0272(11) 0.0290(11) -0.0001(9) 0.0045(9) 0.0026(9) N5 0.0426(14) 0.0363(12) 0.0306(12) 0.0051(10) 0.0091(10) 0.0046(10) N6 0.0661(19) 0.0504(16) 0.0388(14) 0.0161(12) 0.0138(13) 0.0050(14) C10 0.066(2) 0.068(2) 0.0332(16) 0.0110(16) 0.0125(16) 0.0067(19) N7 0.069(2) 0.0614(18) 0.0322(13) -0.0021(12) 0.0126(13) 0.0040(15) C11 0.0517(19) 0.0452(17) 0.0334(15) -0.0009(13) 0.0093(13) 0.0030(14) O3 0.069(2) 0.0669(19) 0.0735(19) 0.0144(15) 0.0228(16) 0.0226(15) _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 1.9433(19) 2_676 ? Cu1 O1 1.9433(19) . ? Cu1 N1 1.986(2) . ? Cu1 N1 1.986(2) 2_676 ? O1 C1 1.274(4) . ? O2 C1 1.226(4) . ? C1 C2 1.501(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N1 C4 1.324(3) . ? N1 C3 1.360(3) . ? C3 N2 1.296(4) . ? C3 H3 0.9300 . ? N2 N3 1.361(3) . ? N3 C4 1.329(3) . ? N3 C5 1.416(3) . ? C4 H4 0.9300 . ? C5 N4 1.318(3) . ? C5 C6 1.372(4) . ? C6 C7 1.378(4) . ? C6 H6 0.9300 . ? C7 C8 1.362(4) . ? C7 H7 0.9300 . ? C8 C9 1.384(4) . ? C8 H8 0.9300 . ? C9 N4 1.313(4) . ? C9 N5 1.412(3) . ? N5 C11 1.335(4) . ? N5 N6 1.359(3) . ? N6 C10 1.303(4) . ? C10 N7 1.344(5) . ? C10 H10 0.9300 . ? N7 C11 1.311(4) . ? C11 H11 0.9300 . ? O3 H31 0.75(9) . ? O3 H32 0.92(6) . ? 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 O1 180.0 2_676 . ? O1 Cu1 N1 89.40(9) 2_676 . ? O1 Cu1 N1 90.60(9) . . ? O1 Cu1 N1 90.60(9) 2_676 2_676 ? O1 Cu1 N1 89.40(9) . 2_676 ? N1 Cu1 N1 180.0 . 2_676 ? C1 O1 Cu1 109.27(18) . . ? O2 C1 O1 122.0(3) . . ? O2 C1 C2 122.0(3) . . ? O1 C1 C2 116.0(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 N1 C3 103.2(2) . . ? C4 N1 Cu1 126.44(18) . . ? C3 N1 Cu1 130.20(19) . . ? N2 C3 N1 114.6(2) . . ? N2 C3 H3 122.7 . . ? N1 C3 H3 122.7 . . ? C3 N2 N3 102.7(2) . . ? C4 N3 N2 110.2(2) . . ? C4 N3 C5 127.2(2) . . ? N2 N3 C5 122.6(2) . . ? N1 C4 N3 109.3(2) . . ? N1 C4 H4 125.3 . . ? N3 C4 H4 125.3 . . ? N4 C5 C6 125.6(3) . . ? N4 C5 N3 113.1(2) . . ? C6 C5 N3 121.2(2) . . ? C5 C6 C7 116.0(3) . . ? C5 C6 H6 122.0 . . ? C7 C6 H6 122.0 . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 117.1(3) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? N4 C9 C8 124.4(3) . . ? N4 C9 N5 114.4(2) . . ? C8 C9 N5 121.2(2) . . ? C9 N4 C5 116.2(2) . . ? C11 N5 N6 109.7(3) . . ? C11 N5 C9 128.5(2) . . ? N6 N5 C9 121.7(2) . . ? C10 N6 N5 101.5(3) . . ? N6 C10 N7 116.2(3) . . ? N6 C10 H10 121.9 . . ? N7 C10 H10 121.9 . . ? C11 N7 C10 102.3(3) . . ? N7 C11 N5 110.2(3) . . ? N7 C11 H11 124.9 . . ? N5 C11 H11 124.9 . . ? H31 O3 H32 97(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 O1 Cu1 O1 C1 33(100) 2_676 . . . ? N1 Cu1 O1 C1 90.54(18) . . . . ? N1 Cu1 O1 C1 -89.46(18) 2_676 . . . ? Cu1 O1 C1 O2 -5.6(3) . . . . ? Cu1 O1 C1 C2 173.6(2) . . . . ? O1 Cu1 N1 C4 180.0(2) 2_676 . . . ? O1 Cu1 N1 C4 0.0(2) . . . . ? N1 Cu1 N1 C4 66(100) 2_676 . . . ? O1 Cu1 N1 C3 5.0(2) 2_676 . . . ? O1 Cu1 N1 C3 -175.0(2) . . . . ? N1 Cu1 N1 C3 -109(100) 2_676 . . . ? C4 N1 C3 N2 -0.7(3) . . . . ? Cu1 N1 C3 N2 175.2(2) . . . . ? N1 C3 N2 N3 0.6(3) . . . . ? C3 N2 N3 C4 -0.2(3) . . . . ? C3 N2 N3 C5 -179.0(2) . . . . ? C3 N1 C4 N3 0.5(3) . . . . ? Cu1 N1 C4 N3 -175.58(17) . . . . ? N2 N3 C4 N1 -0.2(3) . . . . ? C5 N3 C4 N1 178.5(2) . . . . ? C4 N3 C5 N4 -1.0(4) . . . . ? N2 N3 C5 N4 177.6(2) . . . . ? C4 N3 C5 C6 179.9(3) . . . . ? N2 N3 C5 C6 -1.5(4) . . . . ? N4 C5 C6 C7 -0.8(4) . . . . ? N3 C5 C6 C7 178.1(2) . . . . ? C5 C6 C7 C8 0.4(4) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? C7 C8 C9 N4 -1.3(5) . . . . ? C7 C8 C9 N5 179.0(3) . . . . ? C8 C9 N4 C5 1.0(4) . . . . ? N5 C9 N4 C5 -179.3(2) . . . . ? C6 C5 N4 C9 0.1(4) . . . . ? N3 C5 N4 C9 -178.9(2) . . . . ? N4 C9 N5 C11 11.9(4) . . . . ? C8 C9 N5 C11 -168.3(3) . . . . ? N4 C9 N5 N6 -170.7(3) . . . . ? C8 C9 N5 N6 9.0(4) . . . . ? C11 N5 N6 C10 -1.0(4) . . . . ? C9 N5 N6 C10 -178.8(3) . . . . ? N5 N6 C10 N7 1.3(4) . . . . ? N6 C10 N7 C11 -1.1(4) . . . . ? C10 N7 C11 N5 0.4(4) . . . . ? N6 N5 C11 N7 0.4(4) . . . . ? C9 N5 C11 N7 178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.538 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.076 data_[Cu-(btp)](NO3) _database_code_CSD 196739 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H21 Cu2 N25 O12' _chemical_formula_weight 1014.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1473(3) _cell_length_b 13.3356(3) _cell_length_c 13.4689(3) _cell_angle_alpha 78.475(2) _cell_angle_beta 70.419(2) _cell_angle_gamma 76.033(2) _cell_volume 1815.12(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 7835 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.274 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23632 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1389 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.55 _reflns_number_total 23632 _reflns_number_gt 17944 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL V6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL V6.12 (Sheldrick, 2001)' _computing_publication_material 'SHELXTL V6.12 (Sheldrick, 2001)' _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^)+(0.0949P)^2^+2.5453P] 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 SHELXL _refine_ls_extinction_coef 0.0146(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 23632 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.66359(4) 0.21616(3) 0.17238(3) 0.02177(12) Uani 1 1 d . . . Cu2 Cu 0.80163(4) 0.65853(3) 0.59524(3) 0.02366(12) Uani 1 1 d . . . O1 O 0.8218(3) 0.1185(2) 0.0434(2) 0.0423(7) Uani 1 1 d . . . O2 O 0.7620(2) 0.0143(2) -0.0294(2) 0.0361(6) Uani 1 1 d . . . O3 O 0.9536(3) 0.0513(2) -0.0955(2) 0.0448(7) Uani 1 1 d . . . O4 O 0.5813(2) 0.7134(2) 0.5873(2) 0.0354(6) Uani 1 1 d . . . O5 O 0.4695(3) 0.6342(2) 0.7319(2) 0.0391(6) Uani 1 1 d . . . O6 O 0.5146(3) 0.5760(2) 0.5829(2) 0.0528(8) Uani 1 1 d . . . O7 O 1.0089(2) 0.6042(2) 0.6019(2) 0.0347(6) Uani 1 1 d . . . O8 O 1.0182(2) 0.7030(2) 0.7103(2) 0.0409(7) Uani 1 1 d . . . O9 O 1.1867(2) 0.58722(18) 0.64104(19) 0.0294(5) Uani 1 1 d . . . O10 O 0.7381(2) 0.68514(18) 0.75021(18) 0.0280(5) Uani 1 1 d . . . O11 O 0.7865(3) 0.80566(19) 0.62021(19) 0.0345(6) Uani 1 1 d . . . O12 O 0.7243(3) 0.8417(2) 0.7839(2) 0.0398(6) Uani 1 1 d . . . N1 N 0.5703(3) 0.0925(2) 0.2435(2) 0.0241(6) Uani 1 1 d . . . N2 N 0.4918(3) -0.0303(2) 0.3755(2) 0.0280(6) Uani 1 1 d . . . N3 N 0.5306(3) -0.0641(2) 0.2771(2) 0.0229(5) Uani 1 1 d . . . N4 N 0.5202(2) -0.1817(2) 0.1755(2) 0.0225(5) Uani 1 1 d . . . N5 N 0.5060(2) -0.2917(2) 0.0682(2) 0.0213(5) Uani 1 1 d . . . N6 N 0.5438(3) -0.3870(2) 0.0321(2) 0.0258(6) Uani 1 1 d . . . N7 N 0.4432(2) -0.2678(2) -0.0719(2) 0.0226(5) Uani 1 1 d . . . N8 N 0.7631(2) 0.3353(2) 0.1003(2) 0.0223(5) Uani 1 1 d . . . N9 N 0.8439(3) 0.4529(2) -0.0351(2) 0.0248(6) Uani 1 1 d . . . N10 N 0.8247(2) 0.4844(2) 0.06120(19) 0.0203(5) Uani 1 1 d . . . N11 N 0.8425(2) 0.5999(2) 0.1615(2) 0.0213(5) Uani 1 1 d . . . N12 N 0.8557(2) 0.7089(2) 0.2710(2) 0.0232(5) Uani 1 1 d . . . N13 N 0.8580(3) 0.8058(2) 0.2896(2) 0.0336(7) Uani 1 1 d . . . N14 N 0.8454(3) 0.6901(2) 0.4372(2) 0.0241(5) Uani 1 1 d . . . N15 N 0.7619(3) 0.1644(2) 0.2779(2) 0.0245(6) Uani 1 1 d . . . N16 N 0.8558(3) 0.0384(2) 0.3806(2) 0.0306(6) Uani 1 1 d . . . N17 N 0.8025(3) 0.1275(2) 0.4283(2) 0.0241(6) Uani 1 1 d . . . N18 N 0.8001(2) 0.2303(2) 0.5478(2) 0.0232(5) Uani 1 1 d . . . N19 N 0.7992(3) 0.3428(2) 0.6588(2) 0.0230(5) Uani 1 1 d . . . N20 N 0.8160(3) 0.3618(2) 0.7491(2) 0.0325(7) Uani 1 1 d . . . N21 N 0.7912(3) 0.5093(2) 0.6372(2) 0.0247(6) Uani 1 1 d . . . N22 N 0.8470(3) 0.0613(2) -0.0276(2) 0.0295(6) Uani 1 1 d . . . N23 N 0.5208(2) 0.64230(19) 0.6365(2) 0.0200(5) Uani 1 1 d . . . N24 N 1.0702(3) 0.6334(2) 0.6521(2) 0.0289(6) Uani 1 1 d . . . N25 N 0.7486(3) 0.7805(2) 0.7216(2) 0.0278(6) Uani 1 1 d . . . C1 C 0.5775(3) 0.0093(2) 0.2004(3) 0.0249(6) Uani 1 1 d . . . H1A H 0.6107 0.0029 0.1266 0.030 Uiso 1 1 calc R . . C2 C 0.5173(3) 0.0640(3) 0.3500(3) 0.0289(7) Uani 1 1 d . . . H2A H 0.5003 0.1092 0.4014 0.035 Uiso 1 1 calc R . . C3 C 0.5271(3) -0.1687(2) 0.2689(2) 0.0213(6) Uani 1 1 d . . . C4 C 0.5336(3) -0.2459(3) 0.3532(3) 0.0251(7) Uani 1 1 d . . . H4A H 0.5384 -0.2309 0.4177 0.030 Uiso 1 1 calc R . . C5 C 0.5327(3) -0.3463(2) 0.3399(3) 0.0251(6) Uani 1 1 d . . . H5A H 0.5372 -0.4020 0.3956 0.030 Uiso 1 1 calc R . . C6 C 0.5252(3) -0.3645(2) 0.2443(3) 0.0236(6) Uani 1 1 d . . . H6A H 0.5242 -0.4322 0.2326 0.028 Uiso 1 1 calc R . . C7 C 0.5192(3) -0.2794(2) 0.1667(2) 0.0206(6) Uani 1 1 d . . . C8 C 0.4466(3) -0.2214(2) 0.0057(2) 0.0223(6) Uani 1 1 d . . . H8A H 0.4124 -0.1503 0.0151 0.027 Uiso 1 1 calc R . . C9 C 0.5049(3) -0.3674(2) -0.0530(3) 0.0248(6) Uani 1 1 d . . . H9A H 0.5189 -0.4187 -0.0976 0.030 Uiso 1 1 calc R . . C10 C 0.7769(3) 0.4133(2) 0.1409(2) 0.0220(6) Uani 1 1 d . . . H10A H 0.7563 0.4177 0.2145 0.026 Uiso 1 1 calc R . . C11 C 0.8072(3) 0.3625(2) -0.0072(2) 0.0243(6) Uani 1 1 d . . . H11A H 0.8110 0.3197 -0.0572 0.029 Uiso 1 1 calc R . . C12 C 0.8461(3) 0.5848(2) 0.0657(2) 0.0207(6) Uani 1 1 d . . . C13 C 0.8669(3) 0.6569(3) -0.0251(3) 0.0271(7) Uani 1 1 d . . . H13A H 0.8673 0.6417 -0.0912 0.032 Uiso 1 1 calc R . . C14 C 0.8871(3) 0.7522(3) -0.0142(3) 0.0313(7) Uani 1 1 d . . . H14A H 0.9023 0.8042 -0.0742 0.038 Uiso 1 1 calc R . . C15 C 0.8850(3) 0.7721(3) 0.0836(3) 0.0276(7) Uani 1 1 d . . . H15A H 0.8991 0.8368 0.0926 0.033 Uiso 1 1 calc R . . C16 C 0.8615(3) 0.6932(2) 0.1675(2) 0.0222(6) Uani 1 1 d . . . C17 C 0.8466(3) 0.6412(2) 0.3598(2) 0.0232(6) Uani 1 1 d . . . H17A H 0.8418 0.5699 0.3666 0.028 Uiso 1 1 calc R . . C18 C 0.8512(4) 0.7896(3) 0.3910(3) 0.0324(8) Uani 1 1 d . . . H18A H 0.8504 0.8431 0.4285 0.039 Uiso 1 1 calc R . . C19 C 0.7831(3) 0.4325(2) 0.5939(3) 0.0237(6) Uani 1 1 d . . . H19A H 0.7682 0.4391 0.5273 0.028 Uiso 1 1 calc R . . C20 C 0.8117(4) 0.4624(3) 0.7321(3) 0.0307(7) Uani 1 1 d . . . H20A H 0.8219 0.4997 0.7810 0.037 Uiso 1 1 calc R . . C21 C 0.8059(3) 0.2388(2) 0.6433(2) 0.0224(6) Uani 1 1 d . . . C22 C 0.8230(3) 0.1567(3) 0.7214(3) 0.0272(7) Uani 1 1 d . . . H22A H 0.8281 0.1677 0.7873 0.033 Uiso 1 1 calc R . . C23 C 0.8324(3) 0.0579(3) 0.6989(3) 0.0282(7) Uani 1 1 d . . . H23A H 0.8430 -0.0010 0.7503 0.034 Uiso 1 1 calc R . . C24 C 0.8263(3) 0.0449(3) 0.6014(3) 0.0286(7) Uani 1 1 d . . . H24A H 0.8329 -0.0223 0.5840 0.034 Uiso 1 1 calc R . . C25 C 0.8103(3) 0.1334(2) 0.5307(2) 0.0232(6) Uani 1 1 d . . . C26 C 0.7481(3) 0.2016(2) 0.3650(3) 0.0248(7) Uani 1 1 d . . . H26A H 0.7062 0.2702 0.3806 0.030 Uiso 1 1 calc R . . C27 C 0.8296(3) 0.0648(3) 0.2903(3) 0.0273(7) Uani 1 1 d . . . H27A H 0.8553 0.0191 0.2380 0.033 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 0.0301(2) 0.0195(2) 0.0200(2) -0.00106(15) -0.01213(15) -0.00714(15) Cu2 0.0326(2) 0.0206(2) 0.0197(2) -0.00293(15) -0.00887(16) -0.00692(15) O1 0.0419(15) 0.0396(16) 0.0460(17) -0.0263(13) -0.0101(12) 0.0039(11) O2 0.0426(15) 0.0335(14) 0.0318(14) -0.0051(11) -0.0084(11) -0.0098(11) O3 0.0364(15) 0.065(2) 0.0283(14) -0.0096(13) -0.0044(11) -0.0048(13) O4 0.0345(14) 0.0335(14) 0.0372(14) 0.0031(11) -0.0130(11) -0.0081(10) O5 0.0468(16) 0.0427(16) 0.0235(13) -0.0051(11) -0.0030(11) -0.0109(12) O6 0.105(3) 0.0332(15) 0.0363(16) -0.0049(12) -0.0338(16) -0.0237(15) O7 0.0309(13) 0.0422(15) 0.0412(15) -0.0196(12) -0.0168(11) -0.0058(10) O8 0.0385(14) 0.0500(17) 0.0400(15) -0.0236(13) -0.0096(11) -0.0077(12) O9 0.0353(13) 0.0289(13) 0.0284(13) 0.0002(10) -0.0168(10) -0.0072(10) O10 0.0340(12) 0.0250(12) 0.0254(12) -0.0026(9) -0.0071(9) -0.0091(9) O11 0.0512(15) 0.0308(13) 0.0240(12) -0.0028(10) -0.0122(11) -0.0120(11) O12 0.0565(17) 0.0331(14) 0.0343(14) -0.0160(12) -0.0124(12) -0.0090(12) N1 0.0295(14) 0.0230(14) 0.0229(13) -0.0022(11) -0.0114(11) -0.0063(10) N2 0.0378(16) 0.0274(15) 0.0201(13) -0.0072(11) -0.0051(11) -0.0103(12) N3 0.0311(14) 0.0227(13) 0.0186(13) -0.0047(10) -0.0109(10) -0.0052(10) N4 0.0258(13) 0.0212(13) 0.0226(13) -0.0015(10) -0.0101(10) -0.0056(10) N5 0.0289(13) 0.0181(13) 0.0188(12) -0.0020(10) -0.0099(10) -0.0043(10) N6 0.0329(14) 0.0212(13) 0.0254(14) -0.0066(11) -0.0113(11) -0.0026(11) N7 0.0263(13) 0.0212(13) 0.0220(13) -0.0009(10) -0.0086(10) -0.0075(10) N8 0.0258(13) 0.0248(14) 0.0179(12) -0.0042(10) -0.0076(10) -0.0053(10) N9 0.0311(14) 0.0277(14) 0.0162(13) -0.0046(11) -0.0063(10) -0.0066(11) N10 0.0234(13) 0.0229(13) 0.0159(12) -0.0042(10) -0.0059(10) -0.0053(10) N11 0.0219(12) 0.0225(13) 0.0203(13) -0.0041(10) -0.0072(10) -0.0035(10) N12 0.0284(14) 0.0196(13) 0.0227(13) -0.0044(11) -0.0081(10) -0.0046(10) N13 0.059(2) 0.0218(15) 0.0247(15) -0.0042(12) -0.0137(13) -0.0145(13) N14 0.0300(14) 0.0225(14) 0.0220(13) -0.0041(11) -0.0089(11) -0.0065(10) N15 0.0294(14) 0.0230(14) 0.0248(14) -0.0042(11) -0.0112(11) -0.0066(10) N16 0.0420(17) 0.0240(15) 0.0290(15) -0.0105(12) -0.0147(13) -0.0005(12) N17 0.0325(14) 0.0195(13) 0.0233(14) -0.0045(11) -0.0126(11) -0.0029(10) N18 0.0279(14) 0.0229(13) 0.0220(13) -0.0020(11) -0.0108(11) -0.0067(10) N19 0.0320(14) 0.0210(13) 0.0194(13) -0.0050(10) -0.0110(11) -0.0051(10) N20 0.0566(19) 0.0265(15) 0.0220(14) -0.0032(12) -0.0191(13) -0.0115(13) N21 0.0307(14) 0.0255(14) 0.0201(13) -0.0042(11) -0.0098(11) -0.0056(11) N22 0.0333(15) 0.0261(15) 0.0239(14) 0.0020(11) -0.0093(12) 0.0007(11) N23 0.0146(11) 0.0200(13) 0.0213(13) 0.0039(10) -0.0055(9) -0.0013(9) N24 0.0358(15) 0.0319(16) 0.0237(14) -0.0065(12) -0.0084(11) -0.0135(12) N25 0.0357(15) 0.0247(14) 0.0247(14) -0.0061(12) -0.0105(11) -0.0047(11) C1 0.0320(17) 0.0236(16) 0.0212(15) -0.0037(12) -0.0101(13) -0.0057(12) C2 0.0409(19) 0.0224(16) 0.0246(17) -0.0049(13) -0.0101(14) -0.0066(13) C3 0.0233(15) 0.0215(15) 0.0207(15) -0.0021(12) -0.0086(12) -0.0050(11) C4 0.0302(16) 0.0264(17) 0.0206(15) -0.0014(13) -0.0107(13) -0.0059(13) C5 0.0308(16) 0.0226(16) 0.0231(16) -0.0003(12) -0.0091(13) -0.0083(12) C6 0.0268(16) 0.0184(15) 0.0267(16) -0.0026(12) -0.0091(12) -0.0053(12) C7 0.0229(14) 0.0222(15) 0.0202(15) -0.0024(12) -0.0102(11) -0.0057(11) C8 0.0280(16) 0.0187(15) 0.0220(15) -0.0017(12) -0.0098(12) -0.0055(12) C9 0.0337(17) 0.0190(15) 0.0242(16) -0.0031(12) -0.0127(13) -0.0040(12) C10 0.0251(15) 0.0244(16) 0.0184(14) -0.0035(12) -0.0080(11) -0.0056(12) C11 0.0321(17) 0.0242(16) 0.0182(15) -0.0020(12) -0.0078(12) -0.0084(13) C12 0.0229(14) 0.0202(15) 0.0209(15) -0.0038(12) -0.0076(11) -0.0051(11) C13 0.0336(18) 0.0302(18) 0.0199(15) -0.0022(13) -0.0102(13) -0.0085(13) C14 0.043(2) 0.0259(17) 0.0251(17) 0.0040(14) -0.0118(14) -0.0098(14) C15 0.0367(18) 0.0230(16) 0.0261(17) -0.0023(13) -0.0101(14) -0.0109(13) C16 0.0226(15) 0.0236(16) 0.0217(15) -0.0031(12) -0.0071(12) -0.0060(12) C17 0.0280(16) 0.0203(15) 0.0221(15) -0.0028(12) -0.0090(12) -0.0043(12) C18 0.053(2) 0.0232(17) 0.0228(17) -0.0009(13) -0.0103(15) -0.0142(15) C19 0.0285(16) 0.0236(16) 0.0231(15) -0.0041(13) -0.0104(12) -0.0077(12) C20 0.047(2) 0.0238(17) 0.0267(17) -0.0041(14) -0.0162(15) -0.0086(14) C21 0.0236(15) 0.0249(16) 0.0205(15) -0.0033(12) -0.0077(12) -0.0064(12) C22 0.0372(18) 0.0270(17) 0.0219(16) -0.0009(13) -0.0125(13) -0.0112(13) C23 0.0372(18) 0.0244(17) 0.0241(16) 0.0017(13) -0.0140(14) -0.0050(13) C24 0.0382(19) 0.0205(16) 0.0312(18) -0.0032(13) -0.0155(14) -0.0060(13) C25 0.0259(15) 0.0258(16) 0.0215(15) -0.0040(13) -0.0114(12) -0.0048(12) C26 0.0324(17) 0.0192(15) 0.0279(17) -0.0010(13) -0.0169(13) -0.0050(12) C27 0.0338(17) 0.0243(17) 0.0253(17) -0.0069(13) -0.0124(13) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N15 1.995(3) . ? Cu1 N7 2.008(3) 2_655 ? Cu1 N8 2.051(3) . ? Cu1 N1 2.061(3) . ? Cu1 O1 2.359(2) . ? Cu1 O5 2.482(2) 2_666 ? Cu2 N21 1.978(3) . ? Cu2 N14 1.998(3) . ? Cu2 O11 2.014(2) . ? Cu2 O10 2.042(2) . ? Cu2 O7 2.275(2) . ? Cu2 O4 2.420(2) . ? Cu2 N25 2.420(3) . ? O1 N22 1.258(4) . ? O2 N22 1.264(4) . ? O3 N22 1.229(4) . ? O4 N23 1.245(4) . ? O5 N23 1.213(4) . ? O6 N23 1.275(3) . ? O7 N24 1.272(3) . ? O8 N24 1.241(3) . ? O9 N24 1.268(3) . ? O10 N25 1.275(4) . ? O11 N25 1.286(4) . ? O12 N25 1.208(3) . ? N1 C1 1.326(4) . ? N1 C2 1.368(4) . ? N2 C2 1.310(4) . ? N2 N3 1.380(3) . ? N3 C1 1.334(4) . ? N3 C3 1.431(4) . ? N4 C7 1.334(4) . ? N4 C3 1.335(4) . ? N5 C8 1.335(4) . ? N5 N6 1.371(3) . ? N5 C7 1.428(4) . ? N6 C9 1.315(4) . ? N7 C8 1.332(4) . ? N7 C9 1.358(4) . ? N7 Cu1 2.008(3) 2_655 ? N8 C10 1.329(4) . ? N8 C11 1.367(4) . ? N9 C11 1.310(4) . ? N9 N10 1.376(3) . ? N10 C10 1.338(4) . ? N10 C12 1.432(4) . ? N11 C12 1.332(4) . ? N11 C16 1.332(4) . ? N12 C17 1.337(4) . ? N12 N13 1.372(4) . ? N12 C16 1.429(4) . ? N13 C18 1.319(4) . ? N14 C17 1.329(4) . ? N14 C18 1.355(4) . ? N15 C26 1.313(4) . ? N15 C27 1.369(4) . ? N16 C27 1.306(4) . ? N16 N17 1.373(3) . ? N17 C26 1.339(4) . ? N17 C25 1.429(4) . ? N18 C25 1.329(4) . ? N18 C21 1.338(4) . ? N19 C19 1.346(4) . ? N19 N20 1.370(3) . ? N19 C21 1.424(4) . ? N20 C20 1.307(4) . ? N21 C19 1.310(4) . ? N21 C20 1.372(4) . ? C3 C4 1.380(4) . ? C4 C5 1.389(4) . ? C5 C6 1.390(4) . ? C6 C7 1.386(4) . ? C12 C13 1.386(5) . ? C13 C14 1.387(5) . ? C14 C15 1.387(5) . ? C15 C16 1.384(5) . ? C21 C22 1.384(5) . ? C22 C23 1.382(4) . ? C23 C24 1.384(5) . ? C24 C25 1.377(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Cu1 N7 177.28(11) . 2_655 ? N15 Cu1 N8 93.79(11) . . ? N7 Cu1 N8 88.08(10) 2_655 . ? N15 Cu1 N1 85.07(11) . . ? N7 Cu1 N1 93.13(10) 2_655 . ? N8 Cu1 N1 177.81(10) . . ? N15 Cu1 O1 92.45(10) . . ? N7 Cu1 O1 89.67(10) 2_655 . ? N8 Cu1 O1 85.46(10) . . ? N1 Cu1 O1 92.72(10) . . ? N15 Cu1 O5 92.80(9) . 2_666 ? N7 Cu1 O5 85.72(9) 2_655 2_666 ? N8 Cu1 O5 76.12(9) . 2_666 ? N1 Cu1 O5 105.78(10) . 2_666 ? O1 Cu1 O5 161.13(10) . 2_666 ? N21 Cu2 N14 108.81(10) . . ? N21 Cu2 O11 155.54(10) . . ? N14 Cu2 O11 95.56(10) . . ? N21 Cu2 O10 91.68(10) . . ? N14 Cu2 O10 158.63(10) . . ? O11 Cu2 O10 63.86(10) . . ? N21 Cu2 O7 84.24(10) . . ? N14 Cu2 O7 96.79(10) . . ? O11 Cu2 O7 95.19(9) . . ? O10 Cu2 O7 91.07(9) . . ? N21 Cu2 O4 94.89(10) . . ? N14 Cu2 O4 82.99(10) . . ? O11 Cu2 O4 85.81(9) . . ? O10 Cu2 O4 89.47(9) . . ? O7 Cu2 O4 178.99(8) . . ? N21 Cu2 N25 123.45(10) . . ? N14 Cu2 N25 127.51(10) . . ? O11 Cu2 N25 32.09(10) . . ? O10 Cu2 N25 31.78(10) . . ? O7 Cu2 N25 93.12(9) . . ? O4 Cu2 N25 87.79(9) . . ? N22 O1 Cu1 148.1(2) . . ? N23 O4 Cu2 108.01(18) . . ? N24 O7 Cu2 131.2(2) . . ? N25 O10 Cu2 90.71(17) . . ? N25 O11 Cu2 91.61(19) . . ? C1 N1 C2 103.7(3) . . ? C1 N1 Cu1 127.0(2) . . ? C2 N1 Cu1 127.3(2) . . ? C2 N2 N3 101.7(3) . . ? C1 N3 N2 110.8(3) . . ? C1 N3 C3 128.8(3) . . ? N2 N3 C3 120.2(3) . . ? C7 N4 C3 114.5(3) . . ? C8 N5 N6 110.8(2) . . ? C8 N5 C7 127.8(2) . . ? N6 N5 C7 121.0(2) . . ? C9 N6 N5 102.1(2) . . ? C8 N7 C9 104.1(3) . . ? C8 N7 Cu1 128.5(2) . 2_655 ? C9 N7 Cu1 126.0(2) . 2_655 ? C10 N8 C11 104.3(3) . . ? C10 N8 Cu1 130.1(2) . . ? C11 N8 Cu1 124.4(2) . . ? C11 N9 N10 102.7(3) . . ? C10 N10 N9 110.3(2) . . ? C10 N10 C12 129.1(2) . . ? N9 N10 C12 120.4(3) . . ? C12 N11 C16 115.3(3) . . ? C17 N12 N13 110.4(2) . . ? C17 N12 C16 129.7(3) . . ? N13 N12 C16 119.9(3) . . ? C18 N13 N12 102.2(3) . . ? C17 N14 C18 104.2(3) . . ? C17 N14 Cu2 135.2(2) . . ? C18 N14 Cu2 119.0(2) . . ? C26 N15 C27 104.4(3) . . ? C26 N15 Cu1 129.0(2) . . ? C27 N15 Cu1 124.0(2) . . ? C27 N16 N17 102.5(3) . . ? C26 N17 N16 110.2(2) . . ? C26 N17 C25 128.4(3) . . ? N16 N17 C25 121.5(3) . . ? C25 N18 C21 114.8(3) . . ? C19 N19 N20 110.0(2) . . ? C19 N19 C21 129.7(3) . . ? N20 N19 C21 120.2(3) . . ? C20 N20 N19 102.7(3) . . ? C19 N21 C20 104.2(3) . . ? C19 N21 Cu2 137.6(2) . . ? C20 N21 Cu2 117.7(2) . . ? O3 N22 O1 120.3(3) . . ? O3 N22 O2 119.8(3) . . ? O1 N22 O2 119.9(3) . . ? O5 N23 O4 122.6(3) . . ? O5 N23 O6 119.9(3) . . ? O4 N23 O6 117.5(3) . . ? O8 N24 O9 121.3(3) . . ? O8 N24 O7 121.7(3) . . ? O9 N24 O7 117.0(2) . . ? O12 N25 O10 123.1(3) . . ? O12 N25 O11 123.1(3) . . ? O10 N25 O11 113.8(2) . . ? O12 N25 Cu2 178.8(3) . . ? O10 N25 Cu2 57.52(14) . . ? O11 N25 Cu2 56.30(14) . . ? N1 C1 N3 109.1(3) . . ? N2 C2 N1 114.8(3) . . ? N4 C3 C4 125.9(3) . . ? N4 C3 N3 114.3(3) . . ? C4 C3 N3 119.8(3) . . ? C3 C4 C5 117.3(3) . . ? C4 C5 C6 119.4(3) . . ? C7 C6 C5 116.9(3) . . ? N4 C7 C6 126.0(3) . . ? N4 C7 N5 114.1(3) . . ? C6 C7 N5 119.9(3) . . ? N7 C8 N5 108.6(3) . . ? N6 C9 N7 114.4(3) . . ? N8 C10 N10 108.8(3) . . ? N9 C11 N8 113.9(3) . . ? N11 C12 C13 125.7(3) . . ? N11 C12 N10 114.4(3) . . ? C13 C12 N10 119.9(3) . . ? C12 C13 C14 116.4(3) . . ? C15 C14 C13 120.4(3) . . ? C16 C15 C14 116.7(3) . . ? N11 C16 C15 125.5(3) . . ? N11 C16 N12 114.8(3) . . ? C15 C16 N12 119.7(3) . . ? N14 C17 N12 108.9(3) . . ? N13 C18 N14 114.3(3) . . ? N21 C19 N19 109.2(3) . . ? N20 C20 N21 113.9(3) . . ? N18 C21 C22 125.6(3) . . ? N18 C21 N19 114.0(3) . . ? C22 C21 N19 120.4(3) . . ? C23 C22 C21 116.8(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 117.2(3) . . ? N18 C25 C24 125.8(3) . . ? N18 C25 N17 113.2(3) . . ? C24 C25 N17 121.0(3) . . ? N15 C26 N17 109.0(3) . . ? N16 C27 N15 113.9(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.953 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.124