# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email whuang@nju.edu.cn _publ_contact_author_name 'Wei Huang' _publ_author_name 'Wei Huang' data_1 _database_code_depnum_ccdc_archive 'CCDC 853389' #TrackingRef '- 1-3-rev1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 N5 O5' _chemical_formula_sum 'C15 H13 N5 O5' _chemical_formula_weight 343.30 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 16.8753(14) _cell_length_b 8.0175(7) _cell_length_c 11.2187(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1517.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1484 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 22.49 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9862 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8109 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2625 _reflns_number_gt 1881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One restraint is generated automatically by program, which is related to the assignment of non-centrosymmetric space group of Pca21. ; _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^)+(0.0453P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(17) _refine_ls_number_reflns 2625 _refine_ls_number_parameters 229 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.36085(19) 0.7300(4) 0.4244(3) 0.0339(8) Uani 1 1 d . . . C2 C 0.37482(19) 0.8971(4) 0.6065(3) 0.0358(8) Uani 1 1 d . . . C3 C 0.28834(19) 0.9137(4) 0.6099(3) 0.0320(8) Uani 1 1 d . . . C4 C 0.23957(17) 0.8400(4) 0.5300(3) 0.0303(7) Uani 1 1 d . . . C5 C 0.27386(17) 0.7398(4) 0.4381(3) 0.0286(7) Uani 1 1 d . . . C15 C 0.49303(16) 0.7953(5) 0.4990(4) 0.0535(10) Uani 1 1 d . . . H15A H 0.5085 0.8080 0.4153 0.080 Uiso 1 1 calc R . . H15B H 0.5103 0.6859 0.5281 0.080 Uiso 1 1 calc R . . H15C H 0.5181 0.8832 0.5466 0.080 Uiso 1 1 calc R . . C14 C 0.2572(2) 1.0124(4) 0.7052(3) 0.0375(8) Uani 1 1 d . . . C13 C 0.15095(18) 0.8612(4) 0.5340(3) 0.0440(9) Uani 1 1 d . . . H13A H 0.1367 0.9343 0.6006 0.066 Uiso 1 1 calc R . . H13B H 0.1258 0.7521 0.5447 0.066 Uiso 1 1 calc R . . H13C H 0.1327 0.9111 0.4591 0.066 Uiso 1 1 calc R . . C6 C 0.19633(18) 0.4852(4) 0.2060(3) 0.0304(7) Uani 1 1 d . . . C11 C 0.21891(17) 0.3997(4) 0.1026(3) 0.0293(8) Uani 1 1 d . . . C10 C 0.16437(16) 0.3273(4) 0.0252(3) 0.0317(7) Uani 1 1 d . . . H10 H 0.1814 0.2706 -0.0446 0.038 Uiso 1 1 calc R . . C9 C 0.08429(19) 0.3400(4) 0.0528(3) 0.0355(8) Uani 1 1 d . . . C8 C 0.06078(18) 0.4162(4) 0.1580(3) 0.0402(9) Uani 1 1 d . . . H8 H 0.0061 0.4192 0.1783 0.048 Uiso 1 1 calc R . . C7 C 0.11500(19) 0.4870(4) 0.2330(3) 0.0366(8) Uani 1 1 d . . . H7 H 0.0974 0.5383 0.3046 0.044 Uiso 1 1 calc R . . C12 C 0.0472(2) 0.2139(5) -0.1314(3) 0.0482(10) Uani 1 1 d . . . H12A H 0.0833 0.1194 -0.1203 0.072 Uiso 1 1 calc R . . H12B H 0.0736 0.3004 -0.1785 0.072 Uiso 1 1 calc R . . H12C H -0.0006 0.1761 -0.1732 0.072 Uiso 1 1 calc R . . N1 N 0.40603(13) 0.8087(3) 0.5095(3) 0.0357(7) Uani 1 1 d . . . N2 N 0.23019(18) 1.0905(4) 0.7814(3) 0.0511(8) Uani 1 1 d . . . N3 N 0.22372(15) 0.6597(3) 0.3675(2) 0.0309(6) Uani 1 1 d . . . N4 N 0.25042(15) 0.5657(3) 0.2804(2) 0.0297(6) Uani 1 1 d . . . H4 H 0.3017 0.5536 0.2691 0.036 Uiso 1 1 calc R . . N5 N 0.30235(16) 0.3776(4) 0.0696(3) 0.0349(7) Uani 1 1 d . . . O1 O 0.39259(12) 0.6538(3) 0.3423(2) 0.0422(6) Uani 1 1 d . . . O2 O 0.41772(14) 0.9588(3) 0.6813(2) 0.0514(7) Uani 1 1 d . . . O3 O 0.35396(13) 0.4495(3) 0.1293(2) 0.0478(7) Uani 1 1 d . . . O4 O 0.31844(12) 0.2888(3) -0.0140(3) 0.0553(7) Uani 1 1 d . . . O5 O 0.02545(12) 0.2808(3) -0.0170(2) 0.0504(7) 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 C1 0.0274(18) 0.0353(19) 0.039(2) 0.0040(17) -0.0029(17) -0.0006(15) C2 0.034(2) 0.0290(18) 0.044(2) 0.0059(17) -0.0064(18) 0.0009(15) C3 0.0316(17) 0.0306(18) 0.0340(19) 0.0026(15) -0.0037(16) 0.0006(14) C4 0.0268(16) 0.0281(17) 0.0359(19) 0.0045(15) -0.0023(16) 0.0013(14) C5 0.0228(16) 0.0299(17) 0.0331(18) 0.0039(14) -0.0040(15) -0.0006(14) C15 0.0195(16) 0.073(2) 0.068(3) -0.005(2) -0.0064(19) -0.0044(17) C14 0.041(2) 0.0338(19) 0.038(2) 0.0055(17) -0.0071(17) -0.0001(16) C13 0.0295(18) 0.050(2) 0.053(2) -0.0104(19) -0.0010(17) 0.0037(15) C6 0.0233(17) 0.0326(18) 0.0353(19) 0.0033(15) -0.0014(15) -0.0010(13) C11 0.0207(16) 0.0339(18) 0.0332(19) 0.0055(15) 0.0013(14) 0.0002(14) C10 0.0278(16) 0.0354(18) 0.0321(18) 0.0011(15) 0.0003(15) -0.0023(14) C9 0.0275(18) 0.046(2) 0.0333(19) -0.0029(16) -0.0018(15) -0.0074(15) C8 0.0209(17) 0.054(2) 0.046(2) -0.0067(19) 0.0049(16) -0.0022(16) C7 0.0285(19) 0.046(2) 0.035(2) -0.0062(17) 0.0027(15) -0.0026(15) C12 0.043(2) 0.061(2) 0.040(2) -0.007(2) -0.0049(18) -0.0117(19) N1 0.0205(12) 0.0433(16) 0.0434(18) -0.0012(14) -0.0088(13) -0.0003(12) N2 0.054(2) 0.054(2) 0.045(2) -0.0038(17) -0.0030(18) -0.0005(16) N3 0.0262(14) 0.0308(15) 0.0357(16) 0.0003(13) -0.0017(13) 0.0015(12) N4 0.0202(12) 0.0353(14) 0.0338(15) -0.0017(13) 0.0017(13) 0.0033(13) N5 0.0246(15) 0.0398(15) 0.0403(17) -0.0003(15) 0.0006(13) 0.0022(13) O1 0.0266(13) 0.0546(16) 0.0455(15) -0.0090(13) 0.0034(11) -0.0013(11) O2 0.0425(14) 0.0575(15) 0.0543(17) -0.0094(14) -0.0214(13) 0.0003(13) O3 0.0221(12) 0.0673(17) 0.0540(16) -0.0175(13) -0.0039(12) -0.0047(12) O4 0.0306(13) 0.0806(18) 0.0546(16) -0.0305(16) 0.0039(13) 0.0075(13) O5 0.0274(12) 0.0769(17) 0.0468(16) -0.0168(15) -0.0028(12) -0.0137(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.228(4) . ? C1 N1 1.376(4) . ? C1 C5 1.478(4) . ? C2 O2 1.214(4) . ? C2 N1 1.401(4) . ? C2 C3 1.466(4) . ? C3 C4 1.353(4) . ? C3 C14 1.430(5) . ? C4 C5 1.430(4) . ? C4 C13 1.506(4) . ? C5 N3 1.325(4) . ? C15 N1 1.477(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14 N2 1.153(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C6 N4 1.395(4) . ? C6 C11 1.400(4) . ? C6 C7 1.405(4) . ? C11 C10 1.392(4) . ? C11 N5 1.467(4) . ? C10 C9 1.390(4) . ? C10 H10 0.9500 . ? C9 O5 1.351(3) . ? C9 C8 1.387(4) . ? C8 C7 1.366(4) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C12 O5 1.439(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N3 N4 1.314(3) . ? N4 H4 0.8800 . ? N5 O4 1.209(3) . ? N5 O3 1.241(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 120.5(3) . . ? O1 C1 C5 122.5(3) . . ? N1 C1 C5 117.0(3) . . ? O2 C2 N1 121.3(3) . . ? O2 C2 C3 122.6(3) . . ? N1 C2 C3 116.2(3) . . ? C4 C3 C14 120.9(3) . . ? C4 C3 C2 123.2(3) . . ? C14 C3 C2 115.9(3) . . ? C3 C4 C5 118.5(3) . . ? C3 C4 C13 122.4(3) . . ? C5 C4 C13 119.1(3) . . ? N3 C5 C4 116.4(3) . . ? N3 C5 C1 123.1(3) . . ? C4 C5 C1 120.5(3) . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C14 C3 178.3(4) . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C6 C11 122.9(3) . . ? N4 C6 C7 120.4(3) . . ? C11 C6 C7 116.7(3) . . ? C10 C11 C6 122.7(3) . . ? C10 C11 N5 115.3(3) . . ? C6 C11 N5 122.0(3) . . ? C9 C10 C11 118.3(3) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? O5 C9 C8 116.0(3) . . ? O5 C9 C10 124.0(3) . . ? C8 C9 C10 120.0(3) . . ? C7 C8 C9 121.0(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 N1 C2 124.3(3) . . ? C1 N1 C15 117.5(3) . . ? C2 N1 C15 118.2(3) . . ? N4 N3 C5 120.2(3) . . ? N3 N4 C6 119.1(3) . . ? N3 N4 H4 120.5 . . ? C6 N4 H4 120.5 . . ? O4 N5 O3 122.3(3) . . ? O4 N5 C11 118.9(3) . . ? O3 N5 C11 118.8(3) . . ? C9 O5 C12 117.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.181 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.040 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 853390' #TrackingRef '- 1-3-rev1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 N5 O5' _chemical_formula_sum 'C16 H15 N5 O5' _chemical_formula_weight 357.33 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 6.4252(5) _cell_length_b 13.5443(11) _cell_length_c 19.5352(16) _cell_angle_alpha 90.00 _cell_angle_beta 105.3640(10) _cell_angle_gamma 90.00 _cell_volume 1639.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3953 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.89 _exptl_crystal_description block _exptl_crystal_colour red _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 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9868 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8996 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2881 _reflns_number_gt 2321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0619P)^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 SHELXL _refine_ls_extinction_coef 0.0041(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2881 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1308(2) 0.37381(10) 0.36873(7) 0.0357(3) Uani 1 1 d . . . C2 C -0.1820(2) 0.48193(12) 0.32587(8) 0.0446(4) Uani 1 1 d . . . C3 C -0.3096(2) 0.39472(11) 0.29710(7) 0.0375(3) Uani 1 1 d . . . C4 C -0.2291(2) 0.30187(10) 0.30124(7) 0.0339(3) Uani 1 1 d . . . C5 C -0.0042(2) 0.28876(10) 0.33862(7) 0.0328(3) Uani 1 1 d . . . C6 C 0.3330(2) 0.07852(10) 0.38642(7) 0.0314(3) Uani 1 1 d . . . C7 C 0.1823(2) 0.00323(11) 0.36303(7) 0.0362(3) Uani 1 1 d . . . H7 H 0.0362 0.0198 0.3411 0.043 Uiso 1 1 calc R . . C8 C 0.2415(2) -0.09391(11) 0.37123(7) 0.0382(3) Uani 1 1 d . . . H8 H 0.1357 -0.1437 0.3551 0.046 Uiso 1 1 calc R . . C9 C 0.4544(2) -0.12112(10) 0.40277(7) 0.0353(3) Uani 1 1 d . . . C10 C 0.6080(2) -0.04874(10) 0.42614(7) 0.0331(3) Uani 1 1 d . . . H10 H 0.7540 -0.0661 0.4476 0.040 Uiso 1 1 calc R . . C11 C 0.5469(2) 0.04972(10) 0.41790(6) 0.0297(3) Uani 1 1 d . . . C12 C 0.7132(3) -0.25158(12) 0.43264(9) 0.0541(4) Uani 1 1 d . . . H12A H 0.7990 -0.2233 0.4028 0.081 Uiso 1 1 calc R . . H12B H 0.7195 -0.3238 0.4309 0.081 Uiso 1 1 calc R . . H12C H 0.7713 -0.2293 0.4817 0.081 Uiso 1 1 calc R . . C13 C -0.3621(2) 0.21513(11) 0.26800(8) 0.0433(4) Uani 1 1 d . . . H13A H -0.5148 0.2286 0.2639 0.065 Uiso 1 1 calc R . . H13B H -0.3169 0.1566 0.2977 0.065 Uiso 1 1 calc R . . H13C H -0.3418 0.2034 0.2207 0.065 Uiso 1 1 calc R . . C14 C -0.5334(2) 0.41362(12) 0.26154(8) 0.0452(4) Uani 1 1 d . . . C15 C 0.1757(3) 0.55302(11) 0.38536(9) 0.0523(4) Uani 1 1 d . . . H15A H 0.1109 0.6122 0.3582 0.063 Uiso 1 1 calc R . . H15B H 0.3189 0.5421 0.3767 0.063 Uiso 1 1 calc R . . C16 C 0.2046(3) 0.57182(13) 0.46328(10) 0.0636(5) Uani 1 1 d . . . H16A H 0.0636 0.5840 0.4721 0.095 Uiso 1 1 calc R . . H16B H 0.2975 0.6296 0.4780 0.095 Uiso 1 1 calc R . . H16C H 0.2717 0.5140 0.4906 0.095 Uiso 1 1 calc R . . N1 N 0.03629(19) 0.46626(8) 0.35933(6) 0.0406(3) Uani 1 1 d . . . N2 N -0.7107(2) 0.42574(12) 0.23291(7) 0.0628(4) Uani 1 1 d . . . N3 N 0.06642(17) 0.19664(8) 0.34423(6) 0.0327(3) Uani 1 1 d . . . N4 N 0.26743(17) 0.17716(8) 0.37813(6) 0.0333(3) Uani 1 1 d . . . H4 H 0.3588 0.2251 0.3952 0.040 Uiso 1 1 calc R . . N5 N 0.71792(17) 0.12199(9) 0.44391(6) 0.0345(3) Uani 1 1 d . . . O1 O 0.32168(15) 0.36488(7) 0.40137(5) 0.0445(3) Uani 1 1 d . . . O2 O -0.2588(2) 0.56457(8) 0.32072(7) 0.0660(4) Uani 1 1 d . . . O3 O 0.67239(16) 0.21014(7) 0.44437(6) 0.0484(3) Uani 1 1 d . . . O4 O 0.90451(15) 0.09250(8) 0.46364(6) 0.0517(3) Uani 1 1 d . . . O5 O 0.49418(17) -0.21995(7) 0.40717(6) 0.0473(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0336(8) 0.0326(8) 0.0392(7) 0.0008(6) 0.0064(6) 0.0033(6) C2 0.0455(9) 0.0428(9) 0.0428(8) 0.0013(7) 0.0068(7) 0.0150(7) C3 0.0339(7) 0.0432(9) 0.0334(7) 0.0035(6) 0.0050(6) 0.0119(6) C4 0.0299(7) 0.0408(8) 0.0300(7) 0.0040(6) 0.0058(6) 0.0048(6) C5 0.0310(7) 0.0316(8) 0.0343(7) 0.0011(6) 0.0058(6) 0.0046(6) C6 0.0306(7) 0.0308(7) 0.0312(7) -0.0010(5) 0.0056(6) 0.0039(6) C7 0.0289(7) 0.0357(8) 0.0420(8) -0.0039(6) 0.0061(6) 0.0004(6) C8 0.0364(8) 0.0339(8) 0.0433(8) -0.0060(6) 0.0091(6) -0.0025(6) C9 0.0410(8) 0.0287(8) 0.0369(7) -0.0014(6) 0.0113(6) 0.0037(6) C10 0.0329(7) 0.0337(8) 0.0308(7) -0.0002(6) 0.0054(6) 0.0065(6) C11 0.0281(7) 0.0313(7) 0.0285(7) -0.0016(5) 0.0051(5) 0.0002(6) C12 0.0549(10) 0.0363(9) 0.0652(10) -0.0020(8) 0.0057(9) 0.0157(8) C13 0.0332(8) 0.0473(9) 0.0433(8) -0.0010(7) -0.0006(6) 0.0018(6) C14 0.0433(9) 0.0523(10) 0.0383(8) 0.0031(7) 0.0077(7) 0.0170(7) C15 0.0488(9) 0.0322(8) 0.0740(11) -0.0011(8) 0.0133(8) 0.0006(7) C16 0.0607(11) 0.0472(11) 0.0781(12) -0.0187(9) 0.0101(9) -0.0039(8) N1 0.0391(7) 0.0286(7) 0.0506(7) -0.0007(5) 0.0060(6) 0.0048(5) N2 0.0427(8) 0.0878(12) 0.0518(8) 0.0055(7) 0.0020(7) 0.0256(8) N3 0.0274(6) 0.0346(7) 0.0337(6) 0.0013(5) 0.0038(5) 0.0037(5) N4 0.0266(6) 0.0284(6) 0.0411(6) -0.0015(5) 0.0023(5) 0.0017(5) N5 0.0306(6) 0.0350(7) 0.0341(6) -0.0003(5) 0.0019(5) 0.0023(5) O1 0.0324(5) 0.0360(6) 0.0578(6) -0.0017(5) -0.0011(5) 0.0015(4) O2 0.0652(8) 0.0411(7) 0.0810(8) -0.0051(6) 0.0007(7) 0.0242(6) O3 0.0380(6) 0.0314(6) 0.0675(7) -0.0110(5) -0.0006(5) 0.0030(4) O4 0.0279(5) 0.0448(7) 0.0724(7) 0.0050(5) -0.0043(5) 0.0050(5) O5 0.0473(6) 0.0282(6) 0.0630(7) -0.0034(5) 0.0085(5) 0.0063(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 C1 O1 1.2294(15) . ? C1 N1 1.3824(18) . ? C1 C5 1.4679(19) . ? C2 O2 1.2166(18) . ? C2 N1 1.3977(19) . ? C2 C3 1.463(2) . ? C3 C4 1.3540(19) . ? C3 C14 1.4442(19) . ? C4 C5 1.4473(18) . ? C4 C13 1.496(2) . ? C5 N3 1.3222(17) . ? C6 C7 1.3969(19) . ? C6 N4 1.3973(17) . ? C6 C11 1.4040(18) . ? C7 C8 1.367(2) . ? C7 H7 0.9500 . ? C8 C9 1.3925(19) . ? C8 H8 0.9500 . ? C9 O5 1.3613(17) . ? C9 C10 1.380(2) . ? C10 C11 1.3875(18) . ? C10 H10 0.9500 . ? C11 N5 1.4588(17) . ? C12 O5 1.4285(18) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N2 1.1401(18) . ? C15 N1 1.483(2) . ? C15 C16 1.505(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N3 N4 1.3126(15) . ? N4 H4 0.8800 . ? N5 O4 1.2250(13) . ? N5 O3 1.2299(14) . ? 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 C1 N1 120.05(12) . . ? O1 C1 C5 122.20(12) . . ? N1 C1 C5 117.75(12) . . ? O2 C2 N1 120.86(15) . . ? O2 C2 C3 122.51(14) . . ? N1 C2 C3 116.62(12) . . ? C4 C3 C14 120.60(14) . . ? C4 C3 C2 124.11(13) . . ? C14 C3 C2 115.28(13) . . ? C3 C4 C5 117.30(13) . . ? C3 C4 C13 122.57(12) . . ? C5 C4 C13 120.13(12) . . ? N3 C5 C4 115.62(12) . . ? N3 C5 C1 123.65(12) . . ? C4 C5 C1 120.72(12) . . ? C7 C6 N4 119.91(12) . . ? C7 C6 C11 116.98(12) . . ? N4 C6 C11 123.12(12) . . ? C8 C7 C6 121.13(12) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 121.11(13) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? O5 C9 C10 124.85(13) . . ? O5 C9 C8 115.74(12) . . ? C10 C9 C8 119.40(13) . . ? C9 C10 C11 119.24(13) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C6 122.14(13) . . ? C10 C11 N5 116.13(12) . . ? C6 C11 N5 121.73(12) . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C3 178.03(18) . . ? N1 C15 C16 112.46(14) . . ? N1 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 C2 123.41(12) . . ? C1 N1 C15 117.90(12) . . ? C2 N1 C15 118.69(12) . . ? N4 N3 C5 120.10(11) . . ? N3 N4 C6 118.47(11) . . ? N3 N4 H4 120.8 . . ? C6 N4 H4 120.8 . . ? O4 N5 O3 121.94(11) . . ? O4 N5 C11 118.36(11) . . ? O3 N5 C11 119.68(11) . . ? C9 O5 C12 117.92(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.176 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.038 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 882917' #TrackingRef '- 1-3-rev1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H56 Cu2 N20 O20' _chemical_formula_weight 1552.37 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.654(1) _cell_length_b 12.926(1) _cell_length_c 13.271(1) _cell_angle_alpha 76.991(1) _cell_angle_beta 72.708(1) _cell_angle_gamma 65.931(1) _cell_volume 1730.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3457 _cell_measurement_theta_min 2.230 _cell_measurement_theta_max 26.452 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9203 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9792 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6060 _reflns_number_gt 4554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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. Seven restraints are used to restrain the large Ueq for related atomes, namely, "simu 0.01 c29 c30" and "delu 0.001 cu1 o1". ; _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^)+(0.0930P)^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 6060 _refine_ls_number_parameters 478 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.40157(4) 0.23545(3) 0.19512(3) 0.03808(16) Uani 1 1 d . . . C1 C 0.0789(3) 0.3196(3) 0.2121(3) 0.0460(8) Uani 1 1 d . . . C2 C -0.0466(4) 0.3930(4) 0.2245(3) 0.0584(10) Uani 1 1 d . . . H2 H -0.0774 0.4369 0.1655 0.070 Uiso 1 1 calc R . . C3 C -0.1276(5) 0.4022(6) 0.3241(4) 0.1087(16) Uani 1 1 d . . . C4 C -0.0805(4) 0.3345(4) 0.4119(3) 0.0709(13) Uani 1 1 d . . . H4 H -0.1350 0.3375 0.4795 0.085 Uiso 1 1 calc R . . C5 C 0.0470(4) 0.2638(3) 0.3975(3) 0.0584(10) Uani 1 1 d . . . H5 H 0.0780 0.2214 0.4569 0.070 Uiso 1 1 calc R . . C6 C 0.1315(3) 0.2527(3) 0.2988(3) 0.0416(8) Uani 1 1 d . . . C7 C -0.3330(5) 0.4989(6) 0.4301(4) 0.1087(16) Uani 1 1 d . . . H7A H -0.3615 0.4362 0.4603 0.163 Uiso 1 1 calc R . . H7B H -0.4064 0.5678 0.4231 0.163 Uiso 1 1 calc R . . H7C H -0.2877 0.5073 0.4757 0.163 Uiso 1 1 calc R . . C8 C 0.3989(3) 0.0182(3) 0.3689(2) 0.0367(7) Uani 1 1 d . . . C9 C 0.5162(3) 0.0134(3) 0.2920(3) 0.0386(7) Uani 1 1 d . . . C10 C 0.6396(4) -0.1505(3) 0.3990(3) 0.0479(9) Uani 1 1 d . . . C11 C 0.5184(4) -0.1431(3) 0.4746(3) 0.0425(8) Uani 1 1 d . . . C12 C 0.4007(3) -0.0653(3) 0.4597(3) 0.0412(8) Uani 1 1 d . . . C13 C 0.7495(3) -0.0820(3) 0.2240(3) 0.0538(9) Uani 1 1 d . . . H13A H 0.8239 -0.1198 0.2553 0.065 Uiso 1 1 calc R . . H13B H 0.7490 -0.0068 0.1911 0.065 Uiso 1 1 calc R . . C14 C 0.7606(4) -0.1492(4) 0.1411(4) 0.0753(13) Uani 1 1 d . . . H14A H 0.7650 -0.2248 0.1730 0.113 Uiso 1 1 calc R . . H14B H 0.8374 -0.1537 0.0864 0.113 Uiso 1 1 calc R . . H14C H 0.6864 -0.1124 0.1106 0.113 Uiso 1 1 calc R . . C15 C 0.5302(4) -0.2221(3) 0.5693(3) 0.0531(9) Uani 1 1 d . . . C16 C 0.2783(4) -0.0672(4) 0.5354(3) 0.0598(10) Uani 1 1 d . . . H16A H 0.2310 -0.0892 0.5014 0.090 Uiso 1 1 calc R . . H16B H 0.2273 0.0073 0.5571 0.090 Uiso 1 1 calc R . . H16C H 0.2977 -0.1211 0.5966 0.090 Uiso 1 1 calc R . . C17 C 0.7771(4) 0.1929(3) 0.0266(3) 0.0521(9) Uani 1 1 d . . . C18 C 0.8775(4) 0.1267(4) -0.0428(3) 0.0614(10) Uani 1 1 d . . . H18 H 0.9616 0.1187 -0.0466 0.074 Uiso 1 1 calc R . . C19 C 0.8541(4) 0.0716(3) -0.1074(3) 0.0580(10) Uani 1 1 d U . . C20 C 0.7313(4) 0.0790(3) -0.0999(3) 0.0592(10) Uani 1 1 d U . . H20 H 0.7168 0.0384 -0.1414 0.071 Uiso 1 1 calc R . . C21 C 0.6274(4) 0.1485(3) -0.0290(3) 0.0525(9) Uani 1 1 d . . . H21 H 0.5439 0.1538 -0.0239 0.063 Uiso 1 1 calc R . . C22 C 0.6476(3) 0.2089(3) 0.0331(3) 0.0417(8) Uani 1 1 d . . . C23 C 0.9438(6) -0.0300(5) -0.2588(5) 0.1012(18) Uani 1 1 d . . . H23A H 0.8991 -0.0820 -0.2297 0.152 Uiso 1 1 calc R . . H23B H 1.0260 -0.0681 -0.3036 0.152 Uiso 1 1 calc R . . H23C H 0.8934 0.0343 -0.3000 0.152 Uiso 1 1 calc R . . C24 C 0.4627(3) 0.4620(3) 0.1551(2) 0.0366(7) Uani 1 1 d . . . C25 C 0.3331(3) 0.4677(3) 0.2028(2) 0.0387(7) Uani 1 1 d . . . C26 C 0.2843(4) 0.6427(3) 0.2758(3) 0.0560(10) Uani 1 1 d . . . C27 C 0.4161(4) 0.6328(3) 0.2276(3) 0.0484(9) Uani 1 1 d . . . C28 C 0.5027(3) 0.5487(3) 0.1657(3) 0.0419(8) Uani 1 1 d . . . C29 C 0.1133(4) 0.5649(4) 0.3044(4) 0.0778(14) Uani 1 1 d U . . H29A H 0.1110 0.4886 0.3235 0.093 Uiso 1 1 calc R . . H29B H 0.0801 0.6019 0.3686 0.093 Uiso 1 1 calc R . . C30 C 0.0343(6) 0.6278(6) 0.2310(7) 0.142(3) Uani 1 1 d U . . H30A H 0.0235 0.7067 0.2225 0.213 Uiso 1 1 calc R . . H30B H -0.0486 0.6206 0.2574 0.213 Uiso 1 1 calc R . . H30C H 0.0748 0.5985 0.1636 0.213 Uiso 1 1 calc R . . C31 C 0.4532(4) 0.7172(3) 0.2493(3) 0.0585(10) Uani 1 1 d . . . C32 C 0.6366(4) 0.5465(3) 0.1110(3) 0.0569(10) Uani 1 1 d . . . H32A H 0.6482 0.6096 0.1278 0.085 Uiso 1 1 calc R . . H32B H 0.6481 0.5523 0.0355 0.085 Uiso 1 1 calc R . . H32C H 0.6990 0.4762 0.1347 0.085 Uiso 1 1 calc R . . N1 N 0.1573(3) 0.3116(3) 0.1010(2) 0.0561(8) Uani 1 1 d . . . N2 N 0.2649(3) 0.1831(2) 0.2886(2) 0.0382(6) Uani 1 1 d . . . N3 N 0.2798(3) 0.0945(2) 0.3601(2) 0.0394(6) Uani 1 1 d . . . N4 N 0.6306(3) -0.0703(2) 0.3081(2) 0.0417(7) Uani 1 1 d . . . N5 N 0.5414(4) -0.2807(3) 0.6454(3) 0.0739(11) Uani 1 1 d . . . N6 N 0.8115(4) 0.2368(3) 0.1011(3) 0.0675(10) Uani 1 1 d . . . N7 N 0.5385(3) 0.2852(2) 0.0970(2) 0.0381(6) Uani 1 1 d . . . N8 N 0.5545(3) 0.3781(2) 0.0985(2) 0.0391(6) Uani 1 1 d . . . N9 N 0.2491(3) 0.5575(2) 0.2567(2) 0.0519(8) Uani 1 1 d . . . N10 N 0.4816(4) 0.7841(3) 0.2683(3) 0.0849(12) Uani 1 1 d . . . O1 O 0.2617(3) 0.2320(3) 0.0823(2) 0.0672(8) Uani 1 1 d . . . O2 O 0.1165(3) 0.3852(3) 0.0328(2) 0.0899(11) Uani 1 1 d . . . O3 O -0.2498(3) 0.4775(4) 0.3292(3) 0.1128(15) Uani 1 1 d . . . O4 O 0.5212(2) 0.08052(19) 0.20687(18) 0.0454(6) Uani 1 1 d . . . O5 O 0.7440(3) -0.2201(2) 0.4118(2) 0.0697(8) Uani 1 1 d . . . O6 O 0.7606(3) 0.2278(3) 0.1939(3) 0.0827(10) Uani 1 1 d . . . O7 O 0.8950(4) 0.2790(4) 0.0632(3) 0.1148(14) Uani 1 1 d . . . O8 O 0.9628(3) 0.0078(3) -0.1756(3) 0.0869(10) Uani 1 1 d . . . O9 O 0.2903(2) 0.39505(18) 0.19506(18) 0.0424(5) Uani 1 1 d . . . O10 O 0.2060(3) 0.7176(2) 0.3286(3) 0.0806(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0365(3) 0.0326(2) 0.0400(3) -0.00181(16) -0.00579(17) -0.01109(18) C1 0.043(2) 0.059(2) 0.0379(19) -0.0029(16) -0.0100(16) -0.0213(18) C2 0.039(2) 0.077(3) 0.054(2) -0.002(2) -0.0195(18) -0.013(2) C3 0.049(2) 0.145(4) 0.075(3) -0.005(2) -0.0097(18) 0.013(2) C4 0.045(2) 0.094(3) 0.047(2) -0.004(2) -0.0017(19) -0.007(2) C5 0.048(2) 0.063(2) 0.048(2) 0.0021(18) -0.0101(18) -0.009(2) C6 0.040(2) 0.0434(18) 0.042(2) -0.0028(15) -0.0095(16) -0.0170(16) C7 0.049(2) 0.145(4) 0.075(3) -0.005(2) -0.0097(18) 0.013(2) C8 0.0425(19) 0.0332(16) 0.0348(18) -0.0039(13) -0.0092(14) -0.0141(15) C9 0.0418(19) 0.0308(16) 0.0423(19) -0.0075(14) -0.0088(15) -0.0114(15) C10 0.054(2) 0.0435(19) 0.045(2) -0.0025(16) -0.0164(18) -0.0152(18) C11 0.056(2) 0.0385(17) 0.0341(18) 0.0009(14) -0.0155(16) -0.0171(16) C12 0.050(2) 0.0413(18) 0.0354(18) -0.0058(14) -0.0099(15) -0.0188(16) C13 0.040(2) 0.049(2) 0.061(2) 0.0015(18) -0.0073(18) -0.0124(17) C14 0.060(3) 0.087(3) 0.063(3) -0.024(2) 0.007(2) -0.018(2) C15 0.055(2) 0.051(2) 0.051(2) -0.0008(19) -0.0159(19) -0.0181(19) C16 0.053(2) 0.066(3) 0.052(2) 0.0121(19) -0.0089(18) -0.025(2) C17 0.043(2) 0.053(2) 0.050(2) -0.0121(18) -0.0015(17) -0.0102(18) C18 0.046(2) 0.068(3) 0.064(3) -0.016(2) -0.0002(19) -0.019(2) C19 0.047(2) 0.060(2) 0.056(2) -0.0132(19) -0.0004(19) -0.0138(19) C20 0.075(3) 0.054(2) 0.051(2) -0.0116(19) -0.014(2) -0.025(2) C21 0.053(2) 0.049(2) 0.048(2) -0.0026(17) -0.0077(18) -0.0166(18) C22 0.048(2) 0.0365(17) 0.0329(18) -0.0015(14) -0.0026(15) -0.0145(16) C23 0.098(4) 0.109(4) 0.094(4) -0.064(3) 0.011(3) -0.032(3) C24 0.0393(18) 0.0324(16) 0.0330(17) 0.0016(13) -0.0091(14) -0.0105(14) C25 0.045(2) 0.0307(16) 0.0354(18) 0.0017(13) -0.0110(15) -0.0105(15) C26 0.073(3) 0.043(2) 0.047(2) -0.0083(17) -0.003(2) -0.022(2) C27 0.068(3) 0.0404(19) 0.040(2) -0.0014(15) -0.0156(18) -0.0225(18) C28 0.051(2) 0.0385(18) 0.0374(19) 0.0040(14) -0.0171(16) -0.0175(16) C29 0.053(3) 0.057(3) 0.110(4) -0.037(3) 0.015(3) -0.017(2) C30 0.069(4) 0.105(5) 0.210(8) 0.012(5) -0.011(5) -0.019(4) C31 0.077(3) 0.051(2) 0.055(2) -0.0088(19) -0.022(2) -0.024(2) C32 0.057(2) 0.056(2) 0.066(3) -0.0032(19) -0.017(2) -0.029(2) N1 0.048(2) 0.072(2) 0.0477(19) -0.0040(17) -0.0149(16) -0.0209(18) N2 0.0364(16) 0.0365(14) 0.0393(15) -0.0032(12) -0.0102(12) -0.0105(12) N3 0.0401(16) 0.0375(15) 0.0402(16) -0.0033(12) -0.0087(12) -0.0147(13) N4 0.0399(16) 0.0364(14) 0.0444(16) -0.0008(12) -0.0092(13) -0.0119(13) N5 0.076(3) 0.076(2) 0.053(2) 0.0219(19) -0.0219(19) -0.021(2) N6 0.053(2) 0.075(2) 0.074(3) -0.024(2) -0.0117(19) -0.0182(19) N7 0.0385(16) 0.0347(14) 0.0352(15) -0.0009(11) -0.0062(12) -0.0110(12) N8 0.0433(16) 0.0346(14) 0.0380(15) 0.0009(12) -0.0122(13) -0.0136(13) N9 0.0471(18) 0.0424(16) 0.0590(19) -0.0153(14) 0.0028(15) -0.0151(14) N10 0.108(3) 0.072(2) 0.094(3) -0.025(2) -0.030(3) -0.041(2) O1 0.0654(19) 0.0746(19) 0.0501(16) -0.0183(14) -0.0128(14) -0.0091(16) O2 0.065(2) 0.117(3) 0.0540(19) 0.0245(18) -0.0142(15) -0.0183(19) O3 0.0476(19) 0.162(4) 0.066(2) -0.011(2) -0.0093(16) 0.019(2) O4 0.0450(14) 0.0360(12) 0.0411(13) 0.0041(10) -0.0016(10) -0.0112(11) O5 0.0491(17) 0.0675(18) 0.0682(19) 0.0109(14) -0.0193(14) -0.0030(15) O6 0.069(2) 0.099(2) 0.073(2) -0.0243(19) -0.0218(18) -0.0123(19) O7 0.094(3) 0.150(4) 0.134(3) -0.057(3) 0.005(2) -0.080(3) O8 0.062(2) 0.097(2) 0.093(2) -0.051(2) 0.0075(17) -0.0179(18) O9 0.0361(13) 0.0370(12) 0.0526(14) -0.0041(10) -0.0113(11) -0.0119(10) O10 0.093(2) 0.0581(18) 0.080(2) -0.0339(17) 0.0210(18) -0.0320(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4 1.921(2) . ? Cu1 O9 1.938(2) . ? Cu1 N2 1.965(3) . ? Cu1 N7 1.970(3) . ? C1 C2 1.364(5) . ? C1 C6 1.410(4) . ? C1 N1 1.486(5) . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 O3 1.350(5) . ? C3 C4 1.398(6) . ? C4 C5 1.372(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 N2 1.426(4) . ? C7 O3 1.409(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N3 1.357(4) . ? C8 C12 1.424(4) . ? C8 C9 1.431(5) . ? C9 O4 1.262(4) . ? C9 N4 1.371(4) . ? C10 O5 1.216(4) . ? C10 N4 1.402(4) . ? C10 C11 1.449(5) . ? C11 C12 1.371(5) . ? C11 C15 1.432(5) . ? C12 C16 1.486(5) . ? C13 N4 1.475(4) . ? C13 C14 1.497(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N5 1.124(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.359(5) . ? C17 C22 1.416(5) . ? C17 N6 1.460(5) . ? C18 C19 1.375(6) . ? C18 H18 0.9300 . ? C19 C20 1.369(6) . ? C19 O8 1.381(5) . ? C20 C21 1.404(5) . ? C20 H20 0.9300 . ? C21 C22 1.379(5) . ? C21 H21 0.9300 . ? C22 N7 1.421(4) . ? C23 O8 1.409(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N8 1.352(4) . ? C24 C28 1.425(5) . ? C24 C25 1.432(5) . ? C25 O9 1.263(4) . ? C25 N9 1.359(4) . ? C26 O10 1.211(4) . ? C26 N9 1.415(5) . ? C26 C27 1.441(5) . ? C27 C28 1.374(5) . ? C27 C31 1.435(5) . ? C28 C32 1.504(5) . ? C29 C30 1.422(8) . ? C29 N9 1.491(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N10 1.142(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N1 O2 1.204(4) . ? N1 O1 1.231(4) . ? N2 N3 1.299(4) . ? N6 O6 1.200(5) . ? N6 O7 1.231(5) . ? N7 N8 1.294(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 O4 Cu1 O9 173.04(10) . . ? O4 Cu1 N2 88.45(10) . . ? O9 Cu1 N2 93.26(10) . . ? O4 Cu1 N7 90.91(10) . . ? O9 Cu1 N7 87.64(10) . . ? N2 Cu1 N7 177.79(11) . . ? C2 C1 C6 122.4(3) . . ? C2 C1 N1 116.2(3) . . ? C6 C1 N1 121.4(3) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? O3 C3 C2 116.2(4) . . ? O3 C3 C4 124.5(5) . . ? C2 C3 C4 119.3(4) . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 123.0(4) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 115.8(3) . . ? C5 C6 N2 120.8(3) . . ? C1 C6 N2 123.2(3) . . ? O3 C7 H7A 109.5 . . ? O3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C12 115.1(3) . . ? N3 C8 C9 124.7(3) . . ? C12 C8 C9 120.1(3) . . ? O4 C9 N4 116.9(3) . . ? O4 C9 C8 123.7(3) . . ? N4 C9 C8 119.4(3) . . ? O5 C10 N4 120.7(4) . . ? O5 C10 C11 123.7(3) . . ? N4 C10 C11 115.7(3) . . ? C12 C11 C15 121.5(3) . . ? C12 C11 C10 123.6(3) . . ? C15 C11 C10 114.8(3) . . ? C11 C12 C8 117.8(3) . . ? C11 C12 C16 121.5(3) . . ? C8 C12 C16 120.7(3) . . ? N4 C13 C14 111.2(3) . . ? N4 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N4 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C11 176.6(4) . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 121.8(4) . . ? C18 C17 N6 116.0(4) . . ? C22 C17 N6 121.9(3) . . ? C17 C18 C19 119.7(4) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.8(4) . . ? C20 C19 O8 124.4(4) . . ? C18 C19 O8 114.8(4) . . ? C19 C20 C21 119.4(4) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C17 117.2(3) . . ? C21 C22 N7 118.6(3) . . ? C17 C22 N7 124.1(3) . . ? O8 C23 H23A 109.5 . . ? O8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N8 C24 C28 115.3(3) . . ? N8 C24 C25 124.6(3) . . ? C28 C24 C25 120.1(3) . . ? O9 C25 N9 117.4(3) . . ? O9 C25 C24 123.5(3) . . ? N9 C25 C24 119.0(3) . . ? O10 C26 N9 120.4(4) . . ? O10 C26 C27 124.4(4) . . ? N9 C26 C27 115.2(3) . . ? C28 C27 C31 121.1(4) . . ? C28 C27 C26 123.6(3) . . ? C31 C27 C26 115.3(3) . . ? C27 C28 C24 118.1(3) . . ? C27 C28 C32 121.6(3) . . ? C24 C28 C32 120.3(3) . . ? C30 C29 N9 110.3(5) . . ? C30 C29 H29A 109.6 . . ? N9 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? N9 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N10 C31 C27 178.9(5) . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 N1 O1 122.5(3) . . ? O2 N1 C1 118.1(3) . . ? O1 N1 C1 119.4(3) . . ? N3 N2 C6 110.8(3) . . ? N3 N2 Cu1 126.6(2) . . ? C6 N2 Cu1 121.7(2) . . ? N2 N3 C8 121.5(3) . . ? C9 N4 C10 123.1(3) . . ? C9 N4 C13 119.3(3) . . ? C10 N4 C13 117.5(3) . . ? O6 N6 O7 124.1(4) . . ? O6 N6 C17 119.4(4) . . ? O7 N6 C17 116.4(4) . . ? N8 N7 C22 112.0(3) . . ? N8 N7 Cu1 125.0(2) . . ? C22 N7 Cu1 121.5(2) . . ? N7 N8 C24 121.7(3) . . ? C25 N9 C26 123.8(3) . . ? C25 N9 C29 119.1(3) . . ? C26 N9 C29 117.0(3) . . ? C3 O3 C7 118.5(4) . . ? C9 O4 Cu1 122.8(2) . . ? C19 O8 C23 117.3(4) . . ? C25 O9 Cu1 119.9(2) . . ? 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 C6 C1 C2 C3 -1.3(7) . . . . ? N1 C1 C2 C3 177.2(5) . . . . ? C1 C2 C3 O3 179.4(5) . . . . ? C1 C2 C3 C4 -0.8(9) . . . . ? O3 C3 C4 C5 -177.7(6) . . . . ? C2 C3 C4 C5 2.6(9) . . . . ? C3 C4 C5 C6 -2.4(8) . . . . ? C4 C5 C6 C1 0.3(6) . . . . ? C4 C5 C6 N2 176.4(4) . . . . ? C2 C1 C6 C5 1.6(5) . . . . ? N1 C1 C6 C5 -176.9(3) . . . . ? C2 C1 C6 N2 -174.4(3) . . . . ? N1 C1 C6 N2 7.1(5) . . . . ? N3 C8 C9 O4 0.0(5) . . . . ? C12 C8 C9 O4 176.0(3) . . . . ? N3 C8 C9 N4 -177.8(3) . . . . ? C12 C8 C9 N4 -1.9(4) . . . . ? O5 C10 C11 C12 -179.5(3) . . . . ? N4 C10 C11 C12 1.3(5) . . . . ? O5 C10 C11 C15 2.2(5) . . . . ? N4 C10 C11 C15 -177.1(3) . . . . ? C15 C11 C12 C8 173.2(3) . . . . ? C10 C11 C12 C8 -5.1(5) . . . . ? C15 C11 C12 C16 -6.8(5) . . . . ? C10 C11 C12 C16 175.0(3) . . . . ? N3 C8 C12 C11 -178.4(3) . . . . ? C9 C8 C12 C11 5.3(5) . . . . ? N3 C8 C12 C16 1.6(5) . . . . ? C9 C8 C12 C16 -174.8(3) . . . . ? C12 C11 C15 N5 -101(8) . . . . ? C10 C11 C15 N5 77(8) . . . . ? C22 C17 C18 C19 -1.3(6) . . . . ? N6 C17 C18 C19 172.7(4) . . . . ? C17 C18 C19 C20 -2.5(7) . . . . ? C17 C18 C19 O8 179.3(4) . . . . ? C18 C19 C20 C21 3.3(6) . . . . ? O8 C19 C20 C21 -178.8(4) . . . . ? C19 C20 C21 C22 -0.2(6) . . . . ? C20 C21 C22 C17 -3.4(5) . . . . ? C20 C21 C22 N7 174.9(3) . . . . ? C18 C17 C22 C21 4.2(6) . . . . ? N6 C17 C22 C21 -169.5(3) . . . . ? C18 C17 C22 N7 -174.0(3) . . . . ? N6 C17 C22 N7 12.3(5) . . . . ? N8 C24 C25 O9 -1.3(5) . . . . ? C28 C24 C25 O9 178.7(3) . . . . ? N8 C24 C25 N9 -179.1(3) . . . . ? C28 C24 C25 N9 0.9(5) . . . . ? O10 C26 C27 C28 -178.3(4) . . . . ? N9 C26 C27 C28 1.0(5) . . . . ? O10 C26 C27 C31 2.4(6) . . . . ? N9 C26 C27 C31 -178.3(3) . . . . ? C31 C27 C28 C24 174.6(3) . . . . ? C26 C27 C28 C24 -4.7(5) . . . . ? C31 C27 C28 C32 -5.0(5) . . . . ? C26 C27 C28 C32 175.8(3) . . . . ? N8 C24 C28 C27 -176.3(3) . . . . ? C25 C24 C28 C27 3.7(4) . . . . ? N8 C24 C28 C32 3.3(4) . . . . ? C25 C24 C28 C32 -176.7(3) . . . . ? C28 C27 C31 N10 -136(25) . . . . ? C26 C27 C31 N10 43(25) . . . . ? C2 C1 N1 O2 15.7(5) . . . . ? C6 C1 N1 O2 -165.8(4) . . . . ? C2 C1 N1 O1 -165.6(4) . . . . ? C6 C1 N1 O1 13.0(5) . . . . ? C5 C6 N2 N3 34.6(4) . . . . ? C1 C6 N2 N3 -149.6(3) . . . . ? C5 C6 N2 Cu1 -135.0(3) . . . . ? C1 C6 N2 Cu1 40.8(4) . . . . ? O4 Cu1 N2 N3 27.1(3) . . . . ? O9 Cu1 N2 N3 -146.2(3) . . . . ? N7 Cu1 N2 N3 100(3) . . . . ? O4 Cu1 N2 C6 -165.2(2) . . . . ? O9 Cu1 N2 C6 21.6(2) . . . . ? N7 Cu1 N2 C6 -92(3) . . . . ? C6 N2 N3 C8 -177.2(3) . . . . ? Cu1 N2 N3 C8 -8.3(4) . . . . ? C12 C8 N3 N2 171.6(3) . . . . ? C9 C8 N3 N2 -12.2(5) . . . . ? O4 C9 N4 C10 179.9(3) . . . . ? C8 C9 N4 C10 -2.2(5) . . . . ? O4 C9 N4 C13 -3.8(4) . . . . ? C8 C9 N4 C13 174.2(3) . . . . ? O5 C10 N4 C9 -176.8(3) . . . . ? C11 C10 N4 C9 2.5(5) . . . . ? O5 C10 N4 C13 6.8(5) . . . . ? C11 C10 N4 C13 -173.9(3) . . . . ? C14 C13 N4 C9 -82.5(4) . . . . ? C14 C13 N4 C10 94.0(4) . . . . ? C18 C17 N6 O6 -131.7(4) . . . . ? C22 C17 N6 O6 42.4(5) . . . . ? C18 C17 N6 O7 46.6(6) . . . . ? C22 C17 N6 O7 -139.3(4) . . . . ? C21 C22 N7 N8 -140.9(3) . . . . ? C17 C22 N7 N8 37.3(4) . . . . ? C21 C22 N7 Cu1 52.2(4) . . . . ? C17 C22 N7 Cu1 -129.6(3) . . . . ? O4 Cu1 N7 N8 -139.2(2) . . . . ? O9 Cu1 N7 N8 34.0(2) . . . . ? N2 Cu1 N7 N8 148(3) . . . . ? O4 Cu1 N7 C22 25.9(2) . . . . ? O9 Cu1 N7 C22 -160.9(2) . . . . ? N2 Cu1 N7 C22 -47(3) . . . . ? C22 N7 N8 C24 -179.5(3) . . . . ? Cu1 N7 N8 C24 -13.2(4) . . . . ? C28 C24 N8 N7 168.6(3) . . . . ? C25 C24 N8 N7 -11.4(5) . . . . ? O9 C25 N9 C26 177.2(3) . . . . ? C24 C25 N9 C26 -4.9(5) . . . . ? O9 C25 N9 C29 0.7(5) . . . . ? C24 C25 N9 C29 178.7(3) . . . . ? O10 C26 N9 C25 -176.6(4) . . . . ? C27 C26 N9 C25 4.0(5) . . . . ? O10 C26 N9 C29 -0.1(6) . . . . ? C27 C26 N9 C29 -179.5(4) . . . . ? C30 C29 N9 C25 -90.9(5) . . . . ? C30 C29 N9 C26 92.4(5) . . . . ? C2 C3 O3 C7 -173.6(6) . . . . ? C4 C3 O3 C7 6.7(11) . . . . ? N4 C9 O4 Cu1 -150.8(2) . . . . ? C8 C9 O4 Cu1 31.3(4) . . . . ? O9 Cu1 O4 C9 66.8(9) . . . . ? N2 Cu1 O4 C9 -37.5(3) . . . . ? N7 Cu1 O4 C9 144.6(3) . . . . ? C20 C19 O8 C23 15.4(7) . . . . ? C18 C19 O8 C23 -166.5(5) . . . . ? N9 C25 O9 Cu1 -145.8(2) . . . . ? C24 C25 O9 Cu1 36.3(4) . . . . ? O4 Cu1 O9 C25 34.0(9) . . . . ? N2 Cu1 O9 C25 138.1(2) . . . . ? N7 Cu1 O9 C25 -44.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.087 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.066 #===END