# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Miguel Quiros' _publ_contact_author_email MQUIROS@UGR.ES _publ_section_title ; Versatility in the binding modes of 4,6-dimethyl-1,2,3-triazolo[4,5-d]-pyrimidin-5,7-dionato in presence of bipyrimidine. Analyses of their supramolecular architectures through H-bonds ; loop_ _publ_author_name 'Miguel Quiros' 'Carmen R. Maldonado' 'Antonio Rodriguez Dieguez' 'Juan M Salas' # Attachment 'Cpd1_znaxbpir.cif' data_znaxbpir _database_code_depnum_ccdc_archive 'CCDC 732839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 N24 O10 Zn2, 2(H2 O)' _chemical_formula_sum 'C32 H38 N24 O12 Zn2' _chemical_formula_weight 1081.60 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' Zn Zn 0.2839 1.4301 '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 10.3170(9) _cell_length_b 10.3555(9) _cell_length_c 11.0667(9) _cell_angle_alpha 97.483(1) _cell_angle_beta 100.866(1) _cell_angle_gamma 112.462(1) _cell_volume 1046.06(15) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2899 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.0 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 108 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 12383 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4771 _reflns_number_gt 3798 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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^)+(0.0500P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4771 _refine_ls_number_parameters 332 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Zn Zn 0.48665(3) 0.32123(3) 0.26900(3) 0.03037(11) Uani 1 1 d . . . N1A N 0.2044(2) 0.2867(2) 0.1366(2) 0.0323(5) Uani 1 1 d . . . N2A N 0.2715(2) 0.2162(2) 0.1941(2) 0.0315(5) Uani 1 1 d . . . N3A N 0.1785(2) 0.0890(2) 0.2102(2) 0.0323(5) Uani 1 1 d . . . C3AA C 0.0485(3) 0.0818(3) 0.1590(2) 0.0279(5) Uani 1 1 d . . . N4A N -0.0858(2) -0.0261(2) 0.1499(2) 0.0330(5) Uani 1 1 d . . . C4A C -0.0969(3) -0.1534(3) 0.1991(3) 0.0470(8) Uani 1 1 d . . . H41A H -0.1547 -0.1650 0.2588 0.056 Uiso 1 1 d R . . H42A H -0.0014 -0.1427 0.2399 0.056 Uiso 1 1 d R . . H43A H -0.1415 -0.2362 0.1304 0.056 Uiso 1 1 d R . . C5A C -0.2083(3) -0.0152(3) 0.0913(2) 0.0338(6) Uani 1 1 d . . . O5A O -0.3295(2) -0.1091(2) 0.08140(19) 0.0434(5) Uani 1 1 d . . . N6A N -0.1932(2) 0.1065(2) 0.0437(2) 0.0340(5) Uani 1 1 d . . . C6A C -0.3275(3) 0.1095(3) -0.0261(3) 0.0550(9) Uani 1 1 d . . . H61A H -0.3785 0.1310 0.0322 0.066 Uiso 1 1 d R . . H62A H -0.3879 0.0177 -0.0818 0.066 Uiso 1 1 d R . . H63A H -0.3041 0.1818 -0.0745 0.066 Uiso 1 1 d R . . C7A C -0.0624(3) 0.2244(3) 0.0534(3) 0.0336(6) Uani 1 1 d . . . O7A O -0.0605(2) 0.3291(2) 0.0140(2) 0.0521(6) Uani 1 1 d . . . C7AA C 0.0615(3) 0.2027(3) 0.1140(2) 0.0280(5) Uani 1 1 d . . . N1B N 0.6405(2) 0.2507(2) 0.3053(2) 0.0341(5) Uani 1 1 d . . . N2B N 0.6166(2) 0.1267(2) 0.3416(2) 0.0412(6) Uani 1 1 d . . . N3B N 0.7432(3) 0.1168(2) 0.3828(2) 0.0419(6) Uani 1 1 d . . . C3AB C 0.8466(3) 0.2377(3) 0.3709(2) 0.0305(6) Uani 1 1 d . . . N4B N 0.9949(2) 0.2787(2) 0.4039(2) 0.0355(5) Uani 1 1 d . . . C4B C 1.0587(3) 0.1940(3) 0.4679(3) 0.0461(8) Uani 1 1 d . . . H41B H 1.1141 0.1655 0.4182 0.055 Uiso 1 1 d R . . H42B H 0.9828 0.1103 0.4786 0.055 Uiso 1 1 d R . . H43B H 1.1212 0.2507 0.5490 0.055 Uiso 1 1 d R . . C5B C 1.0848(3) 0.4074(3) 0.3863(2) 0.0360(6) Uani 1 1 d . . . O5B O 1.2160(2) 0.4487(2) 0.4162(2) 0.0527(6) Uani 1 1 d . . . N6B N 1.0202(2) 0.4898(2) 0.3320(2) 0.0346(5) Uani 1 1 d . . . C6B C 1.1185(3) 0.6208(3) 0.3031(3) 0.0510(8) Uani 1 1 d . . . H61B H 1.0655 0.6460 0.2362 0.061 Uiso 1 1 d R . . H62B H 1.1957 0.6046 0.2773 0.061 Uiso 1 1 d R . . H63B H 1.1584 0.6977 0.3769 0.061 Uiso 1 1 d R . . C7B C 0.8709(3) 0.4594(3) 0.3025(2) 0.0316(6) Uani 1 1 d . . . O7B O 0.8260(2) 0.5438(2) 0.2650(2) 0.0445(5) Uani 1 1 d . . . C7AB C 0.7863(3) 0.3221(3) 0.3230(2) 0.0295(6) Uani 1 1 d . . . N1P N 0.5229(2) 0.5294(2) 0.34710(19) 0.0274(5) Uani 1 1 d . . . C2P C 0.5166(2) 0.5592(2) 0.4661(2) 0.0258(5) Uani 1 1 d . . . N3P N 0.5375(2) 0.6865(2) 0.5296(2) 0.0287(5) Uani 1 1 d . . . C4P C 0.5635(3) 0.7919(3) 0.4675(3) 0.0368(6) Uani 1 1 d . . . H4P H 0.5795 0.8827 0.5093 0.044 Uiso 1 1 d R . . C5P C 0.5679(3) 0.7706(3) 0.3435(3) 0.0388(7) Uani 1 1 d . . . H5P H 0.5833 0.8439 0.3000 0.047 Uiso 1 1 d R . . C6P C 0.5481(3) 0.6360(3) 0.2859(3) 0.0341(6) Uani 1 1 d . . . H6P H 0.5521 0.6188 0.2024 0.041 Uiso 1 1 d R . . O1W O 0.5107(2) 0.3656(2) 0.09202(19) 0.0391(5) Uani 1 1 d D . . H11W H 0.583(2) 0.405(3) 0.065(3) 0.047 Uiso 1 1 d D . . H12W H 0.457(3) 0.293(2) 0.036(2) 0.047 Uiso 1 1 d D . . O2W O 0.2812(2) 0.5468(3) 0.0357(2) 0.0516(6) Uani 1 1 d D . . H21W H 0.204(2) 0.555(4) 0.012(3) 0.062 Uiso 1 1 d D . . H22W H 0.259(4) 0.469(2) 0.060(3) 0.062 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02274(17) 0.02790(18) 0.0374(2) 0.00540(13) 0.00540(13) 0.00904(13) N1A 0.0235(11) 0.0322(12) 0.0385(13) 0.0113(10) 0.0062(10) 0.0084(9) N2A 0.0236(11) 0.0335(12) 0.0342(12) 0.0090(10) 0.0079(9) 0.0079(9) N3A 0.0264(11) 0.0311(12) 0.0371(13) 0.0106(10) 0.0076(10) 0.0091(9) C3AA 0.0272(13) 0.0273(13) 0.0257(13) 0.0051(10) 0.0083(10) 0.0072(10) N4A 0.0294(12) 0.0258(11) 0.0374(13) 0.0089(10) 0.0102(10) 0.0035(9) C4A 0.0437(17) 0.0395(17) 0.0524(19) 0.0232(15) 0.0136(15) 0.0073(14) C5A 0.0277(14) 0.0348(15) 0.0322(14) -0.0004(12) 0.0113(11) 0.0067(12) O5A 0.0269(10) 0.0377(11) 0.0518(12) 0.0029(9) 0.0130(9) -0.0003(8) N6A 0.0206(11) 0.0353(13) 0.0407(13) 0.0069(10) 0.0049(10) 0.0077(9) C6A 0.0254(15) 0.052(2) 0.079(2) 0.0138(18) 0.0005(16) 0.0135(14) C7A 0.0275(14) 0.0336(15) 0.0380(15) 0.0099(12) 0.0080(12) 0.0105(11) O7A 0.0357(11) 0.0461(13) 0.0763(16) 0.0310(12) 0.0083(11) 0.0165(10) C7AA 0.0218(12) 0.0273(13) 0.0314(14) 0.0077(11) 0.0062(10) 0.0066(10) N1B 0.0278(12) 0.0302(12) 0.0423(13) 0.0060(10) 0.0071(10) 0.0117(10) N2B 0.0333(13) 0.0330(13) 0.0574(16) 0.0123(12) 0.0139(12) 0.0123(10) N3B 0.0417(14) 0.0335(13) 0.0537(16) 0.0128(11) 0.0130(12) 0.0176(11) C3AB 0.0305(14) 0.0326(14) 0.0316(14) 0.0070(11) 0.0069(11) 0.0170(12) N4B 0.0288(12) 0.0422(14) 0.0383(13) 0.0098(11) 0.0043(10) 0.0197(11) C4B 0.0481(18) 0.055(2) 0.0453(18) 0.0149(15) 0.0067(15) 0.0330(16) C5B 0.0290(15) 0.0476(17) 0.0305(15) 0.0032(13) 0.0050(12) 0.0179(13) O5B 0.0262(11) 0.0691(15) 0.0602(14) 0.0153(12) 0.0073(10) 0.0186(11) N6B 0.0255(11) 0.0363(13) 0.0383(13) 0.0096(10) 0.0077(10) 0.0089(10) C6B 0.0337(16) 0.0481(19) 0.063(2) 0.0196(16) 0.0140(15) 0.0058(14) C7B 0.0291(14) 0.0341(15) 0.0301(14) 0.0049(11) 0.0053(11) 0.0134(12) O7B 0.0377(11) 0.0374(11) 0.0621(14) 0.0219(10) 0.0113(10) 0.0168(9) C7AB 0.0257(13) 0.0331(14) 0.0315(14) 0.0069(11) 0.0068(11) 0.0147(11) N1P 0.0209(10) 0.0253(11) 0.0311(12) 0.0072(9) 0.0047(9) 0.0051(9) C2P 0.0155(11) 0.0257(13) 0.0329(14) 0.0067(10) 0.0031(10) 0.0066(10) N3P 0.0238(11) 0.0239(11) 0.0358(12) 0.0064(9) 0.0068(9) 0.0078(9) C4P 0.0345(15) 0.0252(14) 0.0477(18) 0.0082(12) 0.0104(13) 0.0093(12) C5P 0.0425(16) 0.0299(15) 0.0445(17) 0.0168(13) 0.0116(13) 0.0129(13) C6P 0.0353(15) 0.0333(15) 0.0329(15) 0.0112(12) 0.0100(12) 0.0116(12) O1W 0.0309(11) 0.0387(12) 0.0387(12) 0.0073(9) 0.0112(9) 0.0046(9) O2W 0.0373(12) 0.0590(15) 0.0649(15) 0.0323(12) 0.0187(11) 0.0184(11) _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 Zn N1B 1.984(2) . ? Zn N2A 2.006(2) . ? Zn N1P 2.076(2) . ? Zn O1W 2.107(2) . ? Zn N3P 2.297(2) 2_666 ? N1A N2A 1.326(3) . ? N1A C7AA 1.348(3) . ? N2A N3A 1.359(3) . ? N3A C3AA 1.324(3) . ? C3AA C7AA 1.376(3) . ? C3AA N4A 1.383(3) . ? N4A C5A 1.360(3) . ? N4A C4A 1.464(3) . ? C4A H41A 0.9600 . ? C4A H42A 0.9600 . ? C4A H43A 0.9600 . ? C5A O5A 1.230(3) . ? C5A N6A 1.394(3) . ? N6A C7A 1.405(3) . ? N6A C6A 1.468(3) . ? C6A H61A 0.9600 . ? C6A H62A 0.9600 . ? C6A H63A 0.9600 . ? C7A O7A 1.216(3) . ? C7A C7AA 1.438(3) . ? N1B N2B 1.342(3) . ? N1B C7AB 1.360(3) . ? N2B N3B 1.347(3) . ? N3B C3AB 1.341(3) . ? C3AB C7AB 1.357(3) . ? C3AB N4B 1.381(3) . ? N4B C5B 1.366(4) . ? N4B C4B 1.459(3) . ? C4B H41B 0.9601 . ? C4B H42B 0.9601 . ? C4B H43B 0.9601 . ? C5B O5B 1.215(3) . ? C5B N6B 1.396(3) . ? N6B C7B 1.412(3) . ? N6B C6B 1.468(4) . ? C6B H61B 0.9601 . ? C6B H62B 0.9601 . ? C6B H63B 0.9601 . ? C7B O7B 1.217(3) . ? C7B C7AB 1.430(4) . ? N1P C2P 1.332(3) . ? N1P C6P 1.337(3) . ? C2P N3P 1.328(3) . ? C2P C2P 1.483(5) 2_666 ? N3P C4P 1.332(3) . ? N3P Zn 2.297(2) 2_666 ? C4P C5P 1.374(4) . ? C4P H4P 0.9300 . ? C5P C6P 1.375(4) . ? C5P H5P 0.9300 . ? C6P H6P 0.9300 . ? O1W H11W 0.832(10) . ? O1W H12W 0.829(10) . ? O2W H21W 0.832(10) . ? O2W H22W 0.837(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 N1B Zn N2A 131.33(9) . . ? N1B Zn N1P 121.54(8) . . ? N2A Zn N1P 105.76(8) . . ? N1B Zn O1W 98.00(9) . . ? N2A Zn O1W 89.23(8) . . ? N1P Zn O1W 93.71(8) . . ? N1B Zn N3P 88.67(8) . 2_666 ? N2A Zn N3P 92.20(8) . 2_666 ? N1P Zn N3P 76.13(8) . 2_666 ? O1W Zn N3P 169.75(8) . 2_666 ? N2A N1A C7AA 105.2(2) . . ? N1A N2A N3A 113.19(19) . . ? N1A N2A Zn 117.22(16) . . ? N3A N2A Zn 128.74(16) . . ? C3AA N3A N2A 103.8(2) . . ? N3A C3AA C7AA 110.3(2) . . ? N3A C3AA N4A 128.1(2) . . ? C7AA C3AA N4A 121.6(2) . . ? C5A N4A C3AA 119.4(2) . . ? C5A N4A C4A 119.9(2) . . ? C3AA N4A C4A 120.6(2) . . ? N4A C4A H41A 109.9 . . ? N4A C4A H42A 109.4 . . ? H41A C4A H42A 109.5 . . ? N4A C4A H43A 109.2 . . ? H41A C4A H43A 109.5 . . ? H42A C4A H43A 109.5 . . ? O5A C5A N4A 121.2(3) . . ? O5A C5A N6A 120.6(3) . . ? N4A C5A N6A 118.2(2) . . ? C5A N6A C7A 126.6(2) . . ? C5A N6A C6A 116.4(2) . . ? C7A N6A C6A 117.0(2) . . ? N6A C6A H61A 109.6 . . ? N6A C6A H62A 109.4 . . ? H61A C6A H62A 109.5 . . ? N6A C6A H63A 109.4 . . ? H61A C6A H63A 109.5 . . ? H62A C6A H63A 109.5 . . ? O7A C7A N6A 121.8(2) . . ? O7A C7A C7AA 126.7(2) . . ? N6A C7A C7AA 111.6(2) . . ? N1A C7AA C3AA 107.6(2) . . ? N1A C7AA C7A 129.9(2) . . ? C3AA C7AA C7A 122.6(2) . . ? N2B N1B C7AB 107.4(2) . . ? N2B N1B Zn 122.29(17) . . ? C7AB N1B Zn 129.21(18) . . ? N1B N2B N3B 110.4(2) . . ? C3AB N3B N2B 105.6(2) . . ? N3B C3AB C7AB 110.4(2) . . ? N3B C3AB N4B 127.3(2) . . ? C7AB C3AB N4B 122.2(2) . . ? C5B N4B C3AB 119.3(2) . . ? C5B N4B C4B 119.0(2) . . ? C3AB N4B C4B 121.5(2) . . ? N4B C4B H41B 109.5 . . ? N4B C4B H42B 109.6 . . ? H41B C4B H42B 109.5 . . ? N4B C4B H43B 109.4 . . ? H41B C4B H43B 109.5 . . ? H42B C4B H43B 109.5 . . ? O5B C5B N4B 121.4(3) . . ? O5B C5B N6B 121.1(3) . . ? N4B C5B N6B 117.5(2) . . ? C5B N6B C7B 126.5(2) . . ? C5B N6B C6B 116.2(2) . . ? C7B N6B C6B 117.3(2) . . ? N6B C6B H61B 109.4 . . ? N6B C6B H62B 109.4 . . ? H61B C6B H62B 109.5 . . ? N6B C6B H63B 109.6 . . ? H61B C6B H63B 109.5 . . ? H62B C6B H63B 109.5 . . ? O7B C7B N6B 121.7(2) . . ? O7B C7B C7AB 126.9(2) . . ? N6B C7B C7AB 111.4(2) . . ? C3AB C7AB N1B 106.3(2) . . ? C3AB C7AB C7B 122.8(2) . . ? N1B C7AB C7B 130.9(2) . . ? C2P N1P C6P 116.9(2) . . ? C2P N1P Zn 118.06(16) . . ? C6P N1P Zn 124.99(18) . . ? N3P C2P N1P 125.4(2) . . ? N3P C2P C2P 116.9(3) . 2_666 ? N1P C2P C2P 117.6(3) . 2_666 ? C2P N3P C4P 116.9(2) . . ? C2P N3P Zn 111.24(16) . 2_666 ? C4P N3P Zn 131.85(18) . 2_666 ? N3P C4P C5P 121.9(3) . . ? N3P C4P H4P 119.2 . . ? C5P C4P H4P 118.8 . . ? C4P C5P C6P 117.2(3) . . ? C4P C5P H5P 121.5 . . ? C6P C5P H5P 121.2 . . ? N1P C6P C5P 121.5(3) . . ? N1P C6P H6P 119.2 . . ? C5P C6P H6P 119.2 . . ? Zn O1W H11W 133(2) . . ? Zn O1W H12W 109(2) . . ? H11W O1W H12W 105(3) . . ? H21W O2W H22W 106(3) . . ? 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 O1W H11W O2W 0.832(10) 1.913(13) 2.724(3) 165(3) 2_665 O1W H12W O5A 0.829(10) 1.959(11) 2.785(3) 174(3) 2 O2W H22W N1A 0.837(10) 2.100(11) 2.934(3) 175(3) . O2W H21W O7A 0.832(10) 2.234(17) 3.015(3) 156(3) 2_565 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.415 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.078 # Attachment 'Cpd2_cdaxbpir.cif' data_cdaxbpir _database_code_depnum_ccdc_archive 'CCDC 732840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Cd2 N24 O12, 6(H2 O)' _chemical_formula_sum 'C32 H50 Cd2 N24 O18' _chemical_formula_weight 1283.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 10.5968(5) _cell_length_b 10.7757(5) _cell_length_c 11.7018(6) _cell_angle_alpha 90.286(1) _cell_angle_beta 105.216(1) _cell_angle_gamma 114.417(1) _cell_volume 1164.21(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8224 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 309 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0 _diffrn_reflns_number 13738 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.35 _reflns_number_total 5279 _reflns_number_gt 5044 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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^)+(0.0300P)^2^+1.7000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5279 _refine_ls_number_parameters 377 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.28417(2) 0.498981(19) 0.255354(16) 0.01423(7) Uani 1 1 d . . . N1A N 0.2491(2) 0.2087(2) 0.1519(2) 0.0169(5) Uani 1 1 d . . . N2A N 0.1827(2) 0.2644(2) 0.2004(2) 0.0171(5) Uani 1 1 d . . . N3A N 0.0571(2) 0.1690(2) 0.2179(2) 0.0170(5) Uani 1 1 d . . . C3AA C 0.0479(3) 0.0488(3) 0.1767(2) 0.0150(5) Uani 1 1 d . . . N4A N -0.0608(2) -0.0805(2) 0.1706(2) 0.0159(4) Uani 1 1 d . . . C4A C -0.1924(3) -0.1026(3) 0.2034(3) 0.0203(6) Uani 1 1 d . . . H41A H -0.2779 -0.1624 0.1388 0.024 Uiso 1 1 d R . . H42A H -0.1953 -0.0141 0.2166 0.024 Uiso 1 1 d R . . H43A H -0.1919 -0.1461 0.2768 0.024 Uiso 1 1 d R . . C5A C -0.0508(3) -0.1923(3) 0.1244(2) 0.0162(5) Uani 1 1 d . . . O5A O -0.1455(2) -0.30847(19) 0.11740(17) 0.0189(4) Uani 1 1 d . . . N6A N 0.0717(2) -0.1690(2) 0.0866(2) 0.0165(4) Uani 1 1 d . . . C6A C 0.0821(3) -0.2896(3) 0.0384(3) 0.0206(6) Uani 1 1 d . . . H61A H 0.0192 -0.3723 0.0654 0.025 Uiso 1 1 d R . . H62A H 0.1825 -0.2778 0.0667 0.025 Uiso 1 1 d R . . H63A H 0.0514 -0.2991 -0.0491 0.025 Uiso 1 1 d R . . C7A C 0.1844(3) -0.0402(3) 0.0880(2) 0.0168(5) Uani 1 1 d . . . O7A O 0.2863(2) -0.0291(2) 0.05110(18) 0.0225(4) Uani 1 1 d . . . C7AA C 0.1650(3) 0.0705(3) 0.1359(2) 0.0158(5) Uani 1 1 d . . . N1B N 0.3672(2) 0.7346(2) 0.2822(2) 0.0162(4) Uani 1 1 d . . . N2B N 0.4870(2) 0.8002(2) 0.2492(2) 0.0179(5) Uani 1 1 d . . . N3B N 0.5392(2) 0.9379(2) 0.2750(2) 0.0174(5) Uani 1 1 d . . . C3AB C 0.4491(3) 0.9579(3) 0.3270(2) 0.0150(5) Uani 1 1 d . . . N4B N 0.4580(2) 1.0807(2) 0.3695(2) 0.0169(5) Uani 1 1 d . . . C4B C 0.5754(3) 1.2116(3) 0.3633(3) 0.0197(6) Uani 1 1 d . . . H41B H 0.6603 1.1970 0.3616 0.024 Uiso 1 1 d R . . H42B H 0.6007 1.2767 0.4334 0.024 Uiso 1 1 d R . . H43B H 0.5438 1.2488 0.2907 0.024 Uiso 1 1 d R . . C5B C 0.3540(3) 1.0824(3) 0.4181(2) 0.0178(5) Uani 1 1 d . . . O5B O 0.3564(2) 1.1894(2) 0.45682(18) 0.0230(4) Uani 1 1 d . . . N6B N 0.2427(2) 0.9543(2) 0.4214(2) 0.0174(5) Uani 1 1 d . . . C6B C 0.1342(3) 0.9590(3) 0.4756(3) 0.0235(6) Uani 1 1 d . . . H61B H 0.1778 0.9859 0.5620 0.028 Uiso 1 1 d R . . H62B H 0.0521 0.8681 0.4600 0.028 Uiso 1 1 d R . . H63B H 0.1003 1.0263 0.4409 0.028 Uiso 1 1 d R . . C7B C 0.2254(3) 0.8258(3) 0.3778(2) 0.0168(5) Uani 1 1 d . . . O7B O 0.1180(2) 0.7201(2) 0.38117(18) 0.0227(4) Uani 1 1 d . . . C7AB C 0.3402(3) 0.8330(3) 0.3317(2) 0.0150(5) Uani 1 1 d . . . N1P N 0.3104(2) 0.4634(2) 0.4637(2) 0.0149(4) Uani 1 1 d . . . C2P C 0.4423(3) 0.4829(3) 0.5306(2) 0.0136(5) Uani 1 1 d . . . N3P N 0.4786(2) 0.4739(2) 0.6474(2) 0.0140(4) Uani 1 1 d . . . C4P C 0.3743(3) 0.4412(3) 0.7017(2) 0.0175(5) Uani 1 1 d . . . H4P H 0.3969 0.4344 0.7849 0.021 Uiso 1 1 d R . . C5P C 0.2344(3) 0.4172(3) 0.6391(3) 0.0197(6) Uani 1 1 d . . . H5P H 0.1602 0.3926 0.6773 0.024 Uiso 1 1 d R . . C6P C 0.2067(3) 0.4303(3) 0.5189(3) 0.0184(5) Uani 1 1 d . . . H6P H 0.1118 0.4155 0.4740 0.022 Uiso 1 1 d R . . O1W O 0.3256(2) 0.5131(2) 0.07310(19) 0.0257(5) Uani 1 1 d D . . H11W H 0.268(3) 0.453(3) 0.016(2) 0.031 Uiso 1 1 d D . . H12W H 0.380(3) 0.578(3) 0.045(3) 0.031 Uiso 1 1 d D . . O2W O 0.0647(2) 0.4966(2) 0.23839(19) 0.0219(4) Uani 1 1 d D . . H21W H 0.000(3) 0.424(2) 0.252(3) 0.026 Uiso 1 1 d D . . H22W H 0.074(4) 0.566(2) 0.280(3) 0.026 Uiso 1 1 d D . . O3W O 0.6298(2) 0.1324(2) 0.1121(2) 0.0282(5) Uani 1 1 d D . . H31W H 0.645(4) 0.093(3) 0.058(2) 0.034 Uiso 1 1 d D . . H32W H 0.594(4) 0.069(3) 0.152(3) 0.034 Uiso 1 1 d D . . O4W O -0.1182(2) 0.2680(2) 0.2914(2) 0.0295(5) Uani 1 1 d D . . H41W H -0.192(3) 0.238(4) 0.230(2) 0.035 Uiso 1 1 d D . . H42W H -0.071(4) 0.226(3) 0.274(3) 0.035 Uiso 1 1 d D . . O5W O 0.5066(3) 0.3150(2) 0.0511(2) 0.0330(5) Uani 1 1 d D . . H51W H 0.537(4) 0.254(3) 0.061(4) 0.040 Uiso 1 1 d D . . H52W H 0.429(2) 0.294(4) 0.070(3) 0.040 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.01366(10) 0.01366(10) 0.01307(10) 0.00170(7) 0.00242(7) 0.00456(8) N1A 0.0167(11) 0.0164(11) 0.0148(11) 0.0022(9) 0.0019(9) 0.0061(9) N2A 0.0175(11) 0.0157(11) 0.0168(11) 0.0026(9) 0.0051(9) 0.0058(9) N3A 0.0144(11) 0.0156(11) 0.0175(11) 0.0014(9) 0.0040(9) 0.0035(9) C3AA 0.0161(12) 0.0151(12) 0.0118(12) 0.0017(10) 0.0017(10) 0.0063(10) N4A 0.0150(10) 0.0146(11) 0.0158(11) 0.0023(9) 0.0044(9) 0.0040(9) C4A 0.0189(13) 0.0185(13) 0.0215(14) 0.0013(11) 0.0080(11) 0.0048(11) C5A 0.0162(12) 0.0200(13) 0.0091(11) 0.0026(10) 0.0001(10) 0.0069(11) O5A 0.0208(10) 0.0155(9) 0.0156(9) 0.0011(7) 0.0043(8) 0.0038(8) N6A 0.0187(11) 0.0162(11) 0.0143(11) 0.0026(9) 0.0033(9) 0.0081(9) C6A 0.0256(14) 0.0189(13) 0.0188(14) 0.0020(11) 0.0048(11) 0.0118(12) C7A 0.0192(13) 0.0198(13) 0.0116(12) 0.0041(10) 0.0031(10) 0.0094(11) O7A 0.0232(10) 0.0246(11) 0.0231(11) 0.0025(8) 0.0109(9) 0.0111(9) C7AA 0.0144(12) 0.0173(13) 0.0130(12) 0.0037(10) 0.0031(10) 0.0047(10) N1B 0.0140(10) 0.0189(11) 0.0165(11) 0.0026(9) 0.0060(9) 0.0068(9) N2B 0.0167(11) 0.0176(11) 0.0203(12) 0.0033(9) 0.0083(9) 0.0066(9) N3B 0.0182(11) 0.0168(11) 0.0189(11) 0.0023(9) 0.0082(9) 0.0074(9) C3AB 0.0156(12) 0.0175(13) 0.0114(12) 0.0025(10) 0.0019(10) 0.0078(10) N4B 0.0172(11) 0.0158(11) 0.0163(11) 0.0015(9) 0.0044(9) 0.0061(9) C4B 0.0202(13) 0.0153(13) 0.0215(14) 0.0015(11) 0.0061(11) 0.0054(11) C5B 0.0187(13) 0.0206(14) 0.0135(12) 0.0014(10) 0.0009(10) 0.0101(11) O5B 0.0285(11) 0.0221(10) 0.0220(10) 0.0007(8) 0.0072(9) 0.0145(9) N6B 0.0161(11) 0.0244(12) 0.0146(11) 0.0023(9) 0.0048(9) 0.0111(10) C6B 0.0219(14) 0.0313(16) 0.0230(15) 0.0002(12) 0.0108(12) 0.0144(13) C7B 0.0157(12) 0.0205(13) 0.0125(12) 0.0020(10) 0.0019(10) 0.0075(11) O7B 0.0142(9) 0.0243(11) 0.0251(11) 0.0014(8) 0.0073(8) 0.0031(8) C7AB 0.0157(12) 0.0158(12) 0.0125(12) 0.0016(10) 0.0025(10) 0.0069(10) N1P 0.0141(10) 0.0148(10) 0.0139(10) 0.0014(8) 0.0038(9) 0.0045(9) C2P 0.0148(12) 0.0098(11) 0.0145(12) 0.0012(9) 0.0043(10) 0.0036(10) N3P 0.0147(10) 0.0112(10) 0.0150(10) 0.0019(8) 0.0048(9) 0.0042(8) C4P 0.0198(13) 0.0188(13) 0.0144(12) 0.0050(10) 0.0071(11) 0.0074(11) C5P 0.0168(13) 0.0209(14) 0.0217(14) 0.0057(11) 0.0091(11) 0.0063(11) C6P 0.0149(12) 0.0171(13) 0.0207(14) 0.0036(11) 0.0038(11) 0.0054(10) O1W 0.0287(12) 0.0187(10) 0.0173(10) -0.0013(8) 0.0082(9) -0.0023(9) O2W 0.0171(10) 0.0184(10) 0.0273(11) 0.0012(8) 0.0051(9) 0.0056(8) O3W 0.0301(12) 0.0268(12) 0.0308(12) 0.0043(9) 0.0161(10) 0.0109(10) O4W 0.0241(11) 0.0253(12) 0.0394(14) 0.0010(10) 0.0141(10) 0.0082(10) O5W 0.0336(13) 0.0315(13) 0.0426(14) 0.0141(11) 0.0227(11) 0.0152(11) _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 Cd O2W 2.271(2) . ? Cd O1W 2.281(2) . ? Cd N1B 2.306(2) . ? Cd N2A 2.309(2) . ? Cd N3P 2.364(2) 2_666 ? Cd N1P 2.431(2) . ? N1A N2A 1.317(3) . ? N1A C7AA 1.364(3) . ? N2A N3A 1.373(3) . ? N3A C3AA 1.335(3) . ? C3AA C7AA 1.377(4) . ? C3AA N4A 1.379(3) . ? N4A C5A 1.373(3) . ? N4A C4A 1.469(3) . ? C4A H41A 0.9800 . ? C4A H42A 0.9800 . ? C4A H43A 0.9800 . ? C5A O5A 1.224(3) . ? C5A N6A 1.406(3) . ? N6A C7A 1.405(3) . ? N6A C6A 1.471(3) . ? C6A H61A 0.9800 . ? C6A H62A 0.9800 . ? C6A H63A 0.9800 . ? C7A O7A 1.226(3) . ? C7A C7AA 1.426(4) . ? N1B N2B 1.334(3) . ? N1B C7AB 1.369(3) . ? N2B N3B 1.352(3) . ? N3B C3AB 1.343(3) . ? C3AB N4B 1.368(3) . ? C3AB C7AB 1.377(4) . ? N4B C5B 1.372(3) . ? N4B C4B 1.463(3) . ? C4B H41B 0.9800 . ? C4B H42B 0.9800 . ? C4B H43B 0.9800 . ? C5B O5B 1.225(3) . ? C5B N6B 1.406(4) . ? N6B C7B 1.395(4) . ? N6B C6B 1.468(3) . ? C6B H61B 0.9800 . ? C6B H62B 0.9800 . ? C6B H63B 0.9800 . ? C7B O7B 1.243(3) . ? C7B C7AB 1.429(4) . ? N1P C2P 1.339(3) . ? N1P C6P 1.343(3) . ? C2P N3P 1.334(3) . ? C2P C2P 1.494(5) 2_666 ? N3P C4P 1.342(3) . ? N3P Cd 2.364(2) 2_666 ? C4P C5P 1.383(4) . ? C4P H4P 0.9500 . ? C5P C6P 1.380(4) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? O1W H11W 0.836(10) . ? O1W H12W 0.837(10) . ? O2W H21W 0.847(10) . ? O2W H22W 0.848(10) . ? O3W H31W 0.850(10) . ? O3W H32W 0.847(10) . ? O4W H41W 0.850(10) . ? O4W H42W 0.853(10) . ? O5W H51W 0.846(10) . ? O5W H52W 0.843(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 O2W Cd O1W 109.49(8) . . ? O2W Cd N1B 84.33(7) . . ? O1W Cd N1B 89.24(8) . . ? O2W Cd N2A 92.18(8) . . ? O1W Cd N2A 84.71(8) . . ? N1B Cd N2A 171.60(8) . . ? O2W Cd N3P 157.12(8) . 2_666 ? O1W Cd N3P 92.27(8) . 2_666 ? N1B Cd N3P 89.14(7) . 2_666 ? N2A Cd N3P 96.91(8) . 2_666 ? O2W Cd N1P 89.83(7) . . ? O1W Cd N1P 160.13(8) . . ? N1B Cd N1P 97.48(8) . . ? N2A Cd N1P 90.13(8) . . ? N3P Cd N1P 69.27(7) 2_666 . ? N2A N1A C7AA 105.6(2) . . ? N1A N2A N3A 112.9(2) . . ? N1A N2A Cd 120.51(17) . . ? N3A N2A Cd 126.47(17) . . ? C3AA N3A N2A 104.0(2) . . ? N3A C3AA C7AA 109.8(2) . . ? N3A C3AA N4A 127.7(2) . . ? C7AA C3AA N4A 122.4(2) . . ? C5A N4A C3AA 119.0(2) . . ? C5A N4A C4A 118.4(2) . . ? C3AA N4A C4A 122.4(2) . . ? N4A C4A H41A 109.5 . . ? N4A C4A H42A 109.4 . . ? H41A C4A H42A 109.5 . . ? N4A C4A H43A 109.5 . . ? H41A C4A H43A 109.5 . . ? H42A C4A H43A 109.5 . . ? O5A C5A N4A 120.7(2) . . ? O5A C5A N6A 121.4(2) . . ? N4A C5A N6A 117.9(2) . . ? C7A N6A C5A 126.0(2) . . ? C7A N6A C6A 116.5(2) . . ? C5A N6A C6A 117.5(2) . . ? N6A C6A H61A 109.4 . . ? N6A C6A H62A 109.5 . . ? H61A C6A H62A 109.5 . . ? N6A C6A H63A 109.5 . . ? H61A C6A H63A 109.5 . . ? H62A C6A H63A 109.5 . . ? O7A C7A N6A 121.7(2) . . ? O7A C7A C7AA 125.8(3) . . ? N6A C7A C7AA 112.5(2) . . ? N1A C7AA C3AA 107.6(2) . . ? N1A C7AA C7A 130.3(2) . . ? C3AA C7AA C7A 122.1(2) . . ? N2B N1B C7AB 106.9(2) . . ? N2B N1B Cd 112.74(16) . . ? C7AB N1B Cd 140.01(18) . . ? N1B N2B N3B 111.2(2) . . ? C3AB N3B N2B 105.9(2) . . ? N3B C3AB N4B 127.5(2) . . ? N3B C3AB C7AB 109.5(2) . . ? N4B C3AB C7AB 123.0(2) . . ? C3AB N4B C5B 119.7(2) . . ? C3AB N4B C4B 121.6(2) . . ? C5B N4B C4B 118.7(2) . . ? N4B C4B H41B 109.5 . . ? N4B C4B H42B 109.5 . . ? H41B C4B H42B 109.5 . . ? N4B C4B H43B 109.5 . . ? H41B C4B H43B 109.5 . . ? H42B C4B H43B 109.5 . . ? O5B C5B N4B 122.3(3) . . ? O5B C5B N6B 120.9(3) . . ? N4B C5B N6B 116.8(2) . . ? C7B N6B C5B 126.5(2) . . ? C7B N6B C6B 117.8(2) . . ? C5B N6B C6B 115.6(2) . . ? N6B C6B H61B 109.5 . . ? N6B C6B H62B 109.5 . . ? H61B C6B H62B 109.5 . . ? N6B C6B H63B 109.5 . . ? H61B C6B H63B 109.5 . . ? H62B C6B H63B 109.5 . . ? O7B C7B N6B 120.3(2) . . ? O7B C7B C7AB 126.7(3) . . ? N6B C7B C7AB 113.0(2) . . ? N1B C7AB C3AB 106.5(2) . . ? N1B C7AB C7B 132.6(2) . . ? C3AB C7AB C7B 120.9(2) . . ? C2P N1P C6P 116.9(2) . . ? C2P N1P Cd 116.70(17) . . ? C6P N1P Cd 126.35(18) . . ? N3P C2P N1P 125.1(2) . . ? N3P C2P C2P 117.6(3) . 2_666 ? N1P C2P C2P 117.3(3) . 2_666 ? C2P N3P C4P 117.4(2) . . ? C2P N3P Cd 119.02(17) . 2_666 ? C4P N3P Cd 123.41(18) . 2_666 ? N3P C4P C5P 121.3(2) . . ? N3P C4P H4P 119.4 . . ? C5P C4P H4P 119.4 . . ? C6P C5P C4P 117.5(3) . . ? C6P C5P H5P 121.3 . . ? C4P C5P H5P 121.2 . . ? N1P C6P C5P 121.7(2) . . ? N1P C6P H6P 119.1 . . ? C5P C6P H6P 119.1 . . ? Cd O1W H11W 120(3) . . ? Cd O1W H12W 132(3) . . ? H11W O1W H12W 107(3) . . ? Cd O2W H21W 117(2) . . ? Cd O2W H22W 111(2) . . ? H21W O2W H22W 110(3) . . ? H31W O3W H32W 104(4) . . ? H41W O4W H42W 100(4) . . ? H51W O5W H52W 113(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W O5A 0.836(10) 1.943(11) 2.777(3) 176(4) 2 O1W H12W O5W 0.837(10) 1.900(14) 2.714(3) 164(4) 2_665 O2W H22W O7B 0.848(10) 1.851(11) 2.693(3) 172(3) . O2W H21W O4W 0.847(10) 1.786(11) 2.629(3) 173(4) . O3W H31W O7A 0.850(10) 1.875(13) 2.715(3) 169(4) 2_655 O3W H32W N3B 0.847(10) 2.042(13) 2.879(3) 169(4) 1_545 O4W H42W N3A 0.853(10) 1.954(13) 2.792(3) 167(4) . O4W H41W O3W 0.850(10) 1.901(14) 2.733(3) 166(4) 1_455 O5W H52W N1A 0.843(10) 2.222(14) 3.044(3) 165(4) . O5W H51W O3W 0.846(10) 1.944(13) 2.781(3) 170(4) . _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.535 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.095 # Attachment 'Cpd3_cuaxbpir.cif' data_cuaxbpir _database_code_depnum_ccdc_archive 'CCDC 732841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Cu2 N24 O8, 5(H2 O)' _chemical_formula_sum 'C32 H40 Cu2 N24 O13' _chemical_formula_weight 1095.96 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2470(13) _cell_length_b 10.8660(17) _cell_length_c 12.1170(19) _cell_angle_alpha 80.533(19) _cell_angle_beta 80.839(19) _cell_angle_gamma 88.072(19) _cell_volume 1057.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1757 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 23.5 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 70 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.3 _diffrn_reflns_number 7782 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.38 _reflns_number_total 3816 _reflns_number_gt 2916 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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^)+(0.0500P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3816 _refine_ls_number_parameters 330 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.28377(6) 0.52360(5) 0.08514(4) 0.02106(17) Uani 1 1 d . . . N1P N 0.0693(4) 0.4251(3) 0.1262(3) 0.0201(8) Uani 1 1 d . . . C2P C 0.0255(5) 0.3304(4) 0.2103(3) 0.0217(9) Uani 1 1 d . . . H2P H 0.0926 0.3081 0.2674 0.026 Uiso 1 1 d R . . C3P C -0.1168(5) 0.2643(4) 0.2148(3) 0.0246(10) Uani 1 1 d . . . H3P H -0.1470 0.1956 0.2732 0.030 Uiso 1 1 d R . . C4P C -0.2135(5) 0.3012(4) 0.1321(3) 0.0237(9) Uani 1 1 d . . . H4P H -0.3138 0.2594 0.1352 0.028 Uiso 1 1 d R . . N5P N -0.1676(4) 0.3956(3) 0.0470(3) 0.0205(8) Uani 1 1 d . . . C6P C -0.0267(5) 0.4501(3) 0.0478(3) 0.0184(9) Uani 1 1 d . . . N1A N 0.2596(4) 0.5434(3) 0.3189(3) 0.0286(8) Uani 1 1 d . . . N2A N 0.3292(4) 0.4788(3) 0.2399(3) 0.0260(8) Uani 1 1 d . . . N3A N 0.4064(4) 0.3724(3) 0.2803(3) 0.0265(8) Uani 1 1 d . . . C3AA C 0.3835(5) 0.3722(4) 0.3917(3) 0.0254(10) Uani 1 1 d . . . N4A N 0.4339(4) 0.2841(3) 0.4736(3) 0.0299(9) Uani 1 1 d . . . C4A C 0.5270(7) 0.1743(5) 0.4453(4) 0.0471(14) Uani 1 1 d . . . H41A H 0.5450 0.1773 0.3630 0.057 Uiso 1 1 d R . . H42A H 0.4655 0.0989 0.4818 0.057 Uiso 1 1 d R . . H43A H 0.6332 0.1727 0.4721 0.057 Uiso 1 1 d R . . C5A C 0.3907(5) 0.2964(4) 0.5852(4) 0.0290(10) Uani 1 1 d . . . O5A O 0.4237(4) 0.2167(3) 0.6610(3) 0.0383(8) Uani 1 1 d . . . N6A N 0.3051(4) 0.4049(3) 0.6086(3) 0.0285(8) Uani 1 1 d . . . C6A C 0.2624(7) 0.4126(5) 0.7289(4) 0.0415(12) Uani 1 1 d . . . H61A H 0.1765 0.3520 0.7639 0.050 Uiso 1 1 d R . . H62A H 0.2221 0.4969 0.7378 0.050 Uiso 1 1 d R . . H63A H 0.3599 0.3943 0.7658 0.050 Uiso 1 1 d R . . C7A C 0.2473(6) 0.4982(4) 0.5311(4) 0.0301(10) Uani 1 1 d . . . O7A O 0.1663(4) 0.5862(3) 0.5632(3) 0.0429(9) Uani 1 1 d . . . C7AA C 0.2934(5) 0.4761(4) 0.4170(3) 0.0263(10) Uani 1 1 d . . . N1B N 0.5428(4) 0.3502(3) -0.0455(3) 0.0203(7) Uani 1 1 d . . . N2B N 0.3883(4) 0.3694(3) 0.0001(3) 0.0210(8) Uani 1 1 d . . . N3B N 0.2911(4) 0.2747(3) -0.0075(3) 0.0219(8) Uani 1 1 d . . . C3AB C 0.3915(5) 0.1961(3) -0.0608(3) 0.0199(9) Uani 1 1 d . . . N4B N 0.3494(4) 0.0868(3) -0.0916(3) 0.0228(8) Uani 1 1 d . . . C4B C 0.1782(5) 0.0502(4) -0.0774(4) 0.0341(11) Uani 1 1 d . . . H41B H 0.1699 -0.0405 -0.0554 0.041 Uiso 1 1 d R . . H42B H 0.1360 0.0756 -0.1489 0.041 Uiso 1 1 d R . . H43B H 0.1136 0.0910 -0.0182 0.041 Uiso 1 1 d R . . C5B C 0.4676(5) 0.0239(4) -0.1546(3) 0.0261(10) Uani 1 1 d . . . O5B O 0.4352(4) -0.0679(3) -0.1919(3) 0.0420(9) Uani 1 1 d . . . N6B N 0.6297(4) 0.0668(3) -0.1717(3) 0.0237(8) Uani 1 1 d . . . C6B C 0.7518(6) -0.0058(4) -0.2369(4) 0.0360(12) Uani 1 1 d . . . H61B H 0.8624 0.0202 -0.2314 0.043 Uiso 1 1 d R . . H62B H 0.7360 0.0087 -0.3165 0.043 Uiso 1 1 d R . . H63B H 0.7385 -0.0948 -0.2064 0.043 Uiso 1 1 d R . . C7B C 0.6826(5) 0.1752(4) -0.1405(3) 0.0219(9) Uani 1 1 d . . . O7B O 0.8264(3) 0.2073(3) -0.1590(2) 0.0295(7) Uani 1 1 d . . . C7AB C 0.5479(5) 0.2395(4) -0.0844(3) 0.0191(9) Uani 1 1 d . . . O1W O 0.0101(5) 0.7455(4) 0.4022(3) 0.0533(10) Uani 1 1 d D . . H11W H 0.069(6) 0.747(5) 0.339(2) 0.064 Uiso 1 1 d D . . H12W H 0.053(7) 0.701(5) 0.453(4) 0.064 Uiso 1 1 d D . . O2W O 0.1742(5) 0.0179(4) 0.6288(4) 0.0779(14) Uani 1 1 d . . . O3W O 0.0670(13) 0.1185(10) 0.4494(9) 0.103(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0217(3) 0.0225(3) 0.0186(3) -0.0072(2) 0.00425(19) -0.0106(2) N1P 0.0187(18) 0.0217(18) 0.0194(18) -0.0078(15) 0.0042(14) -0.0064(14) C2P 0.024(2) 0.021(2) 0.019(2) -0.0057(17) 0.0045(17) -0.0051(17) C3P 0.025(2) 0.021(2) 0.025(2) -0.0062(18) 0.0094(18) -0.0062(18) C4P 0.024(2) 0.020(2) 0.026(2) -0.0081(18) 0.0032(18) -0.0097(18) N5P 0.0215(18) 0.0189(17) 0.0203(18) -0.0079(14) 0.0062(14) -0.0107(14) C6P 0.018(2) 0.016(2) 0.020(2) -0.0094(17) 0.0067(17) -0.0033(16) N1A 0.036(2) 0.027(2) 0.024(2) -0.0086(16) 0.0006(16) -0.0088(16) N2A 0.032(2) 0.028(2) 0.0174(18) -0.0049(16) 0.0026(15) -0.0153(16) N3A 0.027(2) 0.031(2) 0.0204(19) -0.0046(16) 0.0015(15) -0.0049(16) C3AA 0.022(2) 0.031(2) 0.023(2) -0.0085(19) 0.0050(18) -0.0125(18) N4A 0.035(2) 0.031(2) 0.0205(19) -0.0039(16) 0.0028(16) -0.0009(17) C4A 0.060(4) 0.044(3) 0.034(3) -0.010(2) 0.002(2) 0.017(3) C5A 0.024(2) 0.038(3) 0.024(2) -0.007(2) 0.0000(19) -0.005(2) O5A 0.045(2) 0.0397(19) 0.0279(18) -0.0044(15) -0.0017(15) 0.0076(16) N6A 0.036(2) 0.030(2) 0.0209(19) -0.0093(16) -0.0029(16) 0.0000(17) C6A 0.062(3) 0.041(3) 0.022(2) -0.010(2) -0.004(2) 0.006(3) C7A 0.035(3) 0.030(3) 0.025(2) -0.008(2) 0.000(2) -0.007(2) O7A 0.070(2) 0.0337(19) 0.0254(17) -0.0127(15) -0.0032(16) 0.0068(17) C7AA 0.033(2) 0.026(2) 0.019(2) -0.0042(18) -0.0001(18) -0.0100(19) N1B 0.0208(18) 0.0230(18) 0.0171(18) -0.0072(14) 0.0029(14) -0.0082(14) N2B 0.0222(19) 0.0225(18) 0.0177(17) -0.0066(14) 0.0042(14) -0.0102(14) N3B 0.0239(19) 0.0225(18) 0.0194(18) -0.0079(15) 0.0029(14) -0.0106(15) C3AB 0.025(2) 0.019(2) 0.016(2) -0.0045(17) 0.0017(17) -0.0113(17) N4B 0.0273(19) 0.0195(18) 0.0210(18) -0.0095(15) 0.0071(15) -0.0134(15) C4B 0.032(3) 0.034(3) 0.039(3) -0.020(2) 0.006(2) -0.019(2) C5B 0.038(3) 0.019(2) 0.020(2) -0.0055(18) 0.0044(19) -0.0106(19) O5B 0.053(2) 0.0295(18) 0.043(2) -0.0204(16) 0.0164(16) -0.0228(15) N6B 0.032(2) 0.0155(17) 0.0214(18) -0.0052(14) 0.0064(15) -0.0017(15) C6B 0.044(3) 0.021(2) 0.039(3) -0.012(2) 0.016(2) -0.005(2) C7B 0.029(2) 0.017(2) 0.018(2) -0.0024(16) 0.0002(18) -0.0003(18) O7B 0.0225(17) 0.0310(17) 0.0344(18) -0.0103(14) 0.0040(13) -0.0047(13) C7AB 0.022(2) 0.022(2) 0.014(2) -0.0080(17) -0.0004(16) -0.0048(17) O1W 0.052(3) 0.066(3) 0.038(2) -0.007(2) 0.0037(18) 0.000(2) O2W 0.064(3) 0.080(3) 0.091(3) -0.040(3) 0.016(2) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2A 1.951(3) . ? Cu N1B 1.963(3) 2_665 ? Cu N1P 2.048(3) . ? Cu N5P 2.055(3) 2_565 ? Cu N2B 2.191(3) . ? N1P C6P 1.320(5) . ? N1P C2P 1.338(5) . ? C2P C3P 1.385(5) . ? C2P H2P 0.9500 . ? C3P C4P 1.379(6) . ? C3P H3P 0.9500 . ? C4P N5P 1.346(5) . ? C4P H4P 0.9500 . ? N5P C6P 1.324(5) . ? N5P Cu 2.055(3) 2_565 ? C6P C6P 1.473(7) 2_565 ? N1A N2A 1.325(5) . ? N1A C7AA 1.353(5) . ? N2A N3A 1.359(5) . ? N3A C3AA 1.333(5) . ? C3AA N4A 1.366(5) . ? C3AA C7AA 1.380(6) . ? N4A C5A 1.370(5) . ? N4A C4A 1.457(6) . ? C4A H41A 0.9800 . ? C4A H42A 0.9800 . ? C4A H43A 0.9800 . ? C5A O5A 1.213(5) . ? C5A N6A 1.400(6) . ? N6A C7A 1.390(5) . ? N6A C6A 1.459(5) . ? C6A H61A 0.9800 . ? C6A H62A 0.9800 . ? C6A H63A 0.9800 . ? C7A O7A 1.229(5) . ? C7A C7AA 1.431(6) . ? N1B N2B 1.330(4) . ? N1B C7AB 1.359(5) . ? N1B Cu 1.963(3) 2_665 ? N2B N3B 1.349(4) . ? N3B C3AB 1.340(5) . ? C3AB C7AB 1.359(5) . ? C3AB N4B 1.373(5) . ? N4B C5B 1.375(5) . ? N4B C4B 1.455(5) . ? C4B H41B 0.9800 . ? C4B H42B 0.9800 . ? C4B H43B 0.9800 . ? C5B O5B 1.214(5) . ? C5B N6B 1.404(5) . ? N6B C7B 1.398(5) . ? N6B C6B 1.469(5) . ? C6B H61B 0.9800 . ? C6B H62B 0.9800 . ? C6B H63B 0.9800 . ? C7B O7B 1.223(5) . ? C7B C7AB 1.431(5) . ? O1W H11W 0.841(10) . ? O1W H12W 0.840(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 N2A Cu N1B 92.67(13) . 2_665 ? N2A Cu N1P 90.89(13) . . ? N1B Cu N1P 167.48(13) 2_665 . ? N2A Cu N5P 159.10(14) . 2_565 ? N1B Cu N5P 91.72(13) 2_665 2_565 ? N1P Cu N5P 80.85(13) . 2_565 ? N2A Cu N2B 104.48(14) . . ? N1B Cu N2B 103.60(12) 2_665 . ? N1P Cu N2B 87.09(12) . . ? N5P Cu N2B 94.30(12) 2_565 . ? C6P N1P C2P 117.1(3) . . ? C6P N1P Cu 112.7(2) . . ? C2P N1P Cu 129.5(3) . . ? N1P C2P C3P 120.7(4) . . ? N1P C2P H2P 119.7 . . ? C3P C2P H2P 119.6 . . ? C4P C3P C2P 118.1(4) . . ? C4P C3P H3P 120.9 . . ? C2P C3P H3P 121.0 . . ? N5P C4P C3P 120.9(4) . . ? N5P C4P H4P 119.5 . . ? C3P C4P H4P 119.5 . . ? C6P N5P C4P 116.5(3) . . ? C6P N5P Cu 112.6(3) . 2_565 ? C4P N5P Cu 130.8(3) . 2_565 ? N1P C6P N5P 126.6(3) . . ? N1P C6P C6P 116.9(4) . 2_565 ? N5P C6P C6P 116.5(4) . 2_565 ? N2A N1A C7AA 104.2(3) . . ? N1A N2A N3A 114.4(3) . . ? N1A N2A Cu 119.7(3) . . ? N3A N2A Cu 124.9(3) . . ? C3AA N3A N2A 103.2(3) . . ? N3A C3AA N4A 127.8(4) . . ? N3A C3AA C7AA 109.9(4) . . ? N4A C3AA C7AA 122.3(4) . . ? C3AA N4A C5A 119.5(4) . . ? C3AA N4A C4A 121.4(4) . . ? C5A N4A C4A 119.0(4) . . ? N4A C4A H41A 109.5 . . ? N4A C4A H42A 109.5 . . ? H41A C4A H42A 109.5 . . ? N4A C4A H43A 109.5 . . ? H41A C4A H43A 109.5 . . ? H42A C4A H43A 109.5 . . ? O5A C5A N4A 121.8(4) . . ? O5A C5A N6A 121.0(4) . . ? N4A C5A N6A 117.2(4) . . ? C7A N6A C5A 127.0(4) . . ? C7A N6A C6A 118.2(4) . . ? C5A N6A C6A 114.6(4) . . ? N6A C6A H61A 109.5 . . ? N6A C6A H62A 109.4 . . ? H61A C6A H62A 109.5 . . ? N6A C6A H63A 109.5 . . ? H61A C6A H63A 109.5 . . ? H62A C6A H63A 109.5 . . ? O7A C7A N6A 120.6(4) . . ? O7A C7A C7AA 127.3(4) . . ? N6A C7A C7AA 112.0(4) . . ? N1A C7AA C3AA 108.2(4) . . ? N1A C7AA C7A 129.9(4) . . ? C3AA C7AA C7A 121.9(4) . . ? N2B N1B C7AB 107.4(3) . . ? N2B N1B Cu 125.6(2) . 2_665 ? C7AB N1B Cu 125.3(3) . 2_665 ? N1B N2B N3B 111.1(3) . . ? N1B N2B Cu 129.2(2) . . ? N3B N2B Cu 119.6(2) . . ? C3AB N3B N2B 104.8(3) . . ? N3B C3AB C7AB 110.7(3) . . ? N3B C3AB N4B 127.1(3) . . ? C7AB C3AB N4B 122.1(4) . . ? C3AB N4B C5B 118.6(3) . . ? C3AB N4B C4B 120.8(3) . . ? C5B N4B C4B 119.6(3) . . ? N4B C4B H41B 109.5 . . ? N4B C4B H42B 109.4 . . ? H41B C4B H42B 109.5 . . ? N4B C4B H43B 109.5 . . ? H41B C4B H43B 109.5 . . ? H42B C4B H43B 109.5 . . ? O5B C5B N4B 121.7(4) . . ? O5B C5B N6B 120.5(4) . . ? N4B C5B N6B 117.7(3) . . ? C7B N6B C5B 126.6(3) . . ? C7B N6B C6B 117.8(3) . . ? C5B N6B C6B 115.5(3) . . ? N6B C6B H61B 109.4 . . ? N6B C6B H62B 109.5 . . ? H61B C6B H62B 109.5 . . ? N6B C6B H63B 109.5 . . ? H61B C6B H63B 109.5 . . ? H62B C6B H63B 109.5 . . ? O7B C7B N6B 122.9(4) . . ? O7B C7B C7AB 126.0(4) . . ? N6B C7B C7AB 111.0(3) . . ? N1B C7AB C3AB 106.0(3) . . ? N1B C7AB C7B 130.5(3) . . ? C3AB C7AB C7B 123.5(4) . . ? H11W O1W H12W 111(6) . . ? 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 O1W H12W O7A 0.840(10) 1.992(13) 2.829(5) 174(6) . O1W H11W O7B 0.841(10) 2.19(2) 3.008(5) 164(5) 2_665 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.922 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.086