# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Bharadwaj, Parimal' _publ_contact_author_email pkb@iitk.ac.in _publ_section_title ; Coordination polymers of various architectures built with mixed imidazole/benzimidazole and carboxylate donor ligands and different metal ions: syntheses, structural features and magnetic properties ; loop_ _publ_author_name A.Aijaz P.Lama E.C.Sanudo P.Bharadwaj # Attachment '- CIF.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 773576' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Cd N4 O4' _chemical_formula_sum 'C20 H14 Cd N4 O4' _chemical_formula_weight 486.76 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.571(3) _cell_length_b 16.443(5) _cell_length_c 8.265(4) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 1844.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.49 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8287 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22242 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1720 _reflns_number_gt 1496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+7.3143P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1720 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Cd1 Cd 0.76229(2) 0.2500 0.2500 0.02545(14) Uani 1 2 d S . . O1 O 0.8112(3) 0.7092(3) 1.0183(5) 0.0846(16) Uani 1 1 d . . . O2 O 0.8158(3) 0.6171(3) 1.2103(4) 0.0714(13) Uani 1 1 d . . . N1 N 0.8805(2) 0.3196(2) 0.3842(4) 0.0377(8) Uani 1 1 d . . . N2 N 0.9148(2) 0.3960(3) 0.5952(5) 0.0499(11) Uani 1 1 d . . . C1 C 0.9608(3) 0.2877(3) 0.4634(5) 0.0388(10) Uani 1 1 d . . . H1 H 0.9950 0.2414 0.4320 0.047 Uiso 1 1 calc R . . C2 C 0.9824(3) 0.3340(3) 0.5943(6) 0.0543(14) Uani 1 1 d . . . H2 H 1.0328 0.3255 0.6685 0.065 Uiso 1 1 calc R . . C3 C 0.8553(3) 0.3857(3) 0.4660(5) 0.0445(11) Uani 1 1 d . . . H3 H 0.8037 0.4202 0.4382 0.053 Uiso 1 1 calc R . . C4 C 0.9010(3) 0.4584(4) 0.7149(6) 0.0573(16) Uani 1 1 d . . . C5 C 0.8985(3) 0.4360(4) 0.8768(6) 0.0596(16) Uani 1 1 d . . . H5 H 0.9108 0.3826 0.9079 0.072 Uiso 1 1 calc R . . C6 C 0.8773(3) 0.4955(4) 0.9916(7) 0.0642(17) Uani 1 1 d . . . H6 H 0.8751 0.4819 1.1008 0.077 Uiso 1 1 calc R . . C7 C 0.8596(3) 0.5747(4) 0.9442(7) 0.0631(18) Uani 1 1 d . . . C8 C 0.8647(4) 0.5963(4) 0.7815(7) 0.0678(19) Uani 1 1 d . . . H8 H 0.8539 0.6498 0.7499 0.081 Uiso 1 1 calc R . . C9 C 0.8864(4) 0.5368(4) 0.6665(7) 0.0675(18) Uani 1 1 d . . . H9 H 0.8909 0.5505 0.5576 0.081 Uiso 1 1 calc R . . C10 C 0.8276(3) 0.6380(4) 1.0656(7) 0.0668(19) 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 Cd1 0.0183(2) 0.0415(2) 0.0165(2) 0.01081(14) 0.000 0.000 O1 0.094(3) 0.076(3) 0.084(3) -0.044(2) 0.067(3) -0.053(2) O2 0.0467(19) 0.116(3) 0.051(2) -0.050(2) -0.0134(16) 0.033(2) N1 0.0352(18) 0.0462(19) 0.0316(18) -0.0195(15) -0.0045(15) 0.0115(15) N2 0.0268(17) 0.076(3) 0.047(2) -0.044(2) 0.0055(16) -0.0037(17) C1 0.0247(18) 0.060(2) 0.032(2) -0.0219(19) -0.0015(16) 0.0086(18) C2 0.0205(19) 0.099(4) 0.044(3) -0.040(3) -0.0054(18) 0.009(2) C3 0.039(2) 0.056(3) 0.038(2) -0.024(2) 0.0007(19) 0.012(2) C4 0.0230(19) 0.089(4) 0.060(3) -0.042(3) 0.0146(19) -0.016(2) C5 0.0184(18) 0.102(4) 0.059(3) -0.037(3) 0.0005(19) -0.002(2) C6 0.0172(18) 0.114(5) 0.061(3) -0.045(3) 0.002(2) -0.003(2) C7 0.0201(19) 0.097(4) 0.072(4) -0.025(3) 0.018(2) -0.024(2) C8 0.044(3) 0.081(4) 0.079(4) -0.041(3) 0.038(3) -0.036(3) C9 0.051(3) 0.084(4) 0.068(4) -0.039(3) 0.036(3) -0.035(3) C10 0.0171(19) 0.110(5) 0.073(4) -0.025(4) 0.016(2) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.261(3) 2_664 ? Cd1 O1 2.261(3) 4_646 ? Cd1 N1 2.261(3) . ? Cd1 N1 2.261(3) 3 ? Cd1 O2 2.451(4) 4_646 ? Cd1 O2 2.451(4) 2_664 ? Cd1 C10 2.684(5) 4_646 ? Cd1 C10 2.684(5) 2_664 ? O1 C10 1.254(8) . ? O1 Cd1 2.261(3) 2_666 ? O2 C10 1.255(8) . ? O2 Cd1 2.451(4) 2_666 ? N1 C3 1.325(5) . ? N1 C1 1.374(5) . ? N2 C3 1.350(6) . ? N2 C2 1.371(6) . ? N2 C4 1.438(5) . ? C1 C2 1.355(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C9 1.365(9) . ? C4 C5 1.388(8) . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 C7 1.380(9) . ? C6 H6 0.9300 . ? C7 C8 1.393(9) . ? C7 C10 1.509(6) . ? C8 C9 1.395(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 Cd1 2.684(5) 2_666 ? 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 Cd1 O1 127.7(2) 2_664 4_646 ? O1 Cd1 N1 125.31(13) 2_664 . ? O1 Cd1 N1 92.74(17) 4_646 . ? O1 Cd1 N1 92.74(17) 2_664 3 ? O1 Cd1 N1 125.31(13) 4_646 3 ? N1 Cd1 N1 89.59(16) . 3 ? O1 Cd1 O2 100.82(11) 2_664 4_646 ? O1 Cd1 O2 55.34(16) 4_646 4_646 ? N1 Cd1 O2 133.81(12) . 4_646 ? N1 Cd1 O2 85.47(14) 3 4_646 ? O1 Cd1 O2 55.34(16) 2_664 2_664 ? O1 Cd1 O2 100.82(11) 4_646 2_664 ? N1 Cd1 O2 85.47(14) . 2_664 ? N1 Cd1 O2 133.81(12) 3 2_664 ? O2 Cd1 O2 128.79(19) 4_646 2_664 ? O1 Cd1 C10 118.97(14) 2_664 4_646 ? O1 Cd1 C10 27.72(19) 4_646 4_646 ? N1 Cd1 C10 113.03(17) . 4_646 ? N1 Cd1 C10 104.70(16) 3 4_646 ? O2 Cd1 C10 27.82(19) 4_646 4_646 ? O2 Cd1 C10 119.45(13) 2_664 4_646 ? O1 Cd1 C10 27.72(19) 2_664 2_664 ? O1 Cd1 C10 118.97(14) 4_646 2_664 ? N1 Cd1 C10 104.70(16) . 2_664 ? N1 Cd1 C10 113.03(17) 3 2_664 ? O2 Cd1 C10 119.45(13) 4_646 2_664 ? O2 Cd1 C10 27.82(19) 2_664 2_664 ? C10 Cd1 C10 125.94(17) 4_646 2_664 ? C10 O1 Cd1 95.3(3) . 2_666 ? C10 O2 Cd1 86.5(4) . 2_666 ? C3 N1 C1 105.9(3) . . ? C3 N1 Cd1 118.8(3) . . ? C1 N1 Cd1 127.1(3) . . ? C3 N2 C2 107.6(3) . . ? C3 N2 C4 123.8(4) . . ? C2 N2 C4 128.4(4) . . ? C2 C1 N1 109.8(4) . . ? C2 C1 H1 125.1 . . ? N1 C1 H1 125.1 . . ? C1 C2 N2 106.1(4) . . ? C1 C2 H2 127.0 . . ? N2 C2 H2 127.0 . . ? N1 C3 N2 110.6(4) . . ? N1 C3 H3 124.7 . . ? N2 C3 H3 124.7 . . ? C9 C4 C5 122.0(4) . . ? C9 C4 N2 119.4(5) . . ? C5 C4 N2 118.5(5) . . ? C4 C5 C6 118.4(6) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C7 C6 C5 120.3(6) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.4(4) . . ? C6 C7 C10 120.8(6) . . ? C8 C7 C10 118.7(6) . . ? C7 C8 C9 119.3(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C4 C9 C8 119.5(6) . . ? C4 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? O1 C10 O2 122.0(4) . . ? O1 C10 C7 119.2(6) . . ? O2 C10 C7 118.8(6) . . ? O1 C10 Cd1 57.0(2) . 2_666 ? O2 C10 Cd1 65.7(3) . 2_666 ? C7 C10 Cd1 168.9(3) . 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 N1 C3 73.4(4) 2_664 . . . ? O1 Cd1 N1 C3 -68.2(3) 4_646 . . . ? N1 Cd1 N1 C3 166.5(4) 3 . . . ? O2 Cd1 N1 C3 -110.2(4) 4_646 . . . ? O2 Cd1 N1 C3 32.5(3) 2_664 . . . ? C10 Cd1 N1 C3 -87.7(4) 4_646 . . . ? C10 Cd1 N1 C3 52.8(4) 2_664 . . . ? O1 Cd1 N1 C1 -142.7(3) 2_664 . . . ? O1 Cd1 N1 C1 75.7(3) 4_646 . . . ? N1 Cd1 N1 C1 -49.6(3) 3 . . . ? O2 Cd1 N1 C1 33.7(4) 4_646 . . . ? O2 Cd1 N1 C1 176.4(3) 2_664 . . . ? C10 Cd1 N1 C1 56.2(4) 4_646 . . . ? C10 Cd1 N1 C1 -163.4(3) 2_664 . . . ? C3 N1 C1 C2 1.1(5) . . . . ? Cd1 N1 C1 C2 -146.4(3) . . . . ? N1 C1 C2 N2 -0.5(6) . . . . ? C3 N2 C2 C1 -0.3(6) . . . . ? C4 N2 C2 C1 175.1(5) . . . . ? C1 N1 C3 N2 -1.3(5) . . . . ? Cd1 N1 C3 N2 149.5(3) . . . . ? C2 N2 C3 N1 1.0(6) . . . . ? C4 N2 C3 N1 -174.7(4) . . . . ? C3 N2 C4 C9 -49.1(6) . . . . ? C2 N2 C4 C9 136.2(5) . . . . ? C3 N2 C4 C5 128.0(5) . . . . ? C2 N2 C4 C5 -46.7(6) . . . . ? C9 C4 C5 C6 2.1(6) . . . . ? N2 C4 C5 C6 -175.0(4) . . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C5 C6 C7 C8 -1.4(6) . . . . ? C5 C6 C7 C10 174.5(4) . . . . ? C6 C7 C8 C9 1.1(7) . . . . ? C10 C7 C8 C9 -174.8(4) . . . . ? C5 C4 C9 C8 -2.4(7) . . . . ? N2 C4 C9 C8 174.6(4) . . . . ? C7 C8 C9 C4 0.8(7) . . . . ? Cd1 O1 C10 O2 -10.2(5) 2_666 . . . ? Cd1 O1 C10 C7 167.8(3) 2_666 . . . ? Cd1 O2 C10 O1 9.4(4) 2_666 . . . ? Cd1 O2 C10 C7 -168.7(3) 2_666 . . . ? C6 C7 C10 O1 -179.3(4) . . . . ? C8 C7 C10 O1 -3.4(6) . . . . ? C6 C7 C10 O2 -1.2(6) . . . . ? C8 C7 C10 O2 174.7(4) . . . . ? C6 C7 C10 Cd1 -112(3) . . . 2_666 ? C8 C7 C10 Cd1 63(3) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.051 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.092 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 773577' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 Cd N6 O10' _chemical_formula_sum 'C34 H40 Cd N6 O10' _chemical_formula_weight 805.13 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.290(2) _cell_length_b 16.292(5) _cell_length_c 13.675(4) _cell_angle_alpha 90.000 _cell_angle_beta 120.330(4) _cell_angle_gamma 90.000 _cell_volume 3517.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8981 _exptl_absorpt_correction_T_max 0.9345 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9899 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3625 _reflns_number_gt 3418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The three restraints applied are: DFIX and DANG option to fix the O-H distance and H-O-H angle in water OW1. ; _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^)+(0.0506P)^2^+7.1182P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3625 _refine_ls_number_parameters 249 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Cd1 Cd 0.5000 0.148438(13) 0.7500 0.01191(10) Uani 1 2 d S . . O1 O 0.85745(10) -0.31923(10) 0.65899(14) 0.0165(4) Uani 1 1 d . . . O2 O 0.94258(11) -0.24622(10) 0.81095(15) 0.0172(4) Uani 1 1 d . . . O3 O 0.93940(12) 0.12779(12) 0.56959(16) 0.0232(4) Uani 1 1 d . . . N1 N 0.51669(13) 0.04429(12) 0.65101(17) 0.0144(4) Uani 1 1 d . . . N2 N 0.58689(12) -0.06844(12) 0.65424(17) 0.0135(4) Uani 1 1 d . . . N3 N 0.88815(14) 0.08553(13) 0.68161(19) 0.0206(5) Uani 1 1 d . . . C1 C 0.59160(15) 0.01243(14) 0.6820(2) 0.0146(5) Uani 1 1 d . . . H1 H 0.6420 0.0419 0.7187 0.017 Uiso 1 1 calc R . . C2 C 0.45896(15) -0.01994(14) 0.6004(2) 0.0143(5) Uani 1 1 d . . . C3 C 0.37159(15) -0.02050(15) 0.5555(2) 0.0174(5) Uani 1 1 d . . . H3 H 0.3424 0.0266 0.5542 0.021 Uiso 1 1 calc R . . C4 C 0.33017(16) -0.09438(16) 0.5129(2) 0.0195(5) Uani 1 1 d . . . H4 H 0.2718 -0.0969 0.4820 0.023 Uiso 1 1 calc R . . C5 C 0.37427(17) -0.16568(16) 0.5154(2) 0.0198(5) Uani 1 1 d . . . H5 H 0.3443 -0.2142 0.4863 0.024 Uiso 1 1 calc R . . C6 C 0.46067(16) -0.16575(15) 0.5598(2) 0.0172(5) Uani 1 1 d . . . H6 H 0.4898 -0.2131 0.5617 0.021 Uiso 1 1 calc R . . C7 C 0.50218(15) -0.09133(14) 0.6018(2) 0.0142(5) Uani 1 1 d . . . C8 C 0.65789(15) -0.11857(14) 0.6755(2) 0.0141(5) Uani 1 1 d . . . C9 C 0.64914(16) -0.17212(15) 0.5907(2) 0.0175(5) Uani 1 1 d . . . H9 H 0.5980 -0.1760 0.5228 0.021 Uiso 1 1 calc R . . C10 C 0.71803(15) -0.21936(15) 0.6096(2) 0.0152(5) Uani 1 1 d . . . H10 H 0.7131 -0.2556 0.5541 0.018 Uiso 1 1 calc R . . C11 C 0.79490(15) -0.21289(14) 0.7116(2) 0.0146(5) Uani 1 1 d . . . C12 C 0.80241(16) -0.15867(14) 0.7952(2) 0.0150(5) Uani 1 1 d . . . H12 H 0.8536 -0.1540 0.8630 0.018 Uiso 1 1 calc R . . C13 C 0.73332(15) -0.11174(14) 0.7768(2) 0.0152(5) Uani 1 1 d . . . H13 H 0.7378 -0.0759 0.8325 0.018 Uiso 1 1 calc R . . C14 C 0.86991(15) -0.26228(14) 0.7288(2) 0.0136(5) Uani 1 1 d . . . C15 C 0.86545(19) 0.01744(18) 0.7301(2) 0.0292(6) Uani 1 1 d . . . H15A H 0.8074 0.0230 0.7109 0.044 Uiso 1 1 calc R . . H15B H 0.9014 0.0178 0.8110 0.044 Uiso 1 1 calc R . . H15C H 0.8726 -0.0334 0.7003 0.044 Uiso 1 1 calc R . . C16 C 0.87681(18) 0.16804(18) 0.7135(2) 0.0254(6) Uani 1 1 d . . . H16A H 0.9045 0.1719 0.7945 0.038 Uiso 1 1 calc R . . H16B H 0.8175 0.1791 0.6811 0.038 Uiso 1 1 calc R . . H16C H 0.9011 0.2074 0.6858 0.038 Uiso 1 1 calc R . . C17 C 0.91907(16) 0.07308(16) 0.6134(2) 0.0205(5) Uani 1 1 d . . . H17 H 0.9259 0.0190 0.5975 0.025 Uiso 1 1 calc R . . OW1 O 0.78506(13) -0.06905(12) 0.4192(2) 0.0322(5) Uani 1 1 d D . . OW2 O 0.95845(13) -0.11947(14) 0.5297(2) 0.0269(4) Uani 1 1 d . . . H1W1 H 0.7510(19) -0.1082(18) 0.405(3) 0.046(11) Uiso 1 1 d D . . H2W1 H 0.8337(15) -0.089(2) 0.441(4) 0.064(14) Uiso 1 1 d D . . H1W2 H 0.982(3) -0.153(2) 0.574(4) 0.046(13) Uiso 1 1 d . . . H2W2 H 0.984(2) -0.1181(19) 0.501(3) 0.022(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.00996(15) 0.00880(14) 0.01848(15) 0.000 0.00829(11) 0.000 O1 0.0123(8) 0.0155(8) 0.0200(8) -0.0025(7) 0.0068(7) 0.0037(7) O2 0.0133(9) 0.0147(8) 0.0233(9) -0.0028(7) 0.0090(7) 0.0009(6) O3 0.0205(9) 0.0281(10) 0.0201(9) 0.0039(8) 0.0097(8) -0.0003(8) N1 0.0144(10) 0.0129(9) 0.0181(10) 0.0002(8) 0.0098(8) 0.0009(8) N2 0.0118(9) 0.0114(9) 0.0176(10) -0.0011(7) 0.0077(8) 0.0014(7) N3 0.0179(11) 0.0210(11) 0.0217(11) 0.0019(8) 0.0089(9) -0.0003(8) C1 0.0145(11) 0.0133(11) 0.0187(11) -0.0014(9) 0.0104(10) 0.0000(9) C2 0.0140(11) 0.0118(11) 0.0172(11) 0.0005(8) 0.0079(9) 0.0009(8) C3 0.0158(12) 0.0160(11) 0.0209(12) 0.0002(9) 0.0096(10) 0.0029(9) C4 0.0120(12) 0.0230(13) 0.0197(12) -0.0025(10) 0.0052(10) -0.0016(9) C5 0.0182(13) 0.0180(12) 0.0199(12) -0.0035(10) 0.0072(11) -0.0037(10) C6 0.0183(12) 0.0140(11) 0.0199(12) -0.0018(9) 0.0100(10) 0.0015(9) C7 0.0146(11) 0.0156(11) 0.0152(11) 0.0011(9) 0.0096(9) 0.0024(9) C8 0.0152(12) 0.0107(11) 0.0195(12) 0.0026(9) 0.0110(10) 0.0032(9) C9 0.0163(12) 0.0156(11) 0.0202(12) 0.0008(9) 0.0089(10) 0.0031(9) C10 0.0168(12) 0.0165(11) 0.0136(11) -0.0007(9) 0.0086(10) 0.0032(9) C11 0.0138(12) 0.0112(11) 0.0224(12) 0.0025(9) 0.0117(10) 0.0032(9) C12 0.0108(12) 0.0133(11) 0.0190(12) 0.0010(9) 0.0062(10) 0.0005(8) C13 0.0177(12) 0.0120(11) 0.0200(12) -0.0015(9) 0.0125(10) 0.0013(9) C14 0.0125(11) 0.0125(11) 0.0167(11) 0.0042(8) 0.0082(9) 0.0027(8) C15 0.0291(15) 0.0290(15) 0.0302(15) 0.0051(12) 0.0154(13) -0.0056(12) C16 0.0247(14) 0.0266(14) 0.0249(14) -0.0015(11) 0.0126(12) 0.0027(11) C17 0.0158(12) 0.0200(12) 0.0206(12) -0.0005(10) 0.0056(10) -0.0004(10) OW1 0.0188(10) 0.0191(10) 0.0555(14) 0.0059(9) 0.0163(10) 0.0035(8) OW2 0.0212(10) 0.0300(11) 0.0329(11) 0.0107(9) 0.0160(10) 0.0087(9) _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 Cd1 N1 2.285(2) . ? Cd1 N1 2.285(2) 2_656 ? Cd1 O1 2.3124(17) 4_656 ? Cd1 O1 2.3124(17) 3_455 ? Cd1 O2 2.3722(18) 4_656 ? Cd1 O2 2.3722(18) 3_455 ? Cd1 C14 2.677(2) 4_656 ? Cd1 C14 2.677(2) 3_455 ? O1 C14 1.267(3) . ? O1 Cd1 2.3124(17) 3_545 ? O2 C14 1.261(3) . ? O2 Cd1 2.3722(17) 3_545 ? O3 C17 1.231(3) . ? N1 C1 1.319(3) . ? N1 C2 1.397(3) . ? N2 C1 1.362(3) . ? N2 C7 1.390(3) . ? N2 C8 1.434(3) . ? N3 C17 1.329(4) . ? N3 C15 1.456(3) . ? N3 C16 1.460(4) . ? C2 C3 1.393(3) . ? C2 C7 1.401(3) . ? C3 C4 1.384(4) . ? C4 C5 1.405(4) . ? C5 C6 1.377(4) . ? C6 C7 1.391(3) . ? C8 C13 1.380(4) . ? C8 C9 1.394(4) . ? C9 C10 1.385(3) . ? C10 C11 1.397(3) . ? C11 C12 1.395(3) . ? C11 C14 1.503(3) . ? C12 C13 1.387(3) . ? C14 Cd1 2.677(2) 3_545 ? 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 N1 Cd1 N1 84.11(10) . 2_656 ? N1 Cd1 O1 92.08(7) . 4_656 ? N1 Cd1 O1 107.57(7) 2_656 4_656 ? N1 Cd1 O1 107.57(7) . 3_455 ? N1 Cd1 O1 92.08(7) 2_656 3_455 ? O1 Cd1 O1 153.67(9) 4_656 3_455 ? N1 Cd1 O2 96.53(7) . 4_656 ? N1 Cd1 O2 163.87(7) 2_656 4_656 ? O1 Cd1 O2 56.32(6) 4_656 4_656 ? O1 Cd1 O2 103.00(6) 3_455 4_656 ? N1 Cd1 O2 163.87(7) . 3_455 ? N1 Cd1 O2 96.53(7) 2_656 3_455 ? O1 Cd1 O2 103.00(6) 4_656 3_455 ? O1 Cd1 O2 56.32(6) 3_455 3_455 ? O2 Cd1 O2 87.31(9) 4_656 3_455 ? N1 Cd1 C14 95.18(7) . 4_656 ? N1 Cd1 C14 135.78(7) 2_656 4_656 ? O1 Cd1 C14 28.23(7) 4_656 4_656 ? O1 Cd1 C14 129.31(7) 3_455 4_656 ? O2 Cd1 C14 28.09(7) 4_656 4_656 ? O2 Cd1 C14 95.50(7) 3_455 4_656 ? N1 Cd1 C14 135.78(7) . 3_455 ? N1 Cd1 C14 95.18(7) 2_656 3_455 ? O1 Cd1 C14 129.31(7) 4_656 3_455 ? O1 Cd1 C14 28.23(7) 3_455 3_455 ? O2 Cd1 C14 95.50(7) 4_656 3_455 ? O2 Cd1 C14 28.09(7) 3_455 3_455 ? C14 Cd1 C14 114.17(10) 4_656 3_455 ? C14 O1 Cd1 92.08(14) . 3_545 ? C14 O2 Cd1 89.51(14) . 3_545 ? C1 N1 C2 105.5(2) . . ? C1 N1 Cd1 121.99(16) . . ? C2 N1 Cd1 123.78(15) . . ? C1 N2 C7 107.49(19) . . ? C1 N2 C8 124.8(2) . . ? C7 N2 C8 127.7(2) . . ? C17 N3 C15 121.6(2) . . ? C17 N3 C16 121.7(2) . . ? C15 N3 C16 116.7(2) . . ? N1 C1 N2 112.5(2) . . ? C3 C2 N1 129.5(2) . . ? C3 C2 C7 121.0(2) . . ? N1 C2 C7 109.6(2) . . ? C4 C3 C2 117.0(2) . . ? C3 C4 C5 121.5(2) . . ? C6 C5 C4 121.9(2) . . ? C5 C6 C7 116.5(2) . . ? C6 C7 N2 132.9(2) . . ? C6 C7 C2 122.1(2) . . ? N2 C7 C2 105.0(2) . . ? C13 C8 C9 121.5(2) . . ? C13 C8 N2 120.1(2) . . ? C9 C8 N2 118.4(2) . . ? C10 C9 C8 118.8(2) . . ? C9 C10 C11 120.4(2) . . ? C12 C11 C10 119.9(2) . . ? C12 C11 C14 120.4(2) . . ? C10 C11 C14 119.6(2) . . ? C13 C12 C11 119.8(2) . . ? C8 C13 C12 119.6(2) . . ? O2 C14 O1 122.1(2) . . ? O2 C14 C11 119.8(2) . . ? O1 C14 C11 118.1(2) . . ? O2 C14 Cd1 62.40(12) . 3_545 ? O1 C14 Cd1 59.69(12) . 3_545 ? C11 C14 Cd1 177.57(17) . 3_545 ? O3 C17 N3 124.8(3) . . ? 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 N1 Cd1 N1 C1 -89.99(19) 2_656 . . . ? O1 Cd1 N1 C1 17.47(19) 4_656 . . . ? O1 Cd1 N1 C1 179.69(18) 3_455 . . . ? O2 Cd1 N1 C1 73.80(19) 4_656 . . . ? O2 Cd1 N1 C1 176.9(2) 3_455 . . . ? C14 Cd1 N1 C1 45.58(19) 4_656 . . . ? C14 Cd1 N1 C1 178.63(16) 3_455 . . . ? N1 Cd1 N1 C2 52.83(16) 2_656 . . . ? O1 Cd1 N1 C2 160.29(18) 4_656 . . . ? O1 Cd1 N1 C2 -37.49(19) 3_455 . . . ? O2 Cd1 N1 C2 -143.38(18) 4_656 . . . ? O2 Cd1 N1 C2 -40.3(3) 3_455 . . . ? C14 Cd1 N1 C2 -171.59(18) 4_656 . . . ? C14 Cd1 N1 C2 -38.5(2) 3_455 . . . ? C2 N1 C1 N2 0.5(3) . . . . ? Cd1 N1 C1 N2 149.09(16) . . . . ? C7 N2 C1 N1 -0.5(3) . . . . ? C8 N2 C1 N1 178.8(2) . . . . ? C1 N1 C2 C3 178.2(3) . . . . ? Cd1 N1 C2 C3 30.3(3) . . . . ? C1 N1 C2 C7 -0.3(3) . . . . ? Cd1 N1 C2 C7 -148.17(16) . . . . ? N1 C2 C3 C4 -178.3(2) . . . . ? C7 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? C5 C6 C7 N2 178.1(3) . . . . ? C5 C6 C7 C2 0.7(4) . . . . ? C1 N2 C7 C6 -177.5(3) . . . . ? C8 N2 C7 C6 3.2(4) . . . . ? C1 N2 C7 C2 0.3(3) . . . . ? C8 N2 C7 C2 -179.0(2) . . . . ? C3 C2 C7 C6 -0.6(4) . . . . ? N1 C2 C7 C6 178.1(2) . . . . ? C3 C2 C7 N2 -178.6(2) . . . . ? N1 C2 C7 N2 0.0(3) . . . . ? C1 N2 C8 C13 41.2(3) . . . . ? C7 N2 C8 C13 -139.6(2) . . . . ? C1 N2 C8 C9 -137.2(2) . . . . ? C7 N2 C8 C9 41.9(4) . . . . ? C13 C8 C9 C10 0.1(4) . . . . ? N2 C8 C9 C10 178.5(2) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C9 C10 C11 C14 -177.7(2) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C14 C11 C12 C13 178.2(2) . . . . ? C9 C8 C13 C12 0.4(4) . . . . ? N2 C8 C13 C12 -178.0(2) . . . . ? C11 C12 C13 C8 -0.6(4) . . . . ? Cd1 O2 C14 O1 1.1(2) 3_545 . . . ? Cd1 O2 C14 C11 -178.78(19) 3_545 . . . ? Cd1 O1 C14 O2 -1.1(2) 3_545 . . . ? Cd1 O1 C14 C11 178.75(18) 3_545 . . . ? C12 C11 C14 O2 -10.4(3) . . . . ? C10 C11 C14 O2 167.4(2) . . . . ? C12 C11 C14 O1 169.7(2) . . . . ? C10 C11 C14 O1 -12.5(3) . . . . ? C15 N3 C17 O3 179.9(2) . . . . ? C16 N3 C17 O3 -1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.683 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.192 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 773578' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Cu N4 O4' _chemical_formula_sum 'C20 H14 Cu N4 O4' _chemical_formula_weight 437.90 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 Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.494(5) _cell_length_b 23.494(5) _cell_length_c 10.003(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_volume 4782(2) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.00 _exptl_crystal_description cubic _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2007 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8488 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7426 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2563 _reflns_number_gt 1748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2563 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 0.5000 0.0000 0.0000 0.0124(3) Uani 1 2 d S . . O1 O 0.08448(14) -0.41707(14) 0.0132(3) 0.0153(6) Uani 1 1 d . . . O2 O 0.04680(15) -0.40502(15) -0.1832(3) 0.0192(7) Uani 1 1 d . . . N1 N 0.41028(17) -0.04510(17) -0.0762(4) 0.0152(7) Uani 1 1 d . . . N2 N 0.30905(17) -0.12443(18) -0.1135(4) 0.0157(7) Uani 1 1 d . . . C1 C 0.3760(2) -0.0192(2) -0.1425(5) 0.0165(8) Uani 1 1 d . . . H1 H 0.3933 0.0247 -0.1662 0.020 Uiso 1 1 calc R . . C2 C 0.3141(2) -0.0674(2) -0.1669(4) 0.0167(8) Uani 1 1 d . . . H2 H 0.2813 -0.0634 -0.2106 0.020 Uiso 1 1 calc R . . C3 C 0.3680(2) -0.1083(2) -0.0613(5) 0.0189(9) Uani 1 1 d . . . H3 H 0.3776 -0.1379 -0.0199 0.023 Uiso 1 1 calc R . . C4 C 0.2519(2) -0.1892(2) -0.1096(5) 0.0200(9) Uani 1 1 d . . . C5 C 0.2135(2) -0.2155(2) -0.2217(4) 0.0193(9) Uani 1 1 d . . . H5 H 0.2231 -0.1912 -0.3003 0.023 Uiso 1 1 calc R . . C6 C 0.1600(2) -0.2791(2) -0.2151(5) 0.0188(9) Uani 1 1 d . . . H6 H 0.1336 -0.2975 -0.2901 0.023 Uiso 1 1 calc R . . C7 C 0.1456(2) -0.3152(2) -0.0986(4) 0.0176(9) Uani 1 1 d . . . C8 C 0.1847(3) -0.2867(3) 0.0139(5) 0.0309(12) Uani 1 1 d . . . H8 H 0.1753 -0.3107 0.0928 0.037 Uiso 1 1 calc R . . C9 C 0.2370(3) -0.2235(2) 0.0095(5) 0.0312(12) Uani 1 1 d . . . H9 H 0.2620 -0.2041 0.0856 0.037 Uiso 1 1 calc R . . C10 C 0.0878(2) -0.3836(2) -0.0922(4) 0.0142(8) 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 0.0116(4) 0.0086(4) 0.0158(4) -0.0006(2) -0.0007(2) 0.0042(3) O1 0.0123(13) 0.0138(13) 0.0170(15) -0.0001(11) 0.0018(11) 0.0043(11) O2 0.0149(14) 0.0199(15) 0.0178(16) -0.0042(12) -0.0010(11) 0.0049(12) N1 0.0137(16) 0.0112(16) 0.0206(18) -0.0005(13) 0.0006(14) 0.0062(13) N2 0.0149(16) 0.0131(16) 0.0159(17) 0.0013(13) 0.0001(13) 0.0046(13) C1 0.0168(19) 0.0124(18) 0.021(2) -0.0005(15) -0.0035(16) 0.0077(15) C2 0.0174(19) 0.0165(19) 0.017(2) -0.0005(16) 0.0002(16) 0.0091(16) C3 0.020(2) 0.0149(19) 0.019(2) 0.0024(16) -0.0029(16) 0.0063(16) C4 0.017(2) 0.017(2) 0.021(2) 0.0007(17) 0.0014(17) 0.0043(16) C5 0.0147(19) 0.021(2) 0.0143(19) 0.0022(16) 0.0013(15) 0.0024(16) C6 0.020(2) 0.020(2) 0.0150(19) 0.0002(16) -0.0027(16) 0.0086(17) C7 0.0141(19) 0.018(2) 0.016(2) -0.0025(16) -0.0018(16) 0.0051(16) C8 0.028(2) 0.026(2) 0.018(2) 0.0054(19) -0.0074(19) -0.0028(19) C9 0.032(3) 0.021(2) 0.018(2) 0.0030(19) -0.0062(19) -0.004(2) C10 0.0124(18) 0.0184(19) 0.0127(19) -0.0020(15) 0.0029(15) 0.0084(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.971(3) 12 ? Cu1 O1 1.971(3) 3_655 ? Cu1 N1 1.978(4) 10_655 ? Cu1 N1 1.978(4) . ? O1 C10 1.294(5) . ? O1 Cu1 1.971(3) 2_545 ? O2 C10 1.235(5) . ? N1 C3 1.318(6) . ? N1 C1 1.397(5) . ? N2 C3 1.345(6) . ? N2 C2 1.391(5) . ? N2 C4 1.440(5) . ? C1 C2 1.346(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.377(6) . ? C4 C9 1.382(7) . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 C7 1.381(6) . ? C6 H6 0.9300 . ? C7 C8 1.394(6) . ? C7 C10 1.499(6) . ? C8 C9 1.377(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 180 . . ? O1 Cu1 N1 90.47(13) 12 10_655 ? O1 Cu1 N1 89.53(13) 3_655 10_655 ? O1 Cu1 N1 89.53(13) 12 . ? O1 Cu1 N1 90.47(13) 3_655 . ? N1 Cu1 N1 180 . . ? C10 O1 Cu1 105.7(2) . 2_545 ? C3 N1 C1 105.7(4) . . ? C3 N1 Cu1 124.1(3) . . ? C1 N1 Cu1 129.9(3) . . ? C3 N2 C2 107.3(4) . . ? C3 N2 C4 124.9(4) . . ? C2 N2 C4 127.8(4) . . ? C2 C1 N1 109.6(4) . . ? C2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? C1 C2 N2 106.1(4) . . ? C1 C2 H2 127.0 . . ? N2 C2 H2 127.0 . . ? N1 C3 N2 111.4(4) . . ? N1 C3 H3 124.3 . . ? N2 C3 H3 124.3 . . ? C5 C4 C9 121.5(4) . . ? C5 C4 N2 120.5(4) . . ? C9 C4 N2 118.0(4) . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 120.8(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.1(4) . . ? C6 C7 C10 120.4(4) . . ? C8 C7 C10 120.5(4) . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C4 119.1(4) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? O2 C10 O1 123.8(4) . . ? O2 C10 C7 120.6(4) . . ? O1 C10 C7 115.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 N1 C3 -158.4(4) 12 . . . ? O1 Cu1 N1 C3 21.6(4) 3_655 . . . ? N1 Cu1 N1 C3 53(41) 10_655 . . . ? O1 Cu1 N1 C1 14.8(4) 12 . . . ? O1 Cu1 N1 C1 -165.2(4) 3_655 . . . ? N1 Cu1 N1 C1 -134(41) 10_655 . . . ? C3 N1 C1 C2 -0.5(5) . . . . ? Cu1 N1 C1 C2 -174.7(3) . . . . ? N1 C1 C2 N2 0.8(5) . . . . ? C3 N2 C2 C1 -0.8(5) . . . . ? C4 N2 C2 C1 177.7(4) . . . . ? C1 N1 C3 N2 0.0(5) . . . . ? Cu1 N1 C3 N2 174.6(3) . . . . ? C2 N2 C3 N1 0.5(5) . . . . ? C4 N2 C3 N1 -178.0(4) . . . . ? C3 N2 C4 C5 -135.5(5) . . . . ? C2 N2 C4 C5 46.3(7) . . . . ? C3 N2 C4 C9 44.8(7) . . . . ? C2 N2 C4 C9 -133.5(5) . . . . ? C9 C4 C5 C6 -2.5(7) . . . . ? N2 C4 C5 C6 177.8(4) . . . . ? C4 C5 C6 C7 0.0(7) . . . . ? C5 C6 C7 C8 1.3(7) . . . . ? C5 C6 C7 C10 179.8(4) . . . . ? C6 C7 C8 C9 -0.1(8) . . . . ? C10 C7 C8 C9 -178.7(5) . . . . ? C7 C8 C9 C4 -2.3(9) . . . . ? C5 C4 C9 C8 3.6(9) . . . . ? N2 C4 C9 C8 -176.7(5) . . . . ? Cu1 O1 C10 O2 -5.1(5) 2_545 . . . ? Cu1 O1 C10 C7 174.6(3) 2_545 . . . ? C6 C7 C10 O2 -10.8(6) . . . . ? C8 C7 C10 O2 167.7(5) . . . . ? C6 C7 C10 O1 169.4(4) . . . . ? C8 C7 C10 O1 -12.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 1.016 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.186 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 773579' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Cd2 N4 O9' _chemical_formula_sum 'C22 H18 Cd2 N4 O9' _chemical_formula_weight 707.22 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.710(5) _cell_length_b 8.481(3) _cell_length_c 19.343(5) _cell_angle_alpha 90.000 _cell_angle_beta 101.405(5) _cell_angle_gamma 90.000 _cell_volume 2204.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.995 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7408 _exptl_absorpt_correction_T_max 0.8254 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11521 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4095 _reflns_number_gt 3570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The three restraints applied are: DFIX and DANG option to fix the O-H distance and H-O-H angle in water. ; _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^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4095 _refine_ls_number_parameters 342 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Cd1 Cd -0.08098(2) 0.36509(3) 0.253156(15) 0.01450(11) Uani 1 1 d . . . Cd2 Cd 0.16476(2) 0.54653(3) 0.256606(15) 0.01455(11) Uani 1 1 d . . . O1 O 0.1233(2) -0.1005(3) -0.21962(14) 0.0181(6) Uani 1 1 d . . . O2 O 0.0895(2) -0.2655(3) -0.13955(14) 0.0195(7) Uani 1 1 d . . . O3 O -0.1607(2) -0.4707(3) 0.62080(15) 0.0208(7) Uani 1 1 d . . . O4 O -0.0944(2) -0.3127(3) 0.70942(14) 0.0176(6) Uani 1 1 d . . . O5 O -0.0087(2) 0.6021(4) 0.25264(16) 0.0186(6) Uani 1 1 d . . . O6 O -0.1257(2) 0.6957(4) 0.30703(15) 0.0232(7) Uani 1 1 d . . . O7 O 0.1890(2) 0.8086(3) 0.25188(15) 0.0199(7) Uani 1 1 d . . . O8 O 0.1696(2) 1.0350(3) 0.19396(15) 0.0207(7) Uani 1 1 d . . . N1 N 0.1370(3) 0.5046(4) 0.13974(17) 0.0163(7) Uani 1 1 d . . . N2 N 0.1296(2) 0.3770(4) 0.03929(17) 0.0152(8) Uani 1 1 d . . . N3 N -0.1029(2) 0.3167(4) 0.36403(17) 0.0153(7) Uani 1 1 d . . . N4 N -0.1170(3) 0.1834(4) 0.45906(17) 0.0145(7) Uani 1 1 d . . . C1 C 0.1234(3) 0.6114(5) 0.0842(2) 0.0180(9) Uani 1 1 d . . . H1 H 0.1179 0.7200 0.0888 0.022 Uiso 1 1 calc R . . C2 C 0.1193(3) 0.5346(5) 0.0226(2) 0.0172(9) Uani 1 1 d . . . H2 H 0.1112 0.5792 -0.0221 0.021 Uiso 1 1 calc R . . C3 C 0.1400(3) 0.3655(5) 0.1108(2) 0.0164(9) Uani 1 1 d . . . H3 H 0.1482 0.2710 0.1357 0.020 Uiso 1 1 calc R . . C4 C 0.1310(3) 0.2486(5) -0.0087(2) 0.0155(9) Uani 1 1 d . . . C5 C 0.1193(3) 0.0955(5) 0.0127(2) 0.0211(10) Uani 1 1 d . . . H5 H 0.1137 0.0747 0.0589 0.025 Uiso 1 1 calc R . . C6 C 0.1158(3) -0.0271(5) -0.0353(2) 0.0226(10) Uani 1 1 d . . . H6 H 0.1070 -0.1299 -0.0210 0.027 Uiso 1 1 calc R . . C7 C 0.1255(3) 0.0016(5) -0.1040(2) 0.0166(9) Uani 1 1 d . . . C8 C 0.1422(3) 0.1548(5) -0.1235(2) 0.0171(9) Uani 1 1 d . . . H8 H 0.1524 0.1746 -0.1688 0.021 Uiso 1 1 calc R . . C9 C 0.1440(3) 0.2788(5) -0.0770(2) 0.0158(9) Uani 1 1 d . . . H9 H 0.1538 0.3814 -0.0912 0.019 Uiso 1 1 calc R . . C10 C 0.1129(3) -0.1303(5) -0.1571(2) 0.0167(9) Uani 1 1 d . . . C11 C -0.1052(3) 0.4223(5) 0.4187(2) 0.0199(9) Uani 1 1 d . . . H11 H -0.1013 0.5314 0.4153 0.024 Uiso 1 1 calc R . . C12 C -0.1137(3) 0.3419(5) 0.4775(2) 0.0195(9) Uani 1 1 d . . . H12 H -0.1168 0.3842 0.5213 0.023 Uiso 1 1 calc R . . C13 C -0.1100(3) 0.1767(5) 0.3904(2) 0.0155(9) Uani 1 1 d . . . H13 H -0.1103 0.0834 0.3651 0.019 Uiso 1 1 calc R . . C14 C -0.1246(3) 0.0525(5) 0.5043(2) 0.0155(9) Uani 1 1 d . . . C15 C -0.1114(3) 0.0766(5) 0.5767(2) 0.0192(9) Uani 1 1 d . . . H15 H -0.1018 0.1778 0.5954 0.023 Uiso 1 1 calc R . . C16 C -0.1129(3) -0.0524(5) 0.6206(2) 0.0186(10) Uani 1 1 d . . . H16 H -0.1031 -0.0368 0.6691 0.022 Uiso 1 1 calc R . . C17 C -0.1284(3) -0.2036(5) 0.5940(2) 0.0149(9) Uani 1 1 d . . . C18 C -0.1459(3) -0.2237(5) 0.5216(2) 0.0178(9) Uani 1 1 d . . . H18 H -0.1592 -0.3242 0.5030 0.021 Uiso 1 1 calc R . . C19 C -0.1440(3) -0.0988(5) 0.4765(2) 0.0195(9) Uani 1 1 d . . . H19 H -0.1555 -0.1150 0.4280 0.023 Uiso 1 1 calc R . . C20 C -0.1280(3) -0.3400(5) 0.6433(2) 0.0189(9) Uani 1 1 d . . . C21 C -0.0503(3) 0.7110(5) 0.2825(2) 0.0186(9) Uani 1 1 d . . . H21 H -0.0208 0.8101 0.2859 0.022 Uiso 1 1 calc R . . C22 C 0.1385(3) 0.9053(5) 0.2106(2) 0.0175(9) Uani 1 1 d . . . H22 H 0.0732 0.8781 0.1909 0.021 Uiso 1 1 calc R . . OW1 O -0.2429(2) 0.4401(4) 0.21251(16) 0.0203(7) Uani 1 1 d D . . H1W1 H -0.269(4) 0.508(5) 0.235(3) 0.07(2) Uiso 1 1 d D . . H2W1 H -0.273(3) 0.358(3) 0.218(2) 0.024(11) 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 Cd1 0.01799(18) 0.01361(18) 0.01195(17) 0.00009(11) 0.00303(13) -0.00152(12) Cd2 0.01855(19) 0.01243(18) 0.01308(17) 0.00055(11) 0.00415(13) -0.00141(11) O1 0.0239(16) 0.0171(15) 0.0148(15) 0.0007(12) 0.0075(13) -0.0018(13) O2 0.0268(17) 0.0166(16) 0.0162(15) -0.0019(12) 0.0066(13) -0.0047(13) O3 0.0260(17) 0.0188(17) 0.0173(16) -0.0001(13) 0.0033(13) -0.0077(13) O4 0.0204(16) 0.0201(16) 0.0128(14) 0.0049(12) 0.0048(12) 0.0006(12) O5 0.0144(15) 0.0159(15) 0.0249(16) 0.0019(13) 0.0024(13) -0.0028(12) O6 0.0256(17) 0.0246(17) 0.0202(16) 0.0037(13) 0.0065(14) 0.0027(14) O7 0.0222(16) 0.0149(15) 0.0202(15) 0.0016(12) -0.0019(13) -0.0005(13) O8 0.0262(17) 0.0181(17) 0.0183(16) 0.0022(12) 0.0054(13) -0.0031(13) N1 0.0195(19) 0.0144(18) 0.0151(18) -0.0008(14) 0.0036(15) -0.0022(15) N2 0.0165(18) 0.0141(18) 0.0148(18) 0.0000(14) 0.0030(15) 0.0003(14) N3 0.0154(18) 0.0198(19) 0.0110(17) 0.0002(14) 0.0033(14) 0.0006(14) N4 0.0175(18) 0.0137(18) 0.0122(17) 0.0002(14) 0.0021(14) 0.0009(14) C1 0.023(2) 0.015(2) 0.015(2) 0.0012(17) 0.0035(18) 0.0013(18) C2 0.024(2) 0.015(2) 0.012(2) 0.0056(16) 0.0019(18) 0.0014(17) C3 0.017(2) 0.018(2) 0.015(2) 0.0026(17) 0.0049(17) -0.0011(17) C4 0.011(2) 0.016(2) 0.018(2) -0.0038(17) 0.0013(17) 0.0019(16) C5 0.033(3) 0.016(2) 0.016(2) 0.0012(18) 0.0077(19) 0.000(2) C6 0.033(3) 0.019(2) 0.017(2) 0.0007(18) 0.008(2) -0.004(2) C7 0.015(2) 0.018(2) 0.017(2) -0.0009(17) 0.0042(17) 0.0007(18) C8 0.019(2) 0.020(2) 0.011(2) -0.0008(17) 0.0014(17) -0.0008(18) C9 0.017(2) 0.015(2) 0.015(2) 0.0021(17) 0.0008(17) -0.0020(17) C10 0.014(2) 0.016(2) 0.018(2) -0.0014(17) 0.0001(17) 0.0022(17) C11 0.028(3) 0.014(2) 0.018(2) 0.0006(17) 0.0059(19) 0.0015(19) C12 0.029(2) 0.017(2) 0.013(2) -0.0027(17) 0.0052(18) -0.0006(19) C13 0.017(2) 0.015(2) 0.014(2) -0.0040(17) 0.0016(17) -0.0004(17) C14 0.011(2) 0.020(2) 0.018(2) 0.0029(17) 0.0055(17) 0.0016(16) C15 0.027(2) 0.015(2) 0.015(2) -0.0005(17) 0.0036(19) -0.0003(18) C16 0.024(2) 0.021(2) 0.010(2) 0.0008(17) 0.0022(18) 0.0011(18) C17 0.013(2) 0.015(2) 0.018(2) 0.0025(17) 0.0046(17) 0.0020(16) C18 0.025(2) 0.012(2) 0.016(2) -0.0047(17) 0.0048(18) -0.0025(18) C19 0.028(2) 0.017(2) 0.013(2) 0.0006(17) 0.0027(18) -0.0007(19) C20 0.016(2) 0.022(2) 0.020(2) 0.0001(18) 0.0071(18) 0.0019(18) C21 0.021(2) 0.016(2) 0.020(2) -0.0012(18) 0.0070(19) -0.0035(18) C22 0.021(2) 0.020(2) 0.012(2) -0.0032(18) 0.0050(18) -0.0011(19) OW1 0.0227(17) 0.0165(17) 0.0215(16) -0.0023(13) 0.0043(14) 0.0007(14) _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 Cd1 O5 2.242(3) . ? Cd1 N3 2.261(3) . ? Cd1 OW1 2.293(3) . ? Cd1 O2 2.336(3) 3 ? Cd1 O1 2.376(3) 3 ? Cd1 O4 2.411(3) 3_556 ? Cd1 C10 2.699(4) 3 ? Cd2 N1 2.245(3) . ? Cd2 O7 2.252(3) . ? Cd2 O8 2.286(3) 2_545 ? Cd2 O4 2.355(3) 3_556 ? Cd2 O5 2.410(3) . ? Cd2 O3 2.468(3) 3_556 ? Cd2 C20 2.730(4) 3_556 ? O1 C10 1.271(5) . ? O1 Cd1 2.376(3) 3 ? O2 C10 1.256(5) . ? O2 Cd1 2.336(3) 3 ? O3 C20 1.241(5) . ? O3 Cd2 2.468(3) 3_556 ? O4 C20 1.291(5) . ? O4 Cd2 2.355(3) 3_556 ? O4 Cd1 2.411(3) 3_556 ? O5 C21 1.282(5) . ? O6 C21 1.227(5) . ? O7 C22 1.253(5) . ? O8 C22 1.245(5) . ? O8 Cd2 2.286(3) 2 ? N1 C3 1.310(5) . ? N1 C1 1.389(5) . ? N2 C3 1.365(5) . ? N2 C2 1.375(5) . ? N2 C4 1.433(5) . ? N3 C13 1.304(5) . ? N3 C11 1.390(5) . ? N4 C13 1.351(5) . ? N4 C12 1.389(5) . ? N4 C14 1.430(5) . ? C1 C2 1.349(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.381(6) . ? C4 C9 1.392(5) . ? C5 C6 1.388(6) . ? C5 H5 0.9300 . ? C6 C7 1.383(6) . ? C6 H6 0.9300 . ? C7 C8 1.384(6) . ? C7 C10 1.506(6) . ? C8 C9 1.380(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 Cd1 2.699(4) 3 ? C11 C12 1.351(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.392(6) . ? C14 C19 1.396(6) . ? C15 C16 1.387(6) . ? C15 H15 0.9300 . ? C16 C17 1.383(6) . ? C16 H16 0.9300 . ? C17 C18 1.382(5) . ? C17 C20 1.500(6) . ? C18 C19 1.376(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 Cd2 2.730(4) 3_556 ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? OW1 H1W1 0.85(5) . ? OW1 H2W1 0.824(18) . ? 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 O5 Cd1 N3 107.99(12) . . ? O5 Cd1 OW1 98.55(11) . . ? N3 Cd1 OW1 94.25(12) . . ? O5 Cd1 O2 105.05(11) . 3 ? N3 Cd1 O2 146.67(12) . 3 ? OW1 Cd1 O2 85.00(11) . 3 ? O5 Cd1 O1 158.42(10) . 3 ? N3 Cd1 O1 90.94(11) . 3 ? OW1 Cd1 O1 90.05(11) . 3 ? O2 Cd1 O1 55.78(10) 3 3 ? O5 Cd1 O4 75.58(11) . 3_556 ? N3 Cd1 O4 89.64(11) . 3_556 ? OW1 Cd1 O4 173.76(10) . 3_556 ? O2 Cd1 O4 94.42(10) 3 3_556 ? O1 Cd1 O4 94.77(10) 3 3_556 ? O5 Cd1 C10 132.05(12) . 3 ? N3 Cd1 C10 119.01(13) . 3 ? OW1 Cd1 C10 87.41(12) . 3 ? O2 Cd1 C10 27.70(11) 3 3 ? O1 Cd1 C10 28.08(11) 3 3 ? O4 Cd1 C10 94.97(11) 3_556 3 ? N1 Cd2 O7 96.45(11) . . ? N1 Cd2 O8 111.76(11) . 2_545 ? O7 Cd2 O8 85.23(10) . 2_545 ? N1 Cd2 O4 98.65(11) . 3_556 ? O7 Cd2 O4 156.11(11) . 3_556 ? O8 Cd2 O4 105.98(10) 2_545 3_556 ? N1 Cd2 O5 91.68(11) . . ? O7 Cd2 O5 87.61(10) . . ? O8 Cd2 O5 156.09(10) 2_545 . ? O4 Cd2 O5 73.59(10) 3_556 . ? N1 Cd2 O3 153.45(11) . 3_556 ? O7 Cd2 O3 109.13(10) . 3_556 ? O8 Cd2 O3 78.25(10) 2_545 3_556 ? O4 Cd2 O3 54.84(9) 3_556 3_556 ? O5 Cd2 O3 82.64(10) . 3_556 ? N1 Cd2 C20 126.45(13) . 3_556 ? O7 Cd2 C20 135.34(12) . 3_556 ? O8 Cd2 C20 89.05(11) 2_545 3_556 ? O4 Cd2 C20 28.21(11) 3_556 3_556 ? O5 Cd2 C20 80.15(11) . 3_556 ? O3 Cd2 C20 27.03(11) 3_556 3_556 ? C10 O1 Cd1 90.3(2) . 3 ? C10 O2 Cd1 92.5(2) . 3 ? C20 O3 Cd2 88.3(2) . 3_556 ? C20 O4 Cd2 92.2(2) . 3_556 ? C20 O4 Cd1 113.8(2) . 3_556 ? Cd2 O4 Cd1 101.55(11) 3_556 3_556 ? C21 O5 Cd1 114.0(3) . . ? C21 O5 Cd2 130.6(3) . . ? Cd1 O5 Cd2 105.01(12) . . ? C22 O7 Cd2 127.2(3) . . ? C22 O8 Cd2 107.0(3) . 2 ? C3 N1 C1 105.5(3) . . ? C3 N1 Cd2 124.0(3) . . ? C1 N1 Cd2 130.2(3) . . ? C3 N2 C2 107.0(3) . . ? C3 N2 C4 126.1(3) . . ? C2 N2 C4 126.9(3) . . ? C13 N3 C11 105.9(3) . . ? C13 N3 Cd1 124.8(3) . . ? C11 N3 Cd1 129.1(3) . . ? C13 N4 C12 106.7(3) . . ? C13 N4 C14 126.6(3) . . ? C12 N4 C14 126.7(3) . . ? C2 C1 N1 110.1(4) . . ? C2 C1 H1 124.9 . . ? N1 C1 H1 124.9 . . ? C1 C2 N2 106.1(4) . . ? C1 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? N1 C3 N2 111.3(4) . . ? N1 C3 H3 124.4 . . ? N2 C3 H3 124.4 . . ? C5 C4 C9 120.1(4) . . ? C5 C4 N2 120.2(4) . . ? C9 C4 N2 119.7(4) . . ? C4 C5 C6 119.7(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 118.6(4) . . ? C6 C7 C10 120.4(4) . . ? C8 C7 C10 120.9(4) . . ? C9 C8 C7 121.4(4) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C4 119.2(4) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? O2 C10 O1 121.5(4) . . ? O2 C10 C7 119.7(4) . . ? O1 C10 C7 118.8(4) . . ? O2 C10 Cd1 59.8(2) . 3 ? O1 C10 Cd1 61.7(2) . 3 ? C7 C10 Cd1 177.3(3) . 3 ? C12 C11 N3 109.5(4) . . ? C12 C11 H11 125.2 . . ? N3 C11 H11 125.2 . . ? C11 C12 N4 106.0(4) . . ? C11 C12 H12 127.0 . . ? N4 C12 H12 127.0 . . ? N3 C13 N4 111.8(4) . . ? N3 C13 H13 124.1 . . ? N4 C13 H13 124.1 . . ? C15 C14 C19 120.0(4) . . ? C15 C14 N4 119.4(4) . . ? C19 C14 N4 120.6(4) . . ? C16 C15 C14 119.0(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 121.5(4) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C18 C17 C16 118.3(4) . . ? C18 C17 C20 121.9(4) . . ? C16 C17 C20 119.8(4) . . ? C19 C18 C17 121.8(4) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C14 119.3(4) . . ? C18 C19 H19 120.4 . . ? C14 C19 H19 120.4 . . ? O3 C20 O4 122.8(4) . . ? O3 C20 C17 120.6(4) . . ? O4 C20 C17 116.6(4) . . ? O3 C20 Cd2 64.7(2) . 3_556 ? O4 C20 Cd2 59.6(2) . 3_556 ? C17 C20 Cd2 165.6(3) . 3_556 ? O6 C21 O5 125.6(4) . . ? O6 C21 H21 117.2 . . ? O5 C21 H21 117.2 . . ? O8 C22 O7 124.7(4) . . ? O8 C22 H22 117.7 . . ? O7 C22 H22 117.7 . . ? Cd1 OW1 H1W1 119(5) . . ? Cd1 OW1 H2W1 101(3) . . ? H1W1 OW1 H2W1 103(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cd1 O5 C21 -48.3(3) . . . . ? OW1 Cd1 O5 C21 49.0(3) . . . . ? O2 Cd1 O5 C21 136.1(3) 3 . . . ? O1 Cd1 O5 C21 161.5(3) 3 . . . ? O4 Cd1 O5 C21 -133.2(3) 3_556 . . . ? C10 Cd1 O5 C21 143.2(3) 3 . . . ? N3 Cd1 O5 Cd2 100.65(13) . . . . ? OW1 Cd1 O5 Cd2 -162.01(12) . . . . ? O2 Cd1 O5 Cd2 -74.93(13) 3 . . . ? O1 Cd1 O5 Cd2 -49.5(3) 3 . . . ? O4 Cd1 O5 Cd2 15.84(10) 3_556 . . . ? C10 Cd1 O5 Cd2 -67.77(18) 3 . . . ? N1 Cd2 O5 C21 -136.1(3) . . . . ? O7 Cd2 O5 C21 -39.8(3) . . . . ? O8 Cd2 O5 C21 32.8(5) 2_545 . . . ? O4 Cd2 O5 C21 125.3(4) 3_556 . . . ? O3 Cd2 O5 C21 69.9(3) 3_556 . . . ? C20 Cd2 O5 C21 97.1(4) 3_556 . . . ? N1 Cd2 O5 Cd1 82.14(13) . . . . ? O7 Cd2 O5 Cd1 178.53(12) . . . . ? O8 Cd2 O5 Cd1 -108.9(2) 2_545 . . . ? O4 Cd2 O5 Cd1 -16.38(11) 3_556 . . . ? O3 Cd2 O5 Cd1 -71.83(12) 3_556 . . . ? C20 Cd2 O5 Cd1 -44.59(13) 3_556 . . . ? N1 Cd2 O7 C22 44.1(3) . . . . ? O8 Cd2 O7 C22 155.5(3) 2_545 . . . ? O4 Cd2 O7 C22 -84.9(4) 3_556 . . . ? O5 Cd2 O7 C22 -47.3(3) . . . . ? O3 Cd2 O7 C22 -128.7(3) 3_556 . . . ? C20 Cd2 O7 C22 -120.7(3) 3_556 . . . ? O7 Cd2 N1 C3 163.9(3) . . . . ? O8 Cd2 N1 C3 76.5(3) 2_545 . . . ? O4 Cd2 N1 C3 -34.6(3) 3_556 . . . ? O5 Cd2 N1 C3 -108.3(3) . . . . ? O3 Cd2 N1 C3 -31.5(5) 3_556 . . . ? C20 Cd2 N1 C3 -29.3(4) 3_556 . . . ? O7 Cd2 N1 C1 -9.3(4) . . . . ? O8 Cd2 N1 C1 -96.7(4) 2_545 . . . ? O4 Cd2 N1 C1 152.2(3) 3_556 . . . ? O5 Cd2 N1 C1 78.5(4) . . . . ? O3 Cd2 N1 C1 155.3(3) 3_556 . . . ? C20 Cd2 N1 C1 157.5(3) 3_556 . . . ? O5 Cd1 N3 C13 -155.3(3) . . . . ? OW1 Cd1 N3 C13 104.3(3) . . . . ? O2 Cd1 N3 C13 16.9(4) 3 . . . ? O1 Cd1 N3 C13 14.2(3) 3 . . . ? O4 Cd1 N3 C13 -80.6(3) 3_556 . . . ? C10 Cd1 N3 C13 14.9(4) 3 . . . ? O5 Cd1 N3 C11 20.1(4) . . . . ? OW1 Cd1 N3 C11 -80.3(3) . . . . ? O2 Cd1 N3 C11 -167.7(3) 3 . . . ? O1 Cd1 N3 C11 -170.4(3) 3 . . . ? O4 Cd1 N3 C11 94.8(3) 3_556 . . . ? C10 Cd1 N3 C11 -169.7(3) 3 . . . ? C3 N1 C1 C2 -0.6(5) . . . . ? Cd2 N1 C1 C2 173.6(3) . . . . ? N1 C1 C2 N2 0.6(5) . . . . ? C3 N2 C2 C1 -0.3(5) . . . . ? C4 N2 C2 C1 -179.3(4) . . . . ? C1 N1 C3 N2 0.4(5) . . . . ? Cd2 N1 C3 N2 -174.3(2) . . . . ? C2 N2 C3 N1 0.0(5) . . . . ? C4 N2 C3 N1 179.0(4) . . . . ? C3 N2 C4 C5 15.9(6) . . . . ? C2 N2 C4 C5 -165.3(4) . . . . ? C3 N2 C4 C9 -164.3(4) . . . . ? C2 N2 C4 C9 14.5(6) . . . . ? C9 C4 C5 C6 -3.0(6) . . . . ? N2 C4 C5 C6 176.8(4) . . . . ? C4 C5 C6 C7 0.9(7) . . . . ? C5 C6 C7 C8 2.2(7) . . . . ? C5 C6 C7 C10 -174.7(4) . . . . ? C6 C7 C8 C9 -3.5(6) . . . . ? C10 C7 C8 C9 173.5(4) . . . . ? C7 C8 C9 C4 1.5(6) . . . . ? C5 C4 C9 C8 1.8(6) . . . . ? N2 C4 C9 C8 -178.0(4) . . . . ? Cd1 O2 C10 O1 -0.9(4) 3 . . . ? Cd1 O2 C10 C7 177.0(3) 3 . . . ? Cd1 O1 C10 O2 0.9(4) 3 . . . ? Cd1 O1 C10 C7 -177.0(3) 3 . . . ? C6 C7 C10 O2 2.9(6) . . . . ? C8 C7 C10 O2 -174.0(4) . . . . ? C6 C7 C10 O1 -179.2(4) . . . . ? C8 C7 C10 O1 3.9(6) . . . . ? C6 C7 C10 Cd1 81(6) . . . 3 ? C8 C7 C10 Cd1 -96(6) . . . 3 ? C13 N3 C11 C12 0.0(5) . . . . ? Cd1 N3 C11 C12 -176.1(3) . . . . ? N3 C11 C12 N4 -0.1(5) . . . . ? C13 N4 C12 C11 0.1(5) . . . . ? C14 N4 C12 C11 179.1(4) . . . . ? C11 N3 C13 N4 0.1(5) . . . . ? Cd1 N3 C13 N4 176.4(3) . . . . ? C12 N4 C13 N3 -0.2(5) . . . . ? C14 N4 C13 N3 -179.2(4) . . . . ? C13 N4 C14 C15 167.3(4) . . . . ? C12 N4 C14 C15 -11.5(6) . . . . ? C13 N4 C14 C19 -12.0(6) . . . . ? C12 N4 C14 C19 169.2(4) . . . . ? C19 C14 C15 C16 3.2(6) . . . . ? N4 C14 C15 C16 -176.1(4) . . . . ? C14 C15 C16 C17 -0.9(7) . . . . ? C15 C16 C17 C18 -2.0(6) . . . . ? C15 C16 C17 C20 179.2(4) . . . . ? C16 C17 C18 C19 2.7(6) . . . . ? C20 C17 C18 C19 -178.5(4) . . . . ? C17 C18 C19 C14 -0.4(7) . . . . ? C15 C14 C19 C18 -2.6(6) . . . . ? N4 C14 C19 C18 176.8(4) . . . . ? Cd2 O3 C20 O4 13.6(4) 3_556 . . . ? Cd2 O3 C20 C17 -164.8(3) 3_556 . . . ? Cd2 O4 C20 O3 -14.3(4) 3_556 . . . ? Cd1 O4 C20 O3 89.3(4) 3_556 . . . ? Cd2 O4 C20 C17 164.2(3) 3_556 . . . ? Cd1 O4 C20 C17 -92.1(4) 3_556 . . . ? Cd1 O4 C20 Cd2 103.66(19) 3_556 . . 3_556 ? C18 C17 C20 O3 -13.0(6) . . . . ? C16 C17 C20 O3 165.8(4) . . . . ? C18 C17 C20 O4 168.4(4) . . . . ? C16 C17 C20 O4 -12.8(6) . . . . ? C18 C17 C20 Cd2 -120.8(11) . . . 3_556 ? C16 C17 C20 Cd2 57.9(13) . . . 3_556 ? Cd1 O5 C21 O6 -3.4(5) . . . . ? Cd2 O5 C21 O6 -142.5(3) . . . . ? Cd2 O8 C22 O7 5.7(5) 2 . . . ? Cd2 O7 C22 O8 -156.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.053 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.166 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 773580' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H33 Cd2 N8 O11' _chemical_formula_sum 'C40 H33 Cd2 N8 O11' _chemical_formula_weight 1026.56 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.147(5) _cell_length_b 9.219(2) _cell_length_c 14.604(3) _cell_angle_alpha 97.973(5) _cell_angle_beta 104.956(4) _cell_angle_gamma 104.565(5) _cell_volume 1123.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 513 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8632 _exptl_absorpt_correction_T_max 0.9057 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5904 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4862 _reflns_number_gt 4391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The seven restraints applied are DFIX and DANG option to fix the O-H distance and H-O-H angle in waters. Another one restrain was added to fix the bond distance of C10-C7 using DFIX instruction. ; _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^)+(0.0981P)^2^+0.1713P] 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 refU _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 0.001(5) _refine_ls_number_reflns 4862 _refine_ls_number_parameters 570 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Cd1 Cd 1.40284(6) 0.92096(6) 0.81123(4) 0.0351(2) Uani 1 1 d . . . Cd2 Cd 0.66166(6) 1.75242(6) 0.40398(4) 0.0370(2) Uani 1 1 d . . . O1 O 1.1941(12) 0.8310(12) 0.8729(7) 0.052(2) Uani 1 1 d . . . O2 O 1.4323(9) 0.8689(10) 0.9676(6) 0.0482(19) Uani 1 1 d . . . O3 O 1.2401(10) 1.0026(9) 0.6880(6) 0.0344(19) Uani 1 1 d . . . O4 O 1.3471(10) 1.1617(9) 0.8336(5) 0.0453(19) Uani 1 1 d . . . O5 O 0.4018(13) 1.5923(13) 0.3304(6) 0.052(3) Uani 1 1 d . . . O6 O 0.5530(11) 1.6152(11) 0.2362(6) 0.052(2) Uani 1 1 d . . . O7 O 0.6074(12) 1.9848(10) 0.3876(6) 0.053(2) Uani 1 1 d . . . O8 O 0.6416(13) 1.9285(11) 0.5320(7) 0.048(3) Uani 1 1 d . . . N1 N 0.8890(14) 0.8104(14) 1.3641(7) 0.048(3) Uani 1 1 d . . . N2 N 1.0522(11) 0.8112(11) 1.2796(6) 0.043(2) Uani 1 1 d . . . N3 N 0.7706(10) 1.6463(10) 0.5259(7) 0.028(2) Uani 1 1 d . . . N4 N 0.9195(10) 1.5372(9) 0.6165(5) 0.0292(17) Uani 1 1 d . . . N5 N -0.3317(12) 1.0212(12) -0.1501(7) 0.046(2) Uani 1 1 d . . . N6 N -0.0875(11) 1.1400(10) -0.0582(6) 0.040(2) Uani 1 1 d . . . N7 N 0.3852(12) 2.7195(12) 0.6962(7) 0.032(2) Uani 1 1 d . . . N8 N 0.4131(11) 2.5255(9) 0.6050(6) 0.0312(18) Uani 1 1 d . . . C1 C 1.0449(15) 0.8282(16) 1.4263(8) 0.051(3) Uani 1 1 d . . . H1 H 1.0747 0.8404 1.4934 0.061 Uiso 1 1 calc R . . C2 C 1.1368(16) 0.8243(16) 1.3723(8) 0.054(3) Uani 1 1 d . . . H2 H 1.2434 0.8297 1.3940 0.065 Uiso 1 1 calc R . . C3 C 0.9061(17) 0.8040(17) 1.2805(9) 0.060(4) Uani 1 1 d . . . H3 H 0.8239 0.7950 1.2250 0.073 Uiso 1 1 calc R . . C4 C 1.1118(15) 0.8119(15) 1.1967(7) 0.048(3) Uani 1 1 d . . . C5 C 1.0021(18) 0.7558(18) 1.1023(9) 0.062(4) Uani 1 1 d . . . H5 H 0.8941 0.7116 1.0911 0.075 Uiso 1 1 calc R . . C6 C 1.0720(15) 0.7731(16) 1.0247(8) 0.055(3) Uani 1 1 d . . . H6 H 1.0044 0.7487 0.9615 0.066 Uiso 1 1 calc R . . C7 C 1.2222(14) 0.8200(14) 1.0381(7) 0.043(3) Uani 1 1 d D . . C8 C 1.3254(16) 0.8700(15) 1.1345(8) 0.053(3) Uani 1 1 d . . . H8 H 1.4337 0.9090 1.1443 0.064 Uiso 1 1 calc R . . C9 C 1.2745(14) 0.8636(14) 1.2118(7) 0.048(3) Uani 1 1 d . . . H9 H 1.3457 0.8929 1.2742 0.057 Uiso 1 1 calc R . . C10 C 1.2924(13) 0.8431(13) 0.9558(7) 0.043(3) Uani 1 1 d D . . C11 C 0.8360(14) 1.7382(12) 0.6170(8) 0.039(2) Uani 1 1 d . . . H11 H 0.8198 1.8317 0.6368 0.047 Uiso 1 1 calc R . . C12 C 0.9268(15) 1.6712(12) 0.6727(8) 0.043(3) Uani 1 1 d . . . H12 H 0.9846 1.7092 0.7380 0.052 Uiso 1 1 calc R . . C13 C 0.8271(13) 1.5276(12) 0.5286(8) 0.035(2) Uani 1 1 d . . . H13 H 0.8046 1.4479 0.4756 0.043 Uiso 1 1 calc R . . C14 C 0.9976(12) 1.4295(11) 0.6470(8) 0.030(2) Uani 1 1 d . . . C15 C 1.0105(14) 1.3145(13) 0.5803(7) 0.039(2) Uani 1 1 d . . . H15 H 0.9660 1.3045 0.5140 0.046 Uiso 1 1 calc R . . C16 C 1.0933(14) 1.2118(12) 0.6157(9) 0.041(3) Uani 1 1 d . . . H16 H 1.0973 1.1299 0.5723 0.049 Uiso 1 1 calc R . . C17 C 1.1661(12) 1.2324(11) 0.7117(7) 0.030(2) Uani 1 1 d . . . C18 C 1.1566(14) 1.3474(14) 0.7765(8) 0.044(3) Uani 1 1 d . . . H18 H 1.2078 1.3591 0.8422 0.053 Uiso 1 1 calc R . . C19 C 1.0731(15) 1.4478(12) 0.7478(7) 0.040(3) Uani 1 1 d . . . H19 H 1.0665 1.5252 0.7933 0.048 Uiso 1 1 calc R . . C20 C 1.2577(13) 1.1247(12) 0.7452(9) 0.035(2) Uani 1 1 d . . . C21 C -0.2307(15) 0.9479(15) -0.1764(9) 0.056(3) Uani 1 1 d . . . H21 H -0.2616 0.8619 -0.2265 0.067 Uiso 1 1 calc R . . C22 C -0.0853(14) 1.0158(14) -0.1212(10) 0.052(3) Uani 1 1 d . . . H22 H 0.0035 0.9858 -0.1239 0.062 Uiso 1 1 calc R . . C23 C -0.2382(16) 1.1392(16) -0.0840(10) 0.058(3) Uani 1 1 d . . . H23 H -0.2729 1.2165 -0.0570 0.069 Uiso 1 1 calc R . . C24 C 0.0427(14) 1.2441(15) 0.0175(8) 0.047(3) Uani 1 1 d . . . C25 C 0.1973(16) 1.2617(14) 0.0164(9) 0.051(3) Uani 1 1 d . . . H25 H 0.2199 1.2077 -0.0342 0.061 Uiso 1 1 calc R . . C26 C 0.3160(16) 1.3638(15) 0.0943(9) 0.053(3) Uani 1 1 d . . . H26 H 0.4201 1.3781 0.0937 0.064 Uiso 1 1 calc R . . C27 C 0.2930(14) 1.4451(15) 0.1718(8) 0.045(3) Uani 1 1 d . . . C28 C 0.140(2) 1.4359(19) 0.1688(11) 0.077(5) Uani 1 1 d . . . H28 H 0.1203 1.5002 0.2161 0.093 Uiso 1 1 calc R . . C29 C 0.014(3) 1.330(3) 0.0952(19) 0.075(6) Uani 1 1 d . . . H29 H -0.0892 1.3164 0.0973 0.108 Uiso 1 1 calc R . . C30 C 0.4229(14) 1.5550(13) 0.2516(7) 0.038(2) Uani 1 1 d . . . C31 C 0.3389(14) 2.7337(12) 0.6010(8) 0.041(3) Uani 1 1 d . . . H31 H 0.2983 2.8102 0.5797 0.049 Uiso 1 1 calc R . . C32 C 0.3612(17) 2.6226(14) 0.5457(9) 0.054(3) Uani 1 1 d . . . H32 H 0.3457 2.6098 0.4792 0.065 Uiso 1 1 calc R . . C33 C 0.4312(13) 2.5957(12) 0.6972(7) 0.031(2) Uani 1 1 d . . . H33 H 0.4703 2.5611 0.7527 0.037 Uiso 1 1 calc R . . C34 C 0.4640(13) 2.3945(13) 0.5772(8) 0.033(2) Uani 1 1 d . . . C35 C 0.4179(16) 2.3291(14) 0.4769(8) 0.051(3) Uani 1 1 d . . . H35 H 0.3516 2.3659 0.4325 0.061 Uiso 1 1 calc R . . C36 C 0.470(2) 2.2133(15) 0.4457(9) 0.060(4) Uani 1 1 d . . . H36 H 0.4507 2.1794 0.3794 0.081 Uiso 1 1 calc R . . C37 C 0.5551(14) 2.1418(12) 0.5119(8) 0.040(2) Uani 1 1 d . . . C38 C 0.5902(17) 2.2002(16) 0.6111(9) 0.050(3) Uani 1 1 d . . . H38 H 0.6428 2.1551 0.6570 0.059 Uiso 1 1 calc R . . C39 C 0.5421(15) 2.3333(14) 0.6404(7) 0.046(3) Uani 1 1 d . . . H39 H 0.5679 2.3759 0.7062 0.055 Uiso 1 1 calc R . . C40 C 0.5988(13) 2.0105(13) 0.4774(9) 0.040(3) Uani 1 1 d . . . O1W O 0.6025(10) 1.6791(10) 0.0584(6) 0.050(2) Uani 1 1 d D . . O2W O 1.5903(16) 1.4525(13) 0.8942(9) 0.078(3) Uani 1 1 d D . . O3W O 0.7845(18) 2.2403(15) 0.3406(10) 0.102(4) Uani 1 1 d D . . H1W1 H 0.596(11) 1.767(5) 0.079(6) 0.05(2) Uiso 1 1 d D . . H2W1 H 0.60(2) 1.634(11) 0.106(6) 0.09(5) Uiso 1 1 d D . . H1W2 H 1.587(15) 1.384(11) 0.929(8) 0.08(4) Uiso 1 1 d D . . H2W2 H 1.53(2) 1.50(2) 0.911(15) 0.19(10) Uiso 1 1 d D . . H1W3 H 0.795(12) 2.189(10) 0.288(5) 0.10(3) 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 Cd1 0.0408(5) 0.0401(5) 0.0296(4) 0.0059(3) 0.0074(4) 0.0255(4) Cd2 0.0404(5) 0.0453(5) 0.0281(4) 0.0030(3) 0.0045(4) 0.0268(4) O1 0.052(6) 0.066(6) 0.045(5) 0.012(4) 0.012(4) 0.035(5) O2 0.029(4) 0.072(5) 0.046(4) 0.017(4) 0.010(4) 0.018(4) O3 0.038(5) 0.037(4) 0.033(4) 0.007(3) 0.006(4) 0.024(4) O4 0.052(5) 0.047(4) 0.037(4) 0.007(3) 0.002(4) 0.028(4) O5 0.053(6) 0.076(7) 0.018(5) 0.002(4) 0.012(4) 0.006(5) O6 0.052(6) 0.077(6) 0.022(4) 0.000(4) 0.011(4) 0.016(5) O7 0.065(6) 0.065(5) 0.026(4) 0.001(4) -0.001(4) 0.035(5) O8 0.082(8) 0.052(6) 0.039(6) 0.026(4) 0.023(5) 0.055(6) N1 0.036(6) 0.068(7) 0.034(6) -0.009(5) 0.005(5) 0.023(5) N2 0.034(5) 0.055(6) 0.031(4) 0.000(4) 0.003(4) 0.012(4) N3 0.018(5) 0.021(4) 0.043(5) 0.001(3) 0.007(4) 0.004(4) N4 0.027(4) 0.034(4) 0.024(4) 0.000(3) 0.001(3) 0.014(4) N5 0.042(6) 0.060(6) 0.030(5) 0.000(4) -0.006(4) 0.025(5) N6 0.035(5) 0.049(5) 0.036(5) 0.003(4) 0.012(4) 0.012(4) N7 0.034(5) 0.031(5) 0.033(5) 0.005(4) 0.008(4) 0.015(4) N8 0.037(5) 0.026(4) 0.035(4) 0.008(3) 0.009(4) 0.016(4) C1 0.042(7) 0.080(9) 0.031(6) 0.005(5) 0.007(5) 0.027(6) C2 0.041(7) 0.087(9) 0.028(5) 0.014(5) -0.005(5) 0.022(7) C3 0.055(8) 0.098(10) 0.032(6) 0.007(6) 0.003(6) 0.042(8) C4 0.046(7) 0.073(8) 0.020(5) 0.008(5) 0.000(5) 0.023(6) C5 0.048(8) 0.094(10) 0.041(6) 0.010(6) 0.011(6) 0.018(7) C6 0.038(7) 0.091(9) 0.025(5) 0.003(5) -0.001(5) 0.014(6) C7 0.040(7) 0.060(7) 0.027(5) 0.007(4) 0.003(5) 0.021(5) C8 0.047(7) 0.071(8) 0.035(6) -0.004(5) 0.004(5) 0.025(6) C9 0.030(6) 0.070(8) 0.025(5) 0.004(5) -0.006(5) 0.002(6) C10 0.041(7) 0.048(6) 0.030(5) -0.001(4) -0.004(5) 0.018(5) C11 0.047(7) 0.035(5) 0.043(6) 0.007(4) 0.009(5) 0.029(5) C12 0.057(8) 0.033(5) 0.036(5) 0.003(4) 0.005(5) 0.019(5) C13 0.036(6) 0.033(5) 0.035(5) 0.013(4) 0.005(5) 0.009(4) C14 0.022(5) 0.020(5) 0.053(6) 0.003(4) 0.015(5) 0.012(4) C15 0.042(7) 0.046(6) 0.025(6) 0.002(5) 0.005(5) 0.018(6) C16 0.037(6) 0.029(5) 0.060(8) 0.004(5) 0.014(6) 0.018(5) C17 0.027(5) 0.026(4) 0.042(5) 0.011(4) 0.005(4) 0.023(4) C18 0.044(7) 0.061(7) 0.035(6) 0.014(5) 0.010(5) 0.028(6) C19 0.060(7) 0.042(6) 0.029(5) 0.005(4) 0.011(5) 0.039(5) C20 0.034(6) 0.039(6) 0.050(7) 0.018(5) 0.024(5) 0.025(5) C21 0.034(7) 0.058(7) 0.058(7) -0.027(6) 0.015(6) 0.004(5) C22 0.028(6) 0.054(7) 0.076(8) 0.001(6) 0.023(6) 0.013(5) C23 0.039(7) 0.073(9) 0.055(7) -0.011(6) 0.008(6) 0.026(7) C24 0.036(6) 0.069(8) 0.036(6) -0.004(5) 0.011(5) 0.023(6) C25 0.051(8) 0.057(7) 0.042(6) 0.003(5) 0.016(6) 0.016(6) C26 0.039(7) 0.069(8) 0.049(7) 0.003(6) 0.014(6) 0.017(6) C27 0.033(6) 0.069(8) 0.038(6) 0.005(5) 0.013(5) 0.022(5) C28 0.092(13) 0.082(11) 0.039(8) -0.015(7) 0.019(8) 0.028(10) C29 0.082(14) 0.085(10) 0.063(15) -0.020(10) 0.046(13) 0.029(10) C30 0.042(7) 0.051(6) 0.026(5) 0.003(4) 0.014(5) 0.023(5) C31 0.058(8) 0.042(6) 0.038(6) 0.018(4) 0.019(5) 0.033(5) C32 0.084(10) 0.064(8) 0.035(6) 0.025(6) 0.027(7) 0.060(7) C33 0.031(6) 0.035(6) 0.025(5) 0.005(4) 0.005(4) 0.013(5) C34 0.033(6) 0.034(6) 0.037(6) 0.014(5) 0.016(5) 0.010(5) C35 0.063(8) 0.050(6) 0.031(5) -0.005(4) -0.007(5) 0.034(6) C36 0.096(11) 0.055(7) 0.021(6) -0.010(5) -0.017(7) 0.054(8) C37 0.043(7) 0.033(5) 0.042(6) 0.006(4) 0.008(5) 0.017(5) C38 0.066(9) 0.059(8) 0.044(7) 0.027(6) 0.018(6) 0.043(8) C39 0.062(8) 0.056(7) 0.028(5) -0.001(5) 0.004(6) 0.049(7) C40 0.018(5) 0.034(6) 0.056(7) -0.005(5) -0.002(5) 0.008(5) O1W 0.046(5) 0.057(5) 0.044(5) 0.006(4) 0.007(4) 0.020(4) O2W 0.086(9) 0.060(6) 0.099(8) 0.010(6) 0.046(7) 0.027(6) O3W 0.109(11) 0.084(9) 0.099(10) 0.015(7) 0.033(8) 0.006(8) _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 Cd1 N5 2.256(11) 1_756 ? Cd1 N7 2.268(10) 1_635 ? Cd1 O1 2.333(11) . ? Cd1 O2 2.360(8) . ? Cd1 O3 2.362(8) . ? Cd1 O4 2.397(8) . ? Cd1 C10 2.674(10) . ? Cd1 C20 2.705(10) . ? Cd2 N1 2.259(12) 1_564 ? Cd2 N3 2.276(10) . ? Cd2 O5 2.337(10) . ? Cd2 O7 2.347(9) . ? Cd2 O8 2.377(10) . ? Cd2 O6 2.417(8) . ? Cd2 C30 2.720(11) . ? Cd2 C40 2.728(11) . ? O1 C10 1.279(13) . ? O2 C10 1.203(14) . ? O3 C20 1.254(13) . ? O4 C20 1.282(14) . ? O5 C30 1.232(13) . ? O6 C30 1.270(14) . ? O7 C40 1.327(15) . ? O8 C40 1.231(14) . ? N1 C3 1.266(17) . ? N1 C1 1.434(16) . ? N1 Cd2 2.259(12) 1_546 ? N2 C3 1.325(17) . ? N2 C2 1.347(14) . ? N2 C4 1.450(14) . ? N3 C13 1.324(15) . ? N3 C11 1.366(14) . ? N4 C13 1.320(14) . ? N4 C12 1.361(14) . ? N4 C14 1.418(13) . ? N5 C23 1.289(16) . ? N5 C21 1.372(16) . ? N5 Cd1 2.256(11) 1_354 ? N6 C23 1.330(16) . ? N6 C22 1.373(15) . ? N6 C24 1.419(14) . ? N7 C33 1.313(15) . ? N7 C31 1.379(14) . ? N7 Cd1 2.268(10) 1_475 ? N8 C33 1.360(13) . ? N8 C32 1.412(13) . ? N8 C34 1.444(15) . ? C1 C2 1.296(18) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C9 1.391(17) . ? C4 C5 1.415(17) . ? C5 C6 1.445(18) . ? C5 H5 0.9300 . ? C6 C7 1.285(17) . ? C6 H6 0.9300 . ? C7 C8 1.414(15) . ? C7 C10 1.518(13) . ? C8 C9 1.331(16) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.335(15) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.386(15) . ? C14 C19 1.421(15) . ? C15 C16 1.425(16) . ? C15 H15 0.9300 . ? C16 C17 1.351(16) . ? C16 H16 0.9300 . ? C17 C18 1.355(15) . ? C17 C20 1.506(13) . ? C18 C19 1.384(15) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C21 C22 1.303(18) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.387(17) . ? C24 C29 1.41(3) . ? C25 C26 1.382(18) . ? C25 H25 0.9300 . ? C26 C27 1.362(17) . ? C26 H26 0.9300 . ? C27 C28 1.37(2) . ? C27 C30 1.466(16) . ? C28 C29 1.39(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 C32 1.306(16) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.299(17) . ? C34 C35 1.413(15) . ? C35 C36 1.346(17) . ? C35 H35 0.9300 . ? C36 C37 1.420(16) . ? C36 H36 0.9300 . ? C37 C38 1.395(17) . ? C37 C40 1.434(15) . ? C38 C39 1.451(17) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? O1W H1W1 0.85(6) . ? O1W H2W1 0.86(9) . ? O2W H1W2 0.86(11) . ? O2W H2W2 0.9(2) . ? O3W H1W3 0.89(9) . ? 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 N5 Cd1 N7 95.0(4) 1_756 1_635 ? N5 Cd1 O1 144.4(3) 1_756 . ? N7 Cd1 O1 104.7(4) 1_635 . ? N5 Cd1 O2 89.9(3) 1_756 . ? N7 Cd1 O2 114.2(3) 1_635 . ? O1 Cd1 O2 55.1(3) . . ? N5 Cd1 O3 118.4(3) 1_756 . ? N7 Cd1 O3 87.9(3) 1_635 . ? O1 Cd1 O3 92.0(3) . . ? O2 Cd1 O3 143.1(3) . . ? N5 Cd1 O4 96.2(3) 1_756 . ? N7 Cd1 O4 143.0(3) 1_635 . ? O1 Cd1 O4 85.6(3) . . ? O2 Cd1 O4 100.9(3) . . ? O3 Cd1 O4 55.9(3) . . ? N5 Cd1 C10 116.0(3) 1_756 . ? N7 Cd1 C10 114.6(4) 1_635 . ? O1 Cd1 C10 28.6(3) . . ? O2 Cd1 C10 26.7(3) . . ? O3 Cd1 C10 118.1(3) . . ? O4 Cd1 C10 91.5(3) . . ? N5 Cd1 C20 110.1(4) 1_756 . ? N7 Cd1 C20 115.3(4) 1_635 . ? O1 Cd1 C20 88.0(3) . . ? O2 Cd1 C20 123.9(3) . . ? O3 Cd1 C20 27.6(3) . . ? O4 Cd1 C20 28.3(3) . . ? C10 Cd1 C20 105.9(3) . . ? N1 Cd2 N3 91.4(4) 1_564 . ? N1 Cd2 O5 136.6(3) 1_564 . ? N3 Cd2 O5 106.0(3) . . ? N1 Cd2 O7 96.0(4) 1_564 . ? N3 Cd2 O7 137.7(3) . . ? O5 Cd2 O7 96.7(4) . . ? N1 Cd2 O8 117.3(4) 1_564 . ? N3 Cd2 O8 84.0(3) . . ? O5 Cd2 O8 104.0(4) . . ? O7 Cd2 O8 55.6(3) . . ? N1 Cd2 O6 82.4(3) 1_564 . ? N3 Cd2 O6 122.8(3) . . ? O5 Cd2 O6 54.6(3) . . ? O7 Cd2 O6 99.6(3) . . ? O8 Cd2 O6 147.8(3) . . ? N1 Cd2 C30 109.9(3) 1_564 . ? N3 Cd2 C30 116.0(3) . . ? O5 Cd2 C30 26.9(3) . . ? O7 Cd2 C30 100.4(3) . . ? O8 Cd2 C30 128.0(4) . . ? O6 Cd2 C30 27.8(3) . . ? N1 Cd2 C40 111.6(4) 1_564 . ? N3 Cd2 C40 110.6(4) . . ? O5 Cd2 C40 99.2(4) . . ? O7 Cd2 C40 29.1(3) . . ? O8 Cd2 C40 26.8(3) . . ? O6 Cd2 C40 124.6(3) . . ? C30 Cd2 C40 115.0(3) . . ? C10 O1 Cd1 90.7(7) . . ? C10 O2 Cd1 91.4(6) . . ? C20 O3 Cd1 91.6(7) . . ? C20 O4 Cd1 89.3(6) . . ? C30 O5 Cd2 94.2(8) . . ? C30 O6 Cd2 89.5(6) . . ? C40 O7 Cd2 91.6(7) . . ? C40 O8 Cd2 92.7(8) . . ? C3 N1 C1 103.8(11) . . ? C3 N1 Cd2 128.5(10) . 1_546 ? C1 N1 Cd2 126.3(8) . 1_546 ? C3 N2 C2 106.1(10) . . ? C3 N2 C4 127.3(10) . . ? C2 N2 C4 126.6(10) . . ? C13 N3 C11 106.0(9) . . ? C13 N3 Cd2 133.8(8) . . ? C11 N3 Cd2 117.3(7) . . ? C13 N4 C12 107.0(9) . . ? C13 N4 C14 126.8(9) . . ? C12 N4 C14 126.2(8) . . ? C23 N5 C21 103.8(11) . . ? C23 N5 Cd1 128.9(9) . 1_354 ? C21 N5 Cd1 125.8(8) . 1_354 ? C23 N6 C22 104.5(9) . . ? C23 N6 C24 128.3(10) . . ? C22 N6 C24 127.2(10) . . ? C33 N7 C31 107.7(9) . . ? C33 N7 Cd1 134.8(8) . 1_475 ? C31 N7 Cd1 116.5(7) . 1_475 ? C33 N8 C32 105.5(9) . . ? C33 N8 C34 126.1(9) . . ? C32 N8 C34 127.5(8) . . ? C2 C1 N1 107.9(10) . . ? C2 C1 H1 126.0 . . ? N1 C1 H1 126.0 . . ? C1 C2 N2 108.6(11) . . ? C1 C2 H2 125.7 . . ? N2 C2 H2 125.7 . . ? N1 C3 N2 113.6(11) . . ? N1 C3 H3 123.2 . . ? N2 C3 H3 123.2 . . ? C9 C4 C5 121.8(11) . . ? C9 C4 N2 119.5(9) . . ? C5 C4 N2 118.7(11) . . ? C4 C5 C6 114.4(12) . . ? C4 C5 H5 122.8 . . ? C6 C5 H5 122.8 . . ? C7 C6 C5 123.8(11) . . ? C7 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C6 C7 C8 118.5(10) . . ? C6 C7 C10 122.8(10) . . ? C8 C7 C10 118.3(10) . . ? C9 C8 C7 123.0(12) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C8 C9 C4 118.2(10) . . ? C8 C9 H9 120.9 . . ? C4 C9 H9 120.9 . . ? O2 C10 O1 121.9(10) . . ? O2 C10 C7 121.8(9) . . ? O1 C10 C7 116.3(10) . . ? O2 C10 Cd1 61.9(6) . . ? O1 C10 Cd1 60.7(6) . . ? C7 C10 Cd1 171.6(8) . . ? C12 C11 N3 108.5(9) . . ? C12 C11 H11 125.7 . . ? N3 C11 H11 125.7 . . ? C11 C12 N4 107.5(9) . . ? C11 C12 H12 126.3 . . ? N4 C12 H12 126.3 . . ? N4 C13 N3 111.0(10) . . ? N4 C13 H13 124.5 . . ? N3 C13 H13 124.5 . . ? C15 C14 N4 121.3(10) . . ? C15 C14 C19 119.9(10) . . ? N4 C14 C19 118.6(9) . . ? C14 C15 C16 118.5(9) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C17 C16 C15 120.6(10) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.7(9) . . ? C16 C17 C20 118.6(9) . . ? C18 C17 C20 120.7(9) . . ? C17 C18 C19 122.0(10) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C14 118.2(9) . . ? C18 C19 H19 120.9 . . ? C14 C19 H19 120.9 . . ? O3 C20 O4 123.1(9) . . ? O3 C20 C17 119.6(10) . . ? O4 C20 C17 117.2(9) . . ? O3 C20 Cd1 60.8(5) . . ? O4 C20 Cd1 62.4(5) . . ? C17 C20 Cd1 175.3(7) . . ? C22 C21 N5 110.5(10) . . ? C22 C21 H21 124.8 . . ? N5 C21 H21 124.8 . . ? C21 C22 N6 107.3(10) . . ? C21 C22 H22 126.3 . . ? N6 C22 H22 126.3 . . ? N5 C23 N6 113.6(11) . . ? N5 C23 H23 123.2 . . ? N6 C23 H23 123.2 . . ? C25 C24 C29 119.6(15) . . ? C25 C24 N6 120.9(10) . . ? C29 C24 N6 119.4(14) . . ? C26 C25 C24 116.6(11) . . ? C26 C25 H25 121.7 . . ? C24 C25 H25 121.7 . . ? C27 C26 C25 125.3(12) . . ? C27 C26 H26 117.3 . . ? C25 C26 H26 117.3 . . ? C26 C27 C28 117.7(12) . . ? C26 C27 C30 123.2(11) . . ? C28 C27 C30 118.7(11) . . ? C27 C28 C29 120.1(16) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 120(2) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? O5 C30 O6 121.5(10) . . ? O5 C30 C27 119.7(10) . . ? O6 C30 C27 118.8(9) . . ? O5 C30 Cd2 59.0(6) . . ? O6 C30 Cd2 62.7(6) . . ? C27 C30 Cd2 178.0(8) . . ? C32 C31 N7 109.1(10) . . ? C32 C31 H31 125.5 . . ? N7 C31 H31 125.5 . . ? C31 C32 N8 107.6(10) . . ? C31 C32 H32 126.2 . . ? N8 C32 H32 126.2 . . ? N7 C33 N8 109.8(9) . . ? N7 C33 H33 125.1 . . ? N8 C33 H33 125.1 . . ? C39 C34 C35 120.5(12) . . ? C39 C34 N8 122.6(10) . . ? C35 C34 N8 116.8(10) . . ? C36 C35 C34 119.8(11) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 121.4(11) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C38 C37 C36 118.1(11) . . ? C38 C37 C40 121.2(11) . . ? C36 C37 C40 120.7(10) . . ? C37 C38 C39 118.0(11) . . ? C37 C38 H38 121.0 . . ? C39 C38 H38 121.0 . . ? C34 C39 C38 121.8(10) . . ? C34 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? O8 C40 O7 119.0(11) . . ? O8 C40 C37 121.2(11) . . ? O7 C40 C37 119.5(10) . . ? O8 C40 Cd2 60.5(6) . . ? O7 C40 Cd2 59.3(6) . . ? C37 C40 Cd2 176.2(8) . . ? H1W1 O1W H2W1 104(9) . . ? H1W2 O2W H2W2 102(15) . . ? 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 N5 Cd1 O1 C10 -6.7(10) 1_756 . . . ? N7 Cd1 O1 C10 114.8(7) 1_635 . . . ? O2 Cd1 O1 C10 5.3(6) . . . . ? O3 Cd1 O1 C10 -156.8(7) . . . . ? O4 Cd1 O1 C10 -101.3(7) . . . . ? C20 Cd1 O1 C10 -129.5(7) . . . . ? N5 Cd1 O2 C10 167.4(7) 1_756 . . . ? N7 Cd1 O2 C10 -97.1(8) 1_635 . . . ? O1 Cd1 O2 C10 -5.6(7) . . . . ? O3 Cd1 O2 C10 25.1(10) . . . . ? O4 Cd1 O2 C10 71.1(7) . . . . ? C20 Cd1 O2 C10 53.0(8) . . . . ? N5 Cd1 O3 C20 -79.0(7) 1_756 . . . ? N7 Cd1 O3 C20 -173.6(7) 1_635 . . . ? O1 Cd1 O3 C20 81.8(7) . . . . ? O2 Cd1 O3 C20 56.9(8) . . . . ? O4 Cd1 O3 C20 -1.6(6) . . . . ? C10 Cd1 O3 C20 69.4(7) . . . . ? N5 Cd1 O4 C20 121.8(6) 1_756 . . . ? N7 Cd1 O4 C20 14.9(9) 1_635 . . . ? O1 Cd1 O4 C20 -93.9(6) . . . . ? O2 Cd1 O4 C20 -147.0(6) . . . . ? O3 Cd1 O4 C20 1.6(6) . . . . ? C10 Cd1 O4 C20 -121.8(6) . . . . ? N1 Cd2 O5 C30 -6.5(11) 1_564 . . . ? N3 Cd2 O5 C30 -116.4(8) . . . . ? O7 Cd2 O5 C30 99.7(8) . . . . ? O8 Cd2 O5 C30 155.9(7) . . . . ? O6 Cd2 O5 C30 2.8(7) . . . . ? C40 Cd2 O5 C30 129.0(8) . . . . ? N1 Cd2 O6 C30 170.9(7) 1_564 . . . ? N3 Cd2 O6 C30 84.2(7) . . . . ? O5 Cd2 O6 C30 -2.7(7) . . . . ? O7 Cd2 O6 C30 -94.2(7) . . . . ? O8 Cd2 O6 C30 -58.0(9) . . . . ? C40 Cd2 O6 C30 -78.0(7) . . . . ? N1 Cd2 O7 C40 -124.8(7) 1_564 . . . ? N3 Cd2 O7 C40 -26.1(9) . . . . ? O5 Cd2 O7 C40 96.7(7) . . . . ? O8 Cd2 O7 C40 -5.6(6) . . . . ? O6 Cd2 O7 C40 151.9(6) . . . . ? C30 Cd2 O7 C40 123.7(7) . . . . ? N1 Cd2 O8 C40 83.9(9) 1_564 . . . ? N3 Cd2 O8 C40 172.4(8) . . . . ? O5 Cd2 O8 C40 -82.5(8) . . . . ? O7 Cd2 O8 C40 6.1(7) . . . . ? O6 Cd2 O8 C40 -38.8(11) . . . . ? C30 Cd2 O8 C40 -69.0(9) . . . . ? N1 Cd2 N3 C13 -62.9(10) 1_564 . . . ? O5 Cd2 N3 C13 76.9(10) . . . . ? O7 Cd2 N3 C13 -163.4(9) . . . . ? O8 Cd2 N3 C13 179.8(11) . . . . ? O6 Cd2 N3 C13 19.0(11) . . . . ? C30 Cd2 N3 C13 50.1(11) . . . . ? C40 Cd2 N3 C13 -176.6(10) . . . . ? N1 Cd2 N3 C11 94.7(8) 1_564 . . . ? O5 Cd2 N3 C11 -125.6(8) . . . . ? O7 Cd2 N3 C11 -5.9(10) . . . . ? O8 Cd2 N3 C11 -22.7(8) . . . . ? O6 Cd2 N3 C11 176.5(7) . . . . ? C30 Cd2 N3 C11 -152.4(8) . . . . ? C40 Cd2 N3 C11 -19.1(9) . . . . ? C3 N1 C1 C2 -2.5(16) . . . . ? Cd2 N1 C1 C2 164.9(10) 1_546 . . . ? N1 C1 C2 N2 2.4(16) . . . . ? C3 N2 C2 C1 -1.3(16) . . . . ? C4 N2 C2 C1 176.1(12) . . . . ? C1 N1 C3 N2 1.7(17) . . . . ? Cd2 N1 C3 N2 -165.3(9) 1_546 . . . ? C2 N2 C3 N1 -0.4(18) . . . . ? C4 N2 C3 N1 -177.8(12) . . . . ? C3 N2 C4 C9 161.5(14) . . . . ? C2 N2 C4 C9 -15.4(19) . . . . ? C3 N2 C4 C5 -20(2) . . . . ? C2 N2 C4 C5 163.0(14) . . . . ? C9 C4 C5 C6 -6(2) . . . . ? N2 C4 C5 C6 175.2(12) . . . . ? C4 C5 C6 C7 7(2) . . . . ? C5 C6 C7 C8 -5(2) . . . . ? C5 C6 C7 C10 -177.5(12) . . . . ? C6 C7 C8 C9 3(2) . . . . ? C10 C7 C8 C9 175.8(12) . . . . ? C7 C8 C9 C4 -3(2) . . . . ? C5 C4 C9 C8 5(2) . . . . ? N2 C4 C9 C8 -176.8(12) . . . . ? Cd1 O2 C10 O1 10.0(12) . . . . ? Cd1 O2 C10 C7 -171.4(10) . . . . ? Cd1 O1 C10 O2 -10.1(12) . . . . ? Cd1 O1 C10 C7 171.2(9) . . . . ? C6 C7 C10 O2 -170.7(13) . . . . ? C8 C7 C10 O2 17.2(17) . . . . ? C6 C7 C10 O1 8.0(18) . . . . ? C8 C7 C10 O1 -164.0(11) . . . . ? N5 Cd1 C10 O2 -14.0(8) 1_756 . . . ? N7 Cd1 C10 O2 95.3(7) 1_635 . . . ? O1 Cd1 C10 O2 170.3(12) . . . . ? O3 Cd1 C10 O2 -163.2(7) . . . . ? O4 Cd1 C10 O2 -111.7(7) . . . . ? C20 Cd1 C10 O2 -136.4(7) . . . . ? N5 Cd1 C10 O1 175.7(7) 1_756 . . . ? N7 Cd1 C10 O1 -75.0(8) 1_635 . . . ? O2 Cd1 C10 O1 -170.3(12) . . . . ? O3 Cd1 C10 O1 26.5(8) . . . . ? O4 Cd1 C10 O1 78.0(7) . . . . ? C20 Cd1 C10 O1 53.3(7) . . . . ? C13 N3 C11 C12 -1.4(13) . . . . ? Cd2 N3 C11 C12 -164.7(8) . . . . ? N3 C11 C12 N4 0.3(13) . . . . ? C13 N4 C12 C11 0.9(13) . . . . ? C14 N4 C12 C11 -179.5(10) . . . . ? C12 N4 C13 N3 -1.8(13) . . . . ? C14 N4 C13 N3 178.6(9) . . . . ? C11 N3 C13 N4 2.0(13) . . . . ? Cd2 N3 C13 N4 161.3(7) . . . . ? C13 N4 C14 C15 13.7(16) . . . . ? C12 N4 C14 C15 -165.8(11) . . . . ? C13 N4 C14 C19 -170.7(10) . . . . ? C12 N4 C14 C19 9.8(16) . . . . ? N4 C14 C15 C16 178.7(10) . . . . ? C19 C14 C15 C16 3.2(17) . . . . ? C14 C15 C16 C17 -4.1(17) . . . . ? C15 C16 C17 C18 2.6(17) . . . . ? C15 C16 C17 C20 -177.6(10) . . . . ? C16 C17 C18 C19 0.0(18) . . . . ? C20 C17 C18 C19 -179.9(11) . . . . ? C17 C18 C19 C14 -0.9(18) . . . . ? C15 C14 C19 C18 -0.8(17) . . . . ? N4 C14 C19 C18 -176.4(10) . . . . ? Cd1 O3 C20 O4 3.0(11) . . . . ? Cd1 O3 C20 C17 -174.7(8) . . . . ? Cd1 O4 C20 O3 -2.9(11) . . . . ? Cd1 O4 C20 C17 174.8(8) . . . . ? C16 C17 C20 O3 -13.8(15) . . . . ? C18 C17 C20 O3 166.1(11) . . . . ? C16 C17 C20 O4 168.5(10) . . . . ? C18 C17 C20 O4 -11.7(15) . . . . ? N5 Cd1 C20 O3 113.1(6) 1_756 . . . ? N7 Cd1 C20 O3 7.1(7) 1_635 . . . ? O1 Cd1 C20 O3 -98.3(7) . . . . ? O2 Cd1 C20 O3 -142.7(6) . . . . ? O4 Cd1 C20 O3 177.2(10) . . . . ? C10 Cd1 C20 O3 -120.8(6) . . . . ? N5 Cd1 C20 O4 -64.1(7) 1_756 . . . ? N7 Cd1 C20 O4 -170.1(6) 1_635 . . . ? O1 Cd1 C20 O4 84.5(6) . . . . ? O2 Cd1 C20 O4 40.1(7) . . . . ? O3 Cd1 C20 O4 -177.2(10) . . . . ? C10 Cd1 C20 O4 62.0(7) . . . . ? C23 N5 C21 C22 5.0(16) . . . . ? Cd1 N5 C21 C22 -161.5(9) 1_354 . . . ? N5 C21 C22 N6 -1.7(16) . . . . ? C23 N6 C22 C21 -2.2(15) . . . . ? C24 N6 C22 C21 177.4(12) . . . . ? C21 N5 C23 N6 -6.6(16) . . . . ? Cd1 N5 C23 N6 159.3(8) 1_354 . . . ? C22 N6 C23 N5 5.7(16) . . . . ? C24 N6 C23 N5 -173.9(11) . . . . ? C23 N6 C24 C25 -158.8(13) . . . . ? C22 N6 C24 C25 21.7(19) . . . . ? C23 N6 C24 C29 21(2) . . . . ? C22 N6 C24 C29 -158.0(18) . . . . ? C29 C24 C25 C26 1(2) . . . . ? N6 C24 C25 C26 -178.9(11) . . . . ? C24 C25 C26 C27 1(2) . . . . ? C25 C26 C27 C28 -6(2) . . . . ? C25 C26 C27 C30 -178.5(12) . . . . ? C26 C27 C28 C29 9(3) . . . . ? C30 C27 C28 C29 -178.5(19) . . . . ? C27 C28 C29 C24 -7(4) . . . . ? C25 C24 C29 C28 2(3) . . . . ? N6 C24 C29 C28 -178.3(19) . . . . ? Cd2 O5 C30 O6 -5.0(12) . . . . ? Cd2 O5 C30 C27 178.3(9) . . . . ? Cd2 O6 C30 O5 4.8(12) . . . . ? Cd2 O6 C30 C27 -178.5(9) . . . . ? C26 C27 C30 O5 -159.9(13) . . . . ? C28 C27 C30 O5 27.7(19) . . . . ? C26 C27 C30 O6 23.3(18) . . . . ? C28 C27 C30 O6 -149.0(14) . . . . ? N1 Cd2 C30 O5 175.3(8) 1_564 . . . ? N3 Cd2 C30 O5 73.4(8) . . . . ? O7 Cd2 C30 O5 -84.4(8) . . . . ? O8 Cd2 C30 O5 -30.2(9) . . . . ? O6 Cd2 C30 O5 -175.2(12) . . . . ? C40 Cd2 C30 O5 -57.9(9) . . . . ? N1 Cd2 C30 O6 -9.5(8) 1_564 . . . ? N3 Cd2 C30 O6 -111.4(7) . . . . ? O5 Cd2 C30 O6 175.2(12) . . . . ? O7 Cd2 C30 O6 90.8(7) . . . . ? O8 Cd2 C30 O6 145.0(6) . . . . ? C40 Cd2 C30 O6 117.3(7) . . . . ? C33 N7 C31 C32 -1.9(15) . . . . ? Cd1 N7 C31 C32 169.0(10) 1_475 . . . ? N7 C31 C32 N8 4.3(15) . . . . ? C33 N8 C32 C31 -5.0(15) . . . . ? C34 N8 C32 C31 -174.9(11) . . . . ? C31 N7 C33 N8 -1.4(13) . . . . ? Cd1 N7 C33 N8 -169.8(8) 1_475 . . . ? C32 N8 C33 N7 3.9(13) . . . . ? C34 N8 C33 N7 174.0(9) . . . . ? C33 N8 C34 C39 -3.6(17) . . . . ? C32 N8 C34 C39 164.3(13) . . . . ? C33 N8 C34 C35 173.2(11) . . . . ? C32 N8 C34 C35 -18.9(17) . . . . ? C39 C34 C35 C36 -8(2) . . . . ? N8 C34 C35 C36 175.6(13) . . . . ? C34 C35 C36 C37 8(2) . . . . ? C35 C36 C37 C38 -3(2) . . . . ? C35 C36 C37 C40 174.8(14) . . . . ? C36 C37 C38 C39 -2(2) . . . . ? C40 C37 C38 C39 -180.0(12) . . . . ? C35 C34 C39 C38 2(2) . . . . ? N8 C34 C39 C38 179.0(11) . . . . ? C37 C38 C39 C34 2(2) . . . . ? Cd2 O8 C40 O7 -10.2(11) . . . . ? Cd2 O8 C40 C37 176.1(9) . . . . ? Cd2 O7 C40 O8 10.3(12) . . . . ? Cd2 O7 C40 C37 -175.9(9) . . . . ? C38 C37 C40 O8 13.5(18) . . . . ? C36 C37 C40 O8 -164.6(13) . . . . ? C38 C37 C40 O7 -160.2(12) . . . . ? C36 C37 C40 O7 21.7(18) . . . . ? N1 Cd2 C40 O8 -108.2(8) 1_564 . . . ? N3 Cd2 C40 O8 -8.0(8) . . . . ? O5 Cd2 C40 O8 103.0(8) . . . . ? O7 Cd2 C40 O8 -169.6(12) . . . . ? O6 Cd2 C40 O8 156.0(7) . . . . ? C30 Cd2 C40 O8 125.8(8) . . . . ? N1 Cd2 C40 O7 61.4(7) 1_564 . . . ? N3 Cd2 C40 O7 161.6(7) . . . . ? O5 Cd2 C40 O7 -87.4(7) . . . . ? O8 Cd2 C40 O7 169.6(12) . . . . ? O6 Cd2 C40 O7 -34.3(8) . . . . ? C30 Cd2 C40 O7 -64.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.002 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.139 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 773581' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 Cd N2 O4' _chemical_formula_sum 'C12 H10 Cd N2 O4' _chemical_formula_weight 358.63 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.725(3) _cell_length_b 8.100(5) _cell_length_c 16.297(4) _cell_angle_alpha 90.000 _cell_angle_beta 103.873(5) _cell_angle_gamma 90.000 _cell_volume 2399.7(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7340 _exptl_absorpt_correction_T_max 0.8102 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6007 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2460 _reflns_number_gt 1958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.2690P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2460 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 Cd1 Cd 0.0000 0.15773(4) 0.2500 0.02565(15) Uani 1 2 d S . . Cd2 Cd 0.0000 -0.34514(4) 0.2500 0.02629(15) Uani 1 2 d S . . O1 O -0.00973(16) -0.0596(3) 0.15514(18) 0.0378(6) Uani 1 1 d . . . O2 O -0.09173(13) -0.2588(3) 0.14487(16) 0.0410(6) Uani 1 1 d . . . O3 O -0.07841(14) -0.4284(3) 0.32663(16) 0.0405(6) Uani 1 1 d . . . O4 O 0.00488(17) -0.6229(4) 0.3477(2) 0.0445(7) Uani 1 1 d . . . N1 N -0.37695(14) 0.3098(4) -0.21888(17) 0.0313(6) Uani 1 1 d . . . N2 N -0.27112(13) 0.2145(3) -0.14464(16) 0.0287(6) Uani 1 1 d . . . C1 C -0.3212(2) 0.3905(5) -0.2434(3) 0.0455(10) Uani 1 1 d . . . H1 H -0.3274 0.4723 -0.2845 0.055 Uiso 1 1 calc R . . C2 C -0.2561(2) 0.3331(5) -0.1987(3) 0.0482(11) Uani 1 1 d . . . H2 H -0.2098 0.3669 -0.2034 0.058 Uiso 1 1 calc R . . C3 C -0.34461(16) 0.2062(4) -0.1598(2) 0.0305(7) Uani 1 1 d . . . H3 H -0.3697 0.1352 -0.1317 0.037 Uiso 1 1 calc R . . C4 C -0.22017(17) 0.1269(4) -0.0791(2) 0.0279(7) Uani 1 1 d . . . C5 C -0.24528(19) 0.0058(4) -0.0339(3) 0.0404(9) Uani 1 1 d . . . H5 H -0.2949 -0.0218 -0.0470 0.049 Uiso 1 1 calc R . . C6 C -0.1971(2) -0.0744(4) 0.0306(2) 0.0391(9) Uani 1 1 d . . . H6 H -0.2144 -0.1560 0.0611 0.047 Uiso 1 1 calc R . . C7 C -0.12289(16) -0.0346(4) 0.05064(19) 0.0281(7) Uani 1 1 d . . . C8 C -0.09843(19) 0.0849(4) 0.0046(2) 0.0329(8) Uani 1 1 d . . . H8 H -0.0487 0.1122 0.0176 0.039 Uiso 1 1 calc R . . C9 C -0.14641(18) 0.1661(4) -0.0612(2) 0.0336(8) Uani 1 1 d . . . H9 H -0.1291 0.2457 -0.0927 0.040 Uiso 1 1 calc R . . C10 C -0.07160(19) -0.1237(4) 0.1214(2) 0.0314(7) Uani 1 1 d . . . C11 C -0.05132(18) -0.5572(4) 0.3628(2) 0.0378(8) Uani 1 1 d . . . C12 C -0.0871(3) -0.6345(6) 0.4264(3) 0.0678(14) Uani 1 1 d . . . H12A H -0.0827 -0.7525 0.4241 0.102 Uiso 1 1 calc R . . H12B H -0.1381 -0.6044 0.4139 0.102 Uiso 1 1 calc R . . H12C H -0.0632 -0.5963 0.4820 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0204(2) 0.0231(3) 0.0305(2) 0.000 0.00037(16) 0.000 Cd2 0.0236(2) 0.0295(3) 0.0248(2) 0.000 0.00382(16) 0.000 O1 0.0309(14) 0.0435(15) 0.0332(14) -0.0066(13) -0.0039(11) 0.0056(12) O2 0.0436(15) 0.0407(15) 0.0342(14) 0.0107(12) -0.0019(12) 0.0010(12) O3 0.0418(15) 0.0384(15) 0.0462(15) 0.0087(12) 0.0198(12) 0.0078(11) O4 0.0307(15) 0.0485(16) 0.0523(19) -0.0201(14) 0.0058(13) 0.0032(12) N1 0.0268(14) 0.0353(16) 0.0297(15) 0.0026(12) 0.0028(12) -0.0013(11) N2 0.0219(13) 0.0317(15) 0.0312(14) 0.0080(12) 0.0037(11) -0.0003(11) C1 0.033(2) 0.053(2) 0.049(2) 0.0231(19) 0.0070(18) -0.0017(16) C2 0.031(2) 0.059(3) 0.053(3) 0.028(2) 0.0073(18) -0.0039(17) C3 0.0221(16) 0.0339(18) 0.0344(18) 0.0076(14) 0.0045(13) 0.0009(13) C4 0.0252(16) 0.0298(16) 0.0272(17) 0.0029(14) 0.0034(14) 0.0032(13) C5 0.0241(17) 0.046(2) 0.049(2) 0.0108(16) 0.0035(15) -0.0069(15) C6 0.037(2) 0.036(2) 0.040(2) 0.0104(16) 0.0033(17) -0.0047(15) C7 0.0276(16) 0.0283(17) 0.0244(15) -0.0016(14) -0.0014(13) 0.0023(13) C8 0.0255(18) 0.034(2) 0.0348(19) -0.0035(14) -0.0011(15) -0.0030(13) C9 0.0306(19) 0.037(2) 0.0335(19) 0.0055(14) 0.0076(16) -0.0013(13) C10 0.035(2) 0.0333(18) 0.0214(17) -0.0024(14) -0.0022(14) 0.0083(15) C11 0.0307(18) 0.0368(19) 0.0471(19) -0.0069(17) 0.0086(15) -0.0003(15) C12 0.068(3) 0.069(3) 0.075(3) 0.026(3) 0.036(3) 0.006(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 Cd1 N1 2.253(3) 8_556 ? Cd1 N1 2.253(3) 7_455 ? Cd1 O1 2.321(3) . ? Cd1 O1 2.321(3) 2 ? Cd1 O4 2.373(3) 1_565 ? Cd1 O4 2.373(3) 2_565 ? Cd2 O2 2.228(2) 2 ? Cd2 O2 2.228(2) . ? Cd2 O3 2.247(2) 2 ? Cd2 O3 2.247(2) . ? O1 C10 1.268(5) . ? O2 C10 1.247(4) . ? O3 C11 1.245(4) . ? O4 C11 1.255(4) . ? O4 Cd1 2.373(3) 1_545 ? N1 C3 1.311(4) . ? N1 C1 1.370(4) . ? N1 Cd1 2.253(3) 7_455 ? N2 C3 1.340(4) . ? N2 C2 1.377(4) . ? N2 C4 1.437(4) . ? C1 C2 1.343(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.376(5) . ? C4 C9 1.379(5) . ? C5 C6 1.373(5) . ? C5 H5 0.9300 . ? C6 C7 1.387(5) . ? C6 H6 0.9300 . ? C7 C8 1.370(5) . ? C7 C10 1.498(4) . ? C8 C9 1.388(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.499(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 N1 Cd1 N1 166.59(15) 8_556 7_455 ? N1 Cd1 O1 98.70(10) 8_556 . ? N1 Cd1 O1 91.48(10) 7_455 . ? N1 Cd1 O1 91.48(10) 8_556 2 ? N1 Cd1 O1 98.70(10) 7_455 2 ? O1 Cd1 O1 81.34(15) . 2 ? N1 Cd1 O4 83.61(10) 8_556 1_565 ? N1 Cd1 O4 86.35(10) 7_455 1_565 ? O1 Cd1 O4 177.56(8) . 1_565 ? O1 Cd1 O4 97.85(14) 2 1_565 ? N1 Cd1 O4 86.35(10) 8_556 2_565 ? N1 Cd1 O4 83.61(10) 7_455 2_565 ? O1 Cd1 O4 97.85(14) . 2_565 ? O1 Cd1 O4 177.56(8) 2 2_565 ? O4 Cd1 O4 83.05(17) 1_565 2_565 ? O2 Cd2 O2 143.41(14) 2 . ? O2 Cd2 O3 92.04(9) 2 2 ? O2 Cd2 O3 98.79(10) . 2 ? O2 Cd2 O3 98.79(10) 2 . ? O2 Cd2 O3 92.04(9) . . ? O3 Cd2 O3 145.07(13) 2 . ? C10 O1 Cd1 121.1(2) . . ? C10 O2 Cd2 106.1(2) . . ? C11 O3 Cd2 105.6(2) . . ? C11 O4 Cd1 123.3(3) . 1_545 ? C3 N1 C1 105.6(3) . . ? C3 N1 Cd1 120.5(2) . 7_455 ? C1 N1 Cd1 133.5(2) . 7_455 ? C3 N2 C2 106.0(3) . . ? C3 N2 C4 125.5(3) . . ? C2 N2 C4 128.2(3) . . ? C2 C1 N1 109.5(3) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? C1 C2 N2 106.9(3) . . ? C1 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? N1 C3 N2 112.1(3) . . ? N1 C3 H3 124.0 . . ? N2 C3 H3 124.0 . . ? C5 C4 C9 120.3(3) . . ? C5 C4 N2 119.9(3) . . ? C9 C4 N2 119.8(3) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 118.9(3) . . ? C8 C7 C10 121.7(3) . . ? C6 C7 C10 119.4(3) . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C4 C9 C8 119.0(3) . . ? C4 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? O2 C10 O1 122.6(3) . . ? O2 C10 C7 118.3(3) . . ? O1 C10 C7 119.1(3) . . ? O3 C11 O4 121.9(3) . . ? O3 C11 C12 118.6(3) . . ? O4 C11 C12 119.5(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 N1 Cd1 O1 C10 178.4(3) 8_556 . . . ? N1 Cd1 O1 C10 -10.4(3) 7_455 . . . ? O1 Cd1 O1 C10 88.2(3) 2 . . . ? O4 Cd1 O1 C10 -94.1(3) 2_565 . . . ? O2 Cd2 O2 C10 29.9(2) 2 . . . ? O3 Cd2 O2 C10 -75.7(2) 2 . . . ? O3 Cd2 O2 C10 137.7(2) . . . . ? O2 Cd2 O3 C11 -72.0(2) 2 . . . ? O2 Cd2 O3 C11 143.0(2) . . . . ? O3 Cd2 O3 C11 34.5(2) 2 . . . ? C3 N1 C1 C2 0.3(5) . . . . ? Cd1 N1 C1 C2 173.2(3) 7_455 . . . ? N1 C1 C2 N2 -0.4(5) . . . . ? C3 N2 C2 C1 0.3(4) . . . . ? C4 N2 C2 C1 -174.3(3) . . . . ? C1 N1 C3 N2 -0.2(4) . . . . ? Cd1 N1 C3 N2 -174.2(2) 7_455 . . . ? C2 N2 C3 N1 0.0(4) . . . . ? C4 N2 C3 N1 174.7(3) . . . . ? C3 N2 C4 C5 9.8(5) . . . . ? C2 N2 C4 C5 -176.7(4) . . . . ? C3 N2 C4 C9 -169.4(3) . . . . ? C2 N2 C4 C9 4.1(5) . . . . ? C9 C4 C5 C6 1.4(5) . . . . ? N2 C4 C5 C6 -177.9(3) . . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C5 C6 C7 C8 -0.5(5) . . . . ? C5 C6 C7 C10 179.8(3) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C10 C7 C8 C9 179.7(3) . . . . ? C5 C4 C9 C8 -1.8(5) . . . . ? N2 C4 C9 C8 177.4(3) . . . . ? C7 C8 C9 C4 1.1(5) . . . . ? Cd2 O2 C10 O1 0.2(4) . . . . ? Cd2 O2 C10 C7 -179.8(2) . . . . ? Cd1 O1 C10 O2 -103.2(3) . . . . ? Cd1 O1 C10 C7 76.8(3) . . . . ? C8 C7 C10 O2 -160.2(3) . . . . ? C6 C7 C10 O2 19.4(5) . . . . ? C8 C7 C10 O1 19.8(5) . . . . ? C6 C7 C10 O1 -160.6(3) . . . . ? Cd2 O3 C11 O4 -5.9(4) . . . . ? Cd2 O3 C11 C12 173.8(3) . . . . ? Cd1 O4 C11 O3 -95.9(4) 1_545 . . . ? Cd1 O4 C11 C12 84.4(4) 1_545 . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.675 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.177 data_6 _database_code_depnum_ccdc_archive 'CCDC 773582' #TrackingRef 'Compound 6.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H48 Cd2 N10 O13' _chemical_formula_sum 'C50 H48 Cd2 N10 O13' _chemical_formula_weight 1221.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' _cell_length_a 14.865(5) _cell_length_b 14.865(5) _cell_length_c 13.139(4) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 2903.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.8965 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15748 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.49 _reflns_number_total 2694 _reflns_number_gt 2430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. To get reasonable bond length and bond angle around C11, C12 and C13 atoms, DFIX and DANG restraints were added. ; _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^)+(0.1258P)^2^+14.5225P] 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 refU _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 -0.03(10) _refine_ls_number_reflns 2694 _refine_ls_number_parameters 171 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2269 _refine_ls_wR_factor_gt 0.2208 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.226 _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 Cd1 Cd 0.26947(5) 0.26947(5) 0.5000 0.0260(3) Uani 1 2 d S . . O1 O 0.1406(5) 0.7180(5) 1.1013(5) 0.0341(16) Uani 1 1 d . . . O2 O 0.2554(5) 0.6352(5) 1.1525(5) 0.0351(17) Uani 1 1 d . . . N1 N 0.1801(5) 0.3442(6) 0.6128(6) 0.0281(17) Uani 1 1 d . . . N2 N 0.1428(5) 0.4234(5) 0.7473(7) 0.0277(16) Uani 1 1 d . . . N3 N 0.3802(6) 0.3802(6) 0.5000 0.038(3) Uani 1 2 d S . . C1 C 0.0864(7) 0.3430(7) 0.6239(7) 0.029(2) Uani 1 1 d . . . H1 H 0.0465 0.3130 0.5813 0.035 Uiso 1 1 calc R . . C2 C 0.0632(7) 0.3923(7) 0.7061(8) 0.030(2) Uani 1 1 d . . . H2 H 0.0054 0.4031 0.7301 0.036 Uiso 1 1 calc R . . C3 C 0.2113(6) 0.3927(7) 0.6888(7) 0.029(2) Uani 1 1 d . . . H3 H 0.2718 0.4042 0.7006 0.035 Uiso 1 1 calc R . . C4 C 0.1541(6) 0.4787(6) 0.8359(7) 0.0239(19) Uani 1 1 d . . . C5 C 0.0960(7) 0.5501(7) 0.8498(8) 0.030(2) Uani 1 1 d . . . H5 H 0.0496 0.5604 0.8038 0.035 Uiso 1 1 calc R . . C6 C 0.1077(7) 0.6070(7) 0.9340(7) 0.029(2) Uani 1 1 d . . . H6 H 0.0688 0.6551 0.9444 0.035 Uiso 1 1 calc R . . C7 C 0.1775(6) 0.5911(6) 1.0016(8) 0.0258(18) Uani 1 1 d . . . C8 C 0.2340(7) 0.5180(7) 0.9868(8) 0.030(2) Uani 1 1 d . . . H8 H 0.2793 0.5062 1.0337 0.036 Uiso 1 1 calc R . . C9 C 0.2237(8) 0.4616(7) 0.9022(8) 0.033(2) Uani 1 1 d . . . H9 H 0.2628 0.4138 0.8911 0.039 Uiso 1 1 calc R . . C10 C 0.1926(7) 0.6518(7) 1.0919(7) 0.029(2) Uani 1 1 d . . . C11 C 0.4636(14) 0.3580(15) 0.525(2) 0.078(9) Uani 1 1 d D . . H11 H 0.4755 0.2987 0.5434 0.150 Uiso 1 1 calc R . . C12 C 0.5377(15) 0.4225(13) 0.526(2) 0.092(9) Uani 1 1 d D . . H12 H 0.5968 0.4073 0.5410 0.140 Uiso 1 1 calc R . . C13 C 0.5099(14) 0.5099(14) 0.5000 0.080(9) Uani 1 2 d SD . . H13 H 0.5541 0.5541 0.5000 0.120 Uiso 1 2 calc SR . . OW1 O 0.4071(7) 0.3536(7) 0.7924(8) 0.064(3) Uani 1 1 d . . . OW2 O 0.5837(12) 0.4163(12) 0.7500 0.050(5) Uiso 0.50 2 d SP . . 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 Cd1 0.0294(4) 0.0294(4) 0.0192(5) -0.0003(3) 0.0003(3) 0.0054(4) O1 0.032(4) 0.037(4) 0.033(4) -0.014(3) 0.003(3) -0.002(3) O2 0.043(5) 0.037(4) 0.025(3) -0.006(3) -0.004(3) -0.003(3) N1 0.025(4) 0.034(4) 0.025(4) -0.004(3) -0.003(3) 0.003(3) N2 0.029(4) 0.032(4) 0.022(4) -0.005(4) -0.002(4) 0.003(3) N3 0.040(4) 0.040(4) 0.034(6) 0.009(5) -0.009(5) 0.004(5) C1 0.032(5) 0.033(5) 0.023(5) -0.004(4) -0.005(4) 0.000(4) C2 0.023(5) 0.035(5) 0.030(5) -0.002(4) 0.001(4) 0.005(4) C3 0.022(5) 0.037(5) 0.029(5) -0.006(4) -0.002(4) 0.003(4) C4 0.024(5) 0.027(5) 0.021(4) -0.003(4) 0.004(4) -0.001(4) C5 0.028(5) 0.035(5) 0.025(5) 0.002(4) 0.003(4) -0.001(4) C6 0.031(5) 0.029(5) 0.028(5) -0.001(4) 0.001(4) -0.002(4) C7 0.029(4) 0.028(4) 0.021(4) -0.004(4) 0.008(5) -0.010(3) C8 0.025(4) 0.037(5) 0.029(5) -0.006(4) -0.001(5) -0.005(4) C9 0.030(5) 0.032(5) 0.036(5) -0.006(4) 0.002(5) 0.001(4) C10 0.037(5) 0.029(5) 0.021(4) -0.003(4) 0.005(4) -0.007(4) C11 0.096(16) 0.097(16) 0.04(3) 0.047(18) 0.005(18) 0.024(13) C12 0.107(19) 0.12(2) 0.05(2) 0.000(16) 0.000(15) 0.000(17) C13 0.100(13) 0.100(13) 0.04(2) 0.000(15) 0.000(15) 0.000(16) OW1 0.059(6) 0.065(6) 0.068(6) -0.005(5) -0.017(5) 0.007(5) _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 Cd1 N1 2.280(8) 6_556 ? Cd1 N1 2.280(8) . ? Cd1 N3 2.328(13) . ? Cd1 O2 2.400(7) 7_454 ? Cd1 O2 2.400(7) 4_546 ? Cd1 O1 2.488(7) 4_546 ? Cd1 O1 2.488(7) 7_454 ? O1 C10 1.258(13) . ? O1 Cd1 2.488(7) 4_556 ? O2 C10 1.251(13) . ? O2 Cd1 2.400(7) 4_556 ? N1 C3 1.315(13) . ? N1 C1 1.400(13) . ? N2 C3 1.354(12) . ? N2 C2 1.380(13) . ? N2 C4 1.436(12) . ? N3 C11 1.32(2) . ? N3 C11 1.32(2) 6_556 ? C1 C2 1.350(14) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C9 1.375(15) . ? C4 C5 1.381(14) . ? C5 C6 1.403(14) . ? C5 H5 0.9300 . ? C6 C7 1.386(14) . ? C6 H6 0.9300 . ? C7 C8 1.387(14) . ? C7 C10 1.508(13) . ? C8 C9 1.401(14) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.460(18) . ? C11 H11 0.9300 . ? C12 C13 1.404(17) . ? C12 H12 0.9300 . ? C13 C12 1.404(17) 6_556 ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 172.3(4) 6_556 . ? N1 Cd1 N3 93.9(2) 6_556 . ? N1 Cd1 N3 93.9(2) . . ? N1 Cd1 O2 88.2(3) 6_556 7_454 ? N1 Cd1 O2 86.4(3) . 7_454 ? N3 Cd1 O2 134.17(17) . 7_454 ? N1 Cd1 O2 86.4(3) 6_556 4_546 ? N1 Cd1 O2 88.2(3) . 4_546 ? N3 Cd1 O2 134.17(17) . 4_546 ? O2 Cd1 O2 91.7(3) 7_454 4_546 ? N1 Cd1 O1 94.0(3) 6_556 4_546 ? N1 Cd1 O1 87.3(3) . 4_546 ? N3 Cd1 O1 80.64(17) . 4_546 ? O2 Cd1 O1 144.9(2) 7_454 4_546 ? O2 Cd1 O1 53.7(2) 4_546 4_546 ? N1 Cd1 O1 87.3(3) 6_556 7_454 ? N1 Cd1 O1 94.0(3) . 7_454 ? N3 Cd1 O1 80.64(17) . 7_454 ? O2 Cd1 O1 53.7(2) 7_454 7_454 ? O2 Cd1 O1 144.9(2) 4_546 7_454 ? O1 Cd1 O1 161.3(3) 4_546 7_454 ? C10 O1 Cd1 89.3(6) . 4_556 ? C10 O2 Cd1 93.5(6) . 4_556 ? C3 N1 C1 106.2(8) . . ? C3 N1 Cd1 123.7(6) . . ? C1 N1 Cd1 129.9(7) . . ? C3 N2 C2 108.0(8) . . ? C3 N2 C4 124.4(8) . . ? C2 N2 C4 127.6(8) . . ? C11 N3 C11 122(2) . 6_556 ? C11 N3 Cd1 119.0(10) . . ? C11 N3 Cd1 119.0(10) 6_556 . ? C2 C1 N1 109.3(9) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? C1 C2 N2 106.0(9) . . ? C1 C2 H2 127.0 . . ? N2 C2 H2 127.0 . . ? N1 C3 N2 110.5(8) . . ? N1 C3 H3 124.7 . . ? N2 C3 H3 124.7 . . ? C9 C4 C5 122.0(9) . . ? C9 C4 N2 119.7(9) . . ? C5 C4 N2 118.3(9) . . ? C4 C5 C6 119.3(9) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 119.7(9) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 119.8(9) . . ? C6 C7 C10 120.9(9) . . ? C8 C7 C10 119.2(9) . . ? C7 C8 C9 120.9(10) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C4 C9 C8 118.3(10) . . ? C4 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? O2 C10 O1 123.4(9) . . ? O2 C10 C7 119.7(9) . . ? O1 C10 C7 117.0(9) . . ? N3 C11 C12 122.9(18) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 113(2) . . ? C13 C12 H12 123.7 . . ? C11 C12 H12 123.7 . . ? C12 C13 C12 127(3) 6_556 . ? C12 C13 H13 116.5 6_556 . ? C12 C13 H13 116.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cd1 N1 C3 -35.7(8) . . . . ? O2 Cd1 N1 C3 -169.8(8) 7_454 . . . ? O2 Cd1 N1 C3 98.4(8) 4_546 . . . ? O1 Cd1 N1 C3 44.7(8) 4_546 . . . ? O1 Cd1 N1 C3 -116.6(8) 7_454 . . . ? N3 Cd1 N1 C1 150.9(8) . . . . ? O2 Cd1 N1 C1 16.8(9) 7_454 . . . ? O2 Cd1 N1 C1 -75.0(9) 4_546 . . . ? O1 Cd1 N1 C1 -128.7(9) 4_546 . . . ? O1 Cd1 N1 C1 70.0(9) 7_454 . . . ? N1 Cd1 N3 C11 -57.3(16) 6_556 . . . ? N1 Cd1 N3 C11 122.7(16) . . . . ? O2 Cd1 N3 C11 -148.5(16) 7_454 . . . ? O2 Cd1 N3 C11 31.5(16) 4_546 . . . ? O1 Cd1 N3 C11 36.2(16) 4_546 . . . ? O1 Cd1 N3 C11 -143.8(16) 7_454 . . . ? N1 Cd1 N3 C11 122.7(16) 6_556 . . 6_556 ? N1 Cd1 N3 C11 -57.3(16) . . . 6_556 ? O2 Cd1 N3 C11 31.5(16) 7_454 . . 6_556 ? O2 Cd1 N3 C11 -148.5(16) 4_546 . . 6_556 ? O1 Cd1 N3 C11 -143.8(16) 4_546 . . 6_556 ? O1 Cd1 N3 C11 36.2(16) 7_454 . . 6_556 ? C3 N1 C1 C2 0.9(12) . . . . ? Cd1 N1 C1 C2 175.2(7) . . . . ? N1 C1 C2 N2 -0.8(12) . . . . ? C3 N2 C2 C1 0.4(12) . . . . ? C4 N2 C2 C1 -179.8(9) . . . . ? C1 N1 C3 N2 -0.6(12) . . . . ? Cd1 N1 C3 N2 -175.4(6) . . . . ? C2 N2 C3 N1 0.2(12) . . . . ? C4 N2 C3 N1 -179.7(9) . . . . ? C3 N2 C4 C9 -40.1(14) . . . . ? C2 N2 C4 C9 140.1(11) . . . . ? C3 N2 C4 C5 137.6(10) . . . . ? C2 N2 C4 C5 -42.2(14) . . . . ? C9 C4 C5 C6 -0.2(15) . . . . ? N2 C4 C5 C6 -177.8(8) . . . . ? C4 C5 C6 C7 0.4(14) . . . . ? C5 C6 C7 C8 -1.4(14) . . . . ? C5 C6 C7 C10 179.1(8) . . . . ? C6 C7 C8 C9 2.4(15) . . . . ? C10 C7 C8 C9 -178.1(9) . . . . ? C5 C4 C9 C8 1.1(15) . . . . ? N2 C4 C9 C8 178.7(9) . . . . ? C7 C8 C9 C4 -2.2(15) . . . . ? Cd1 O2 C10 O1 -4.1(10) 4_556 . . . ? Cd1 O2 C10 C7 175.2(7) 4_556 . . . ? Cd1 O1 C10 O2 4.0(10) 4_556 . . . ? Cd1 O1 C10 C7 -175.4(7) 4_556 . . . ? C6 C7 C10 O2 179.0(9) . . . . ? C8 C7 C10 O2 -0.5(13) . . . . ? C6 C7 C10 O1 -1.6(13) . . . . ? C8 C7 C10 O1 178.9(9) . . . . ? C11 N3 C11 C12 -1(2) 6_556 . . . ? Cd1 N3 C11 C12 179(2) . . . . ? N3 C11 C12 C13 2(4) . . . . ? C11 C12 C13 C12 -0.9(18) . . . 6_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.423 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.225 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 773583' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 N4 O4 Zn' _chemical_formula_sum 'C20 H14 N4 O4 Zn' _chemical_formula_weight 439.74 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 Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 25.391(4) _cell_length_b 19.896(5) _cell_length_c 7.556(4) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 3817(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7968 _exptl_absorpt_correction_T_max 0.8575 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9903 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3471 _reflns_number_gt 2936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _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 -0.018(14) _refine_ls_number_reflns 3471 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.131230(13) 1.438117(16) 0.84296(7) 0.04078(12) Uani 1 1 d . . . O1 O 0.07589(11) 1.40811(14) 0.6871(4) 0.0588(8) Uani 1 1 d . . . O2 O 0.11314(12) 1.30920(16) 0.6416(5) 0.0743(9) Uani 1 1 d . . . O3 O 0.18112(10) 1.49841(11) 0.7282(3) 0.0532(7) Uani 1 1 d . . . O4 O 0.12198(11) 1.57983(13) 0.7118(4) 0.0522(7) Uani 1 1 d . . . N1 N -0.10017(12) 1.51450(15) 0.0521(4) 0.0434(7) Uani 1 1 d . . . N2 N -0.05640(12) 1.43934(14) 0.2065(4) 0.0426(7) Uani 1 1 d . . . N3 N 0.18388(12) 1.87485(14) 0.4486(4) 0.0390(7) Uani 1 1 d . . . N4 N 0.22835(11) 1.78533(13) 0.5321(4) 0.0365(7) Uani 1 1 d . . . C1 C -0.11451(15) 1.5191(2) 0.2278(5) 0.0478(9) Uani 1 1 d . . . H1 H -0.1388 1.5496 0.2734 0.057 Uiso 1 1 calc R . . C2 C -0.08832(14) 1.47332(19) 0.3230(6) 0.0481(9) Uani 1 1 d . . . H2 H -0.0912 1.4659 0.4442 0.058 Uiso 1 1 calc R . . C3 C -0.06539(15) 1.4654(2) 0.0448(5) 0.0486(9) Uani 1 1 d . . . H3 H -0.0492 1.4507 -0.0585 0.058 Uiso 1 1 calc R . . C4 C -0.01857(16) 1.38825(19) 0.2476(5) 0.0476(10) Uani 1 1 d . . . C5 C 0.00974(15) 1.39224(19) 0.4034(5) 0.0434(10) Uani 1 1 d . . . H5 H 0.0029 1.4267 0.4834 0.052 Uiso 1 1 calc R . . C6 C 0.04782(15) 1.34575(18) 0.4404(5) 0.0454(9) Uani 1 1 d . . . C7 C 0.05758(15) 1.29421(19) 0.3231(7) 0.0606(11) Uani 1 1 d . . . H7 H 0.0832 1.2622 0.3490 0.073 Uiso 1 1 calc R . . C8 C 0.0293(2) 1.2899(2) 0.1663(7) 0.0783(15) Uani 1 1 d . . . H8 H 0.0364 1.2558 0.0856 0.094 Uiso 1 1 calc R . . C9 C -0.01001(19) 1.3370(2) 0.1303(7) 0.0717(14) Uani 1 1 d . . . H9 H -0.0301 1.3336 0.0279 0.086 Uiso 1 1 calc R . . C10 C 0.08133(15) 1.3534(2) 0.6025(5) 0.0477(10) Uani 1 1 d . . . C11 C 0.23378(15) 1.89311(17) 0.4997(5) 0.0478(10) Uani 1 1 d . . . H11 H 0.2466 1.9369 0.4983 0.057 Uiso 1 1 calc R . . C12 C 0.26127(15) 1.83954(17) 0.5515(5) 0.0461(10) Uani 1 1 d . . . H12 H 0.2958 1.8390 0.5926 0.055 Uiso 1 1 calc R . . C13 C 0.18230(14) 1.80889(17) 0.4701(5) 0.0401(8) Uani 1 1 d . . . H13 H 0.1531 1.7823 0.4454 0.048 Uiso 1 1 calc R . . C14 C 0.24021(14) 1.71677(15) 0.5767(5) 0.0364(8) Uani 1 1 d . . . C15 C 0.20033(15) 1.67305(17) 0.6157(5) 0.0393(9) Uani 1 1 d . . . H15 H 0.1656 1.6877 0.6132 0.047 Uiso 1 1 calc R . . C16 C 0.21165(14) 1.60647(16) 0.6595(5) 0.0366(8) Uani 1 1 d . . . C17 C 0.26359(15) 1.58659(18) 0.6676(5) 0.0471(9) Uani 1 1 d . . . H17 H 0.2719 1.5426 0.6988 0.057 Uiso 1 1 calc R . . C18 C 0.30322(15) 1.63149(19) 0.6298(6) 0.0512(10) Uani 1 1 d . . . H18 H 0.3381 1.6176 0.6374 0.061 Uiso 1 1 calc R . . C19 C 0.29214(14) 1.6961(2) 0.5813(6) 0.0440(9) Uani 1 1 d . . . H19 H 0.3191 1.7257 0.5519 0.053 Uiso 1 1 calc R . . C20 C 0.16743(16) 1.55943(16) 0.7038(5) 0.0401(8) 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 Zn1 0.0448(2) 0.02976(19) 0.0488(2) 0.0019(2) -0.0013(3) 0.00265(16) O1 0.0639(18) 0.0533(16) 0.0592(19) -0.0067(15) -0.0240(15) 0.0049(14) O2 0.0662(17) 0.075(2) 0.082(2) -0.012(2) -0.0264(18) 0.0215(18) O3 0.0659(18) 0.0298(13) 0.0637(17) 0.0076(13) 0.0154(15) 0.0031(12) O4 0.0532(17) 0.0463(15) 0.0572(18) 0.0107(13) 0.0025(14) 0.0005(13) N1 0.0487(18) 0.0429(17) 0.0386(17) 0.0000(14) -0.0044(15) 0.0000(15) N2 0.0447(18) 0.0426(18) 0.0406(18) 0.0034(14) -0.0089(15) 0.0000(13) N3 0.0441(17) 0.0309(15) 0.0419(17) 0.0062(13) -0.0025(14) -0.0012(13) N4 0.0422(17) 0.0311(14) 0.0363(17) 0.0051(12) -0.0064(14) 0.0004(12) C1 0.047(2) 0.049(2) 0.048(2) -0.0063(19) -0.0020(19) 0.0028(18) C2 0.049(2) 0.060(2) 0.035(2) -0.002(2) -0.007(2) -0.0009(17) C3 0.049(2) 0.055(2) 0.041(2) -0.0011(18) -0.0046(19) 0.0023(19) C4 0.054(2) 0.038(2) 0.051(2) -0.0024(18) -0.011(2) 0.0008(19) C5 0.046(2) 0.039(2) 0.046(2) 0.0012(15) -0.0091(17) -0.0055(17) C6 0.045(2) 0.042(2) 0.049(2) 0.0033(18) -0.0081(19) -0.0087(17) C7 0.061(2) 0.048(2) 0.073(3) -0.009(2) -0.022(3) 0.0066(18) C8 0.093(4) 0.065(3) 0.077(4) -0.027(3) -0.027(3) 0.017(3) C9 0.082(3) 0.064(3) 0.069(3) -0.014(2) -0.028(3) 0.012(2) C10 0.044(2) 0.047(2) 0.052(3) 0.0064(19) -0.0067(19) -0.0009(18) C11 0.058(2) 0.0306(18) 0.055(2) 0.0016(17) -0.012(2) -0.0094(17) C12 0.045(3) 0.0380(18) 0.055(3) 0.0056(18) -0.017(2) -0.0063(16) C13 0.0417(19) 0.0352(19) 0.043(2) 0.0079(16) -0.0037(17) -0.0060(16) C14 0.048(2) 0.0277(15) 0.0340(19) 0.0066(16) -0.0020(18) 0.0030(15) C15 0.042(2) 0.040(2) 0.036(2) 0.0003(17) -0.0069(17) 0.0049(16) C16 0.047(2) 0.0321(17) 0.0304(18) 0.0051(15) -0.0002(17) 0.0026(15) C17 0.061(3) 0.0322(18) 0.049(2) 0.0056(17) 0.001(2) 0.0078(18) C18 0.046(2) 0.046(2) 0.062(3) 0.006(2) 0.002(2) 0.0122(18) C19 0.044(2) 0.043(2) 0.046(2) 0.0090(18) 0.0025(19) -0.0024(19) C20 0.057(2) 0.0314(19) 0.0321(19) 0.0043(14) 0.0008(18) -0.0022(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 Zn1 O1 1.928(3) . ? Zn1 O3 1.948(2) . ? Zn1 N1 2.002(3) 2_586 ? Zn1 N3 2.002(3) 5_545 ? O1 C10 1.269(4) . ? O2 C10 1.230(4) . ? O3 C20 1.276(4) . ? O4 C20 1.225(4) . ? N1 C3 1.318(5) . ? N1 C1 1.380(5) . ? N1 Zn1 2.002(3) 2_584 ? N2 C3 1.347(5) . ? N2 C2 1.374(5) . ? N2 C4 1.433(5) . ? N3 C13 1.323(4) . ? N3 C11 1.373(5) . ? N3 Zn1 2.002(3) 5_554 ? N4 C13 1.344(4) . ? N4 C12 1.372(5) . ? N4 C14 1.437(4) . ? C1 C2 1.338(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C9 1.369(6) . ? C4 C5 1.381(5) . ? C5 C6 1.367(5) . ? C5 H5 0.9300 . ? C6 C7 1.378(6) . ? C6 C10 1.499(5) . ? C7 C8 1.389(7) . ? C7 H7 0.9300 . ? C8 C9 1.395(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.333(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.367(5) . ? C14 C19 1.382(5) . ? C15 C16 1.395(5) . ? C15 H15 0.9300 . ? C16 C17 1.378(5) . ? C16 C20 1.500(5) . ? C17 C18 1.376(5) . ? C17 H17 0.9300 . ? C18 C19 1.366(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 113.11(13) . . ? O1 Zn1 N1 109.94(13) . 2_586 ? O3 Zn1 N1 108.52(11) . 2_586 ? O1 Zn1 N3 122.37(12) . 5_545 ? O3 Zn1 N3 97.50(11) . 5_545 ? N1 Zn1 N3 104.14(13) 2_586 5_545 ? C10 O1 Zn1 119.6(3) . . ? C20 O3 Zn1 118.2(2) . . ? C3 N1 C1 105.5(3) . . ? C3 N1 Zn1 125.4(3) . 2_584 ? C1 N1 Zn1 128.6(3) . 2_584 ? C3 N2 C2 107.0(3) . . ? C3 N2 C4 125.7(3) . . ? C2 N2 C4 127.3(3) . . ? C13 N3 C11 104.8(3) . . ? C13 N3 Zn1 130.7(2) . 5_554 ? C11 N3 Zn1 124.2(2) . 5_554 ? C13 N4 C12 107.0(3) . . ? C13 N4 C14 126.5(3) . . ? C12 N4 C14 126.4(3) . . ? C2 C1 N1 109.9(3) . . ? C2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? C1 C2 N2 106.5(4) . . ? C1 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? N1 C3 N2 111.2(4) . . ? N1 C3 H3 124.4 . . ? N2 C3 H3 124.4 . . ? C9 C4 C5 120.8(4) . . ? C9 C4 N2 119.6(4) . . ? C5 C4 N2 119.5(4) . . ? C6 C5 C4 120.2(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.9(4) . . ? C5 C6 C10 120.0(4) . . ? C7 C6 C10 120.0(4) . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C4 C9 C8 119.2(4) . . ? C4 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? O2 C10 O1 124.3(4) . . ? O2 C10 C6 119.7(4) . . ? O1 C10 C6 115.9(3) . . ? C12 C11 N3 110.7(3) . . ? C12 C11 H11 124.6 . . ? N3 C11 H11 124.6 . . ? C11 C12 N4 106.2(3) . . ? C11 C12 H12 126.9 . . ? N4 C12 H12 126.9 . . ? N3 C13 N4 111.2(3) . . ? N3 C13 H13 124.4 . . ? N4 C13 H13 124.4 . . ? C15 C14 C19 120.8(3) . . ? C15 C14 N4 120.0(3) . . ? C19 C14 N4 119.2(3) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C20 121.8(3) . . ? C15 C16 C20 119.4(3) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C14 118.9(3) . . ? C18 C19 H19 120.5 . . ? C14 C19 H19 120.5 . . ? O4 C20 O3 124.4(3) . . ? O4 C20 C16 120.6(3) . . ? O3 C20 C16 115.0(3) . . ? 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 O3 Zn1 O1 C10 92.8(3) . . . . ? N1 Zn1 O1 C10 -145.7(3) 2_586 . . . ? N3 Zn1 O1 C10 -23.2(4) 5_545 . . . ? O1 Zn1 O3 C20 77.4(3) . . . . ? N1 Zn1 O3 C20 -44.9(3) 2_586 . . . ? N3 Zn1 O3 C20 -152.6(3) 5_545 . . . ? C3 N1 C1 C2 0.1(4) . . . . ? Zn1 N1 C1 C2 172.5(2) 2_584 . . . ? N1 C1 C2 N2 0.6(4) . . . . ? C3 N2 C2 C1 -1.0(4) . . . . ? C4 N2 C2 C1 176.0(3) . . . . ? C1 N1 C3 N2 -0.8(4) . . . . ? Zn1 N1 C3 N2 -173.5(2) 2_584 . . . ? C2 N2 C3 N1 1.2(4) . . . . ? C4 N2 C3 N1 -175.9(3) . . . . ? C3 N2 C4 C9 -37.2(6) . . . . ? C2 N2 C4 C9 146.3(4) . . . . ? C3 N2 C4 C5 141.3(4) . . . . ? C2 N2 C4 C5 -35.2(5) . . . . ? C9 C4 C5 C6 1.7(6) . . . . ? N2 C4 C5 C6 -176.7(4) . . . . ? C4 C5 C6 C7 -0.8(6) . . . . ? C4 C5 C6 C10 175.1(3) . . . . ? C5 C6 C7 C8 0.8(6) . . . . ? C10 C6 C7 C8 -175.1(4) . . . . ? C6 C7 C8 C9 -1.6(8) . . . . ? C5 C4 C9 C8 -2.5(7) . . . . ? N2 C4 C9 C8 175.9(4) . . . . ? C7 C8 C9 C4 2.5(8) . . . . ? Zn1 O1 C10 O2 18.4(6) . . . . ? Zn1 O1 C10 C6 -158.6(2) . . . . ? C5 C6 C10 O2 175.2(4) . . . . ? C7 C6 C10 O2 -8.9(6) . . . . ? C5 C6 C10 O1 -7.7(5) . . . . ? C7 C6 C10 O1 168.3(4) . . . . ? C13 N3 C11 C12 -0.4(4) . . . . ? Zn1 N3 C11 C12 -174.9(3) 5_554 . . . ? N3 C11 C12 N4 0.4(5) . . . . ? C13 N4 C12 C11 -0.3(4) . . . . ? C14 N4 C12 C11 -178.0(3) . . . . ? C11 N3 C13 N4 0.2(4) . . . . ? Zn1 N3 C13 N4 174.1(2) 5_554 . . . ? C12 N4 C13 N3 0.0(4) . . . . ? C14 N4 C13 N3 177.7(3) . . . . ? C13 N4 C14 C15 -22.3(5) . . . . ? C12 N4 C14 C15 154.9(4) . . . . ? C13 N4 C14 C19 158.4(4) . . . . ? C12 N4 C14 C19 -24.3(5) . . . . ? C19 C14 C15 C16 -0.6(6) . . . . ? N4 C14 C15 C16 -179.8(3) . . . . ? C14 C15 C16 C17 2.0(5) . . . . ? C14 C15 C16 C20 179.3(3) . . . . ? C15 C16 C17 C18 -1.3(6) . . . . ? C20 C16 C17 C18 -178.5(4) . . . . ? C16 C17 C18 C19 -0.9(6) . . . . ? C17 C18 C19 C14 2.3(6) . . . . ? C15 C14 C19 C18 -1.5(6) . . . . ? N4 C14 C19 C18 177.7(4) . . . . ? Zn1 O3 C20 O4 -16.4(5) . . . . ? Zn1 O3 C20 C16 164.8(2) . . . . ? C17 C16 C20 O4 173.1(4) . . . . ? C15 C16 C20 O4 -4.2(5) . . . . ? C17 C16 C20 O3 -8.1(5) . . . . ? C15 C16 C20 O3 174.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.423 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.049 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 773584' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Cd2 N8 O9' _chemical_formula_sum 'C40 H30 Cd2 N8 O9' _chemical_formula_weight 991.54 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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.370(5) _cell_length_b 10.292(3) _cell_length_c 20.590(4) _cell_angle_alpha 90.000 _cell_angle_beta 114.102(5) _cell_angle_gamma 90.000 _cell_volume 3746.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7774 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19427 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6968 _reflns_number_gt 6166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One restraint applied is: DFIX option to fix the O-H distance in water. ; _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^)+(0.0515P)^2^+0.4036P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6968 _refine_ls_number_parameters 540 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Cd1 Cd 1.011683(13) 0.08488(2) 0.807847(11) 0.01522(9) Uani 1 1 d . . . Cd2 Cd 0.550530(13) 0.53568(2) 0.830330(12) 0.01764(9) Uani 1 1 d . . . O1 O 1.44501(13) 0.4037(2) 0.81902(12) 0.0215(5) Uani 1 1 d . . . O2 O 1.42896(13) 0.5744(2) 0.74919(12) 0.0214(5) Uani 1 1 d . . . O3 O 1.05384(13) 0.8606(2) 0.83785(12) 0.0239(5) Uani 1 1 d . . . O4 O 1.00851(13) 0.9744(2) 0.90297(12) 0.0197(5) Uani 1 1 d . . . O5 O 0.89702(12) 0.0233(2) 0.71454(11) 0.0174(5) Uani 1 1 d . . . O6 O 0.89725(12) 0.1978(2) 0.77746(11) 0.0175(5) Uani 1 1 d . . . O7 O 0.59856(14) -0.2591(2) 0.85461(12) 0.0277(6) Uani 1 1 d . . . O8 O 0.58062(13) -0.3512(2) 0.94326(12) 0.0236(5) Uani 1 1 d . . . N1 N 1.08952(15) 0.1059(3) 0.75161(13) 0.0160(6) Uani 1 1 d . . . N2 N 1.17566(14) 0.2071(2) 0.72625(13) 0.0152(5) Uani 1 1 d . . . N3 N 1.07756(15) 0.2351(3) 0.89324(14) 0.0178(6) Uani 1 1 d . . . N4 N 1.09726(15) 0.4134(2) 0.95782(14) 0.0162(6) Uani 1 1 d . . . N5 N 0.58783(15) 0.4817(3) 0.74179(14) 0.0212(6) Uani 1 1 d . . . N6 N 0.62702(15) 0.3596(3) 0.67523(14) 0.0195(6) Uani 1 1 d . . . N7 N 0.63286(15) 0.3821(3) 0.89887(14) 0.0190(6) Uani 1 1 d . . . N8 N 0.68191(14) 0.2006(3) 0.95523(13) 0.0170(6) Uani 1 1 d . . . C1 C 1.13531(18) 0.0147(3) 0.73982(16) 0.0164(7) Uani 1 1 d . . . H1 H 1.1304 -0.0748 0.7422 0.020 Uiso 1 1 calc R . . C2 C 1.18869(19) 0.0764(3) 0.72419(17) 0.0181(7) Uani 1 1 d . . . H2 H 1.2266 0.0376 0.7141 0.022 Uiso 1 1 calc R . . C3 C 1.11560(18) 0.2202(3) 0.74279(16) 0.0184(7) Uani 1 1 d . . . H3 H 1.0951 0.2995 0.7474 0.022 Uiso 1 1 calc R . . C4 C 1.21219(18) 0.3147(3) 0.70812(16) 0.0162(7) Uani 1 1 d . . . C5 C 1.28908(18) 0.3368(3) 0.74640(16) 0.0171(7) Uani 1 1 d . . . H5 H 1.3182 0.2807 0.7827 0.021 Uiso 1 1 calc R . . C6 C 1.32150(18) 0.4450(3) 0.72912(17) 0.0165(7) Uani 1 1 d . . . C7 C 1.27609(19) 0.5277(3) 0.67469(17) 0.0191(7) Uani 1 1 d . . . H7 H 1.2975 0.6004 0.6634 0.023 Uiso 1 1 calc R . . C8 C 1.20031(19) 0.5032(3) 0.63764(17) 0.0212(7) Uani 1 1 d . . . H8 H 1.1708 0.5595 0.6016 0.025 Uiso 1 1 calc R . . C9 C 1.16770(19) 0.3954(3) 0.65360(17) 0.0193(7) Uani 1 1 d . . . H9 H 1.1166 0.3775 0.6280 0.023 Uiso 1 1 calc R . . C10 C 1.40357(18) 0.4756(3) 0.76851(17) 0.0179(7) Uani 1 1 d . . . C11 C 1.12335(19) 0.2051(3) 0.96336(17) 0.0201(7) Uani 1 1 d . . . H11 H 1.1429 0.1233 0.9802 0.024 Uiso 1 1 calc R . . C12 C 1.13517(18) 0.3144(3) 1.00349(17) 0.0199(7) Uani 1 1 d . . . H12 H 1.1634 0.3210 1.0523 0.024 Uiso 1 1 calc R . . C13 C 1.06350(17) 0.3597(3) 0.89237(16) 0.0158(7) Uani 1 1 d . . . H13 H 1.0338 0.4057 0.8516 0.019 Uiso 1 1 calc R . . C14 C 1.08608(17) 0.5426(3) 0.97610(16) 0.0146(6) Uani 1 1 d . . . C15 C 1.07028(16) 0.6406(3) 0.92647(15) 0.0140(6) Uani 1 1 d . . . H15 H 1.0709 0.6243 0.8823 0.017 Uiso 1 1 calc R . . C16 C 1.05337(17) 0.7643(3) 0.94318(16) 0.0162(7) Uani 1 1 d . . . C17 C 1.05434(17) 0.7883(3) 1.01056(16) 0.0165(7) Uani 1 1 d . . . H17 H 1.0413 0.8701 1.0212 0.020 Uiso 1 1 calc R . . C18 C 1.07451(17) 0.6911(3) 1.06115(16) 0.0178(7) Uani 1 1 d . . . H18 H 1.0780 0.7091 1.1067 0.021 Uiso 1 1 calc R . . C19 C 1.08955(18) 0.5671(3) 1.04446(17) 0.0180(7) Uani 1 1 d . . . H19 H 1.1018 0.5009 1.0780 0.022 Uiso 1 1 calc R . . C20 C 1.03774(17) 0.8726(3) 0.89072(16) 0.0173(7) Uani 1 1 d . . . C21 C 0.5981(2) 0.4734(4) 0.63775(19) 0.0289(8) Uani 1 1 d . . . H21 H 0.5953 0.4949 0.5929 0.035 Uiso 1 1 calc R . . C22 C 0.5750(2) 0.5465(3) 0.67942(19) 0.0258(8) Uani 1 1 d . . . H22 H 0.5535 0.6286 0.6677 0.031 Uiso 1 1 calc R . . C23 C 0.61911(19) 0.3705(3) 0.73736(17) 0.0207(7) Uani 1 1 d . . . H23 H 0.6340 0.3071 0.7726 0.025 Uiso 1 1 calc R . . C24 C 0.66555(18) 0.2567(3) 0.65690(16) 0.0190(7) Uani 1 1 d . . . C25 C 0.74107(18) 0.2346(3) 0.70040(16) 0.0171(7) Uani 1 1 d . . . H25 H 0.7651 0.2847 0.7411 0.021 Uiso 1 1 calc R . . C26 C 0.78092(18) 0.1377(3) 0.68331(16) 0.0176(7) Uani 1 1 d . . . C27 C 0.74281(19) 0.0629(3) 0.62227(17) 0.0195(7) Uani 1 1 d . . . H27 H 0.7687 -0.0021 0.6101 0.023 Uiso 1 1 calc R . . C28 C 0.6672(2) 0.0842(3) 0.57972(18) 0.0252(8) Uani 1 1 d . . . H28 H 0.6426 0.0329 0.5397 0.030 Uiso 1 1 calc R . . C29 C 0.6277(2) 0.1821(3) 0.59650(17) 0.0232(7) Uani 1 1 d . . . H29 H 0.5770 0.1973 0.5678 0.028 Uiso 1 1 calc R . . C30 C 0.86319(18) 0.1190(3) 0.72806(16) 0.0155(7) Uani 1 1 d . . . C31 C 0.71025(19) 0.3906(3) 0.92608(18) 0.0228(7) Uani 1 1 d . . . H31 H 0.7372 0.4618 0.9210 0.027 Uiso 1 1 calc R . . C32 C 0.74167(18) 0.2796(3) 0.96143(17) 0.0205(7) Uani 1 1 d . . . H32 H 0.7929 0.2608 0.9850 0.025 Uiso 1 1 calc R . . C33 C 0.61779(18) 0.2658(3) 0.91715(17) 0.0203(7) Uani 1 1 d . . . H33 H 0.5693 0.2333 0.9053 0.024 Uiso 1 1 calc R . . C34 C 0.68674(18) 0.0718(3) 0.98333(17) 0.0178(7) Uani 1 1 d . . . C35 C 0.64385(18) -0.0267(3) 0.93877(17) 0.0181(7) Uani 1 1 d . . . H35 H 0.6130 -0.0093 0.8914 0.022 Uiso 1 1 calc R . . C36 C 0.64775(18) -0.1509(3) 0.96590(16) 0.0179(7) Uani 1 1 d . . . C37 C 0.69492(18) -0.1759(3) 1.03673(17) 0.0197(7) Uani 1 1 d . . . H37 H 0.6966 -0.2588 1.0552 0.024 Uiso 1 1 calc R . . C38 C 0.7395(2) -0.0779(3) 1.07991(18) 0.0231(8) Uani 1 1 d . . . H38 H 0.7720 -0.0959 1.1268 0.028 Uiso 1 1 calc R . . C39 C 0.73564(19) 0.0468(3) 1.05330(17) 0.0193(7) Uani 1 1 d . . . H39 H 0.7654 0.1128 1.0819 0.023 Uiso 1 1 calc R . . C40 C 0.60558(18) -0.2604(3) 0.91802(16) 0.0185(7) Uani 1 1 d . . . OW1 O 0.46236(16) 0.2722(3) 0.94455(15) 0.0316(6) Uani 1 1 d D . . H1W1 H 0.445(2) 0.296(4) 0.968(2) 0.036(13) Uiso 1 1 d . . . H2W1 H 0.449(3) 0.321(4) 0.9099(18) 0.063(16) 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 Cd1 0.01635(14) 0.01207(15) 0.01793(14) -0.00060(9) 0.00769(11) -0.00078(9) Cd2 0.01526(14) 0.01430(15) 0.02181(14) -0.00166(9) 0.00601(11) -0.00104(9) O1 0.0171(12) 0.0244(13) 0.0202(12) 0.0021(10) 0.0047(10) -0.0027(10) O2 0.0182(13) 0.0140(12) 0.0301(13) 0.0005(10) 0.0080(11) -0.0035(9) O3 0.0358(15) 0.0175(13) 0.0254(12) 0.0036(10) 0.0195(12) 0.0030(10) O4 0.0217(12) 0.0133(12) 0.0265(12) 0.0024(9) 0.0120(11) 0.0026(9) O5 0.0182(12) 0.0148(12) 0.0202(11) -0.0004(9) 0.0089(10) 0.0010(9) O6 0.0182(12) 0.0154(12) 0.0187(11) -0.0013(9) 0.0073(10) 0.0015(9) O7 0.0407(15) 0.0221(13) 0.0225(12) -0.0053(10) 0.0151(12) -0.0126(11) O8 0.0325(14) 0.0148(12) 0.0254(12) 0.0000(10) 0.0139(11) -0.0049(10) N1 0.0147(14) 0.0147(14) 0.0170(13) 0.0014(11) 0.0050(11) -0.0016(11) N2 0.0125(13) 0.0151(14) 0.0188(13) -0.0006(11) 0.0070(11) -0.0010(11) N3 0.0194(14) 0.0134(14) 0.0220(14) -0.0008(11) 0.0098(12) -0.0009(11) N4 0.0194(15) 0.0135(14) 0.0170(13) 0.0002(11) 0.0086(12) -0.0011(11) N5 0.0179(15) 0.0196(15) 0.0256(15) 0.0019(12) 0.0085(13) 0.0028(12) N6 0.0156(14) 0.0189(15) 0.0232(14) 0.0032(12) 0.0073(12) 0.0058(11) N7 0.0169(14) 0.0174(15) 0.0206(14) -0.0022(12) 0.0057(12) 0.0003(11) N8 0.0147(14) 0.0160(14) 0.0189(13) -0.0020(11) 0.0055(11) -0.0006(11) C1 0.0182(17) 0.0119(16) 0.0164(15) -0.0029(13) 0.0044(14) 0.0002(13) C2 0.0172(17) 0.0169(17) 0.0205(17) -0.0028(13) 0.0080(14) 0.0029(13) C3 0.0190(17) 0.0158(17) 0.0230(16) 0.0014(13) 0.0111(14) 0.0006(13) C4 0.0171(16) 0.0153(16) 0.0175(15) -0.0039(13) 0.0086(14) -0.0008(13) C5 0.0167(16) 0.0166(17) 0.0185(15) -0.0005(13) 0.0077(14) 0.0011(13) C6 0.0172(17) 0.0147(16) 0.0201(16) -0.0018(13) 0.0103(14) 0.0027(13) C7 0.0212(18) 0.0153(18) 0.0262(17) -0.0011(14) 0.0151(15) -0.0014(13) C8 0.0203(18) 0.0210(18) 0.0213(17) 0.0069(14) 0.0074(15) 0.0075(14) C9 0.0162(17) 0.0216(18) 0.0220(17) -0.0005(14) 0.0096(14) 0.0000(13) C10 0.0166(17) 0.0207(18) 0.0183(16) -0.0034(14) 0.0091(14) -0.0005(13) C11 0.0223(18) 0.0122(16) 0.0236(17) 0.0006(13) 0.0071(15) 0.0032(13) C12 0.0181(17) 0.0205(18) 0.0177(16) 0.0004(14) 0.0037(14) 0.0004(14) C13 0.0170(16) 0.0152(17) 0.0160(15) 0.0010(13) 0.0075(14) -0.0015(13) C14 0.0109(15) 0.0134(16) 0.0183(16) 0.0000(13) 0.0047(13) -0.0005(12) C15 0.0115(15) 0.0157(16) 0.0129(14) -0.0022(12) 0.0031(13) -0.0033(12) C16 0.0083(15) 0.0180(17) 0.0196(16) 0.0040(13) 0.0029(13) -0.0005(12) C17 0.0104(15) 0.0178(17) 0.0205(16) -0.0034(13) 0.0055(13) -0.0025(12) C18 0.0168(16) 0.0201(17) 0.0176(16) -0.0036(13) 0.0083(14) -0.0027(13) C19 0.0184(17) 0.0190(17) 0.0164(16) 0.0025(13) 0.0069(14) -0.0010(13) C20 0.0106(15) 0.0184(17) 0.0183(16) 0.0016(13) 0.0012(13) -0.0045(13) C21 0.027(2) 0.032(2) 0.0295(19) 0.0136(16) 0.0136(17) 0.0101(16) C22 0.0223(19) 0.0219(19) 0.035(2) 0.0080(16) 0.0133(17) 0.0044(15) C23 0.0231(18) 0.0196(18) 0.0215(16) 0.0000(14) 0.0112(15) 0.0010(14) C24 0.0199(17) 0.0206(18) 0.0185(16) 0.0040(13) 0.0097(14) 0.0018(14) C25 0.0220(17) 0.0150(16) 0.0170(15) -0.0012(13) 0.0107(14) -0.0024(13) C26 0.0207(17) 0.0159(17) 0.0193(16) 0.0037(13) 0.0113(14) -0.0007(14) C27 0.0243(18) 0.0158(17) 0.0213(17) -0.0009(13) 0.0122(15) -0.0008(14) C28 0.027(2) 0.026(2) 0.0219(18) -0.0068(15) 0.0087(16) -0.0061(15) C29 0.0189(17) 0.027(2) 0.0223(17) 0.0035(15) 0.0065(15) -0.0001(14) C30 0.0216(17) 0.0121(16) 0.0168(15) 0.0037(13) 0.0119(14) -0.0003(13) C31 0.0167(17) 0.0199(18) 0.0285(18) -0.0027(15) 0.0060(15) -0.0044(14) C32 0.0120(16) 0.0203(18) 0.0275(17) -0.0041(14) 0.0064(14) -0.0017(13) C33 0.0142(16) 0.0206(18) 0.0227(17) -0.0014(14) 0.0042(14) -0.0009(14) C34 0.0144(16) 0.0195(17) 0.0211(16) -0.0020(13) 0.0090(14) 0.0006(13) C35 0.0181(17) 0.0192(18) 0.0166(16) -0.0022(13) 0.0068(14) -0.0022(13) C36 0.0164(16) 0.0176(17) 0.0206(16) -0.0021(13) 0.0085(14) -0.0007(13) C37 0.0201(17) 0.0175(17) 0.0215(16) 0.0004(14) 0.0085(14) 0.0001(14) C38 0.0217(19) 0.027(2) 0.0175(17) 0.0008(14) 0.0050(15) 0.0017(15) C39 0.0188(17) 0.0194(18) 0.0173(16) -0.0056(13) 0.0050(14) -0.0020(13) C40 0.0155(16) 0.0207(18) 0.0176(16) -0.0018(13) 0.0051(14) 0.0019(13) OW1 0.0340(16) 0.0365(17) 0.0287(15) 0.0071(13) 0.0172(14) 0.0083(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.255(3) . ? Cd1 O4 2.287(2) 1_545 ? Cd1 N3 2.297(3) . ? Cd1 O6 2.350(2) . ? Cd1 O5 2.354(2) . ? Cd1 O3 2.442(3) 1_545 ? Cd1 C20 2.690(3) 1_545 ? Cd1 C30 2.690(3) . ? Cd2 N7 2.279(3) . ? Cd2 O7 2.280(3) 1_565 ? Cd2 N5 2.287(3) . ? Cd2 O2 2.298(2) 1_455 ? Cd2 O1 2.385(2) 1_455 ? Cd2 O8 2.449(2) 1_565 ? Cd2 C10 2.673(3) 1_455 ? Cd2 C40 2.689(3) 1_565 ? O1 C10 1.261(4) . ? O1 Cd2 2.385(2) 1_655 ? O2 C10 1.263(4) . ? O2 Cd2 2.298(2) 1_655 ? O3 C20 1.255(4) . ? O3 Cd1 2.442(3) 1_565 ? O4 C20 1.264(4) . ? O4 Cd1 2.287(2) 1_565 ? O5 C30 1.275(4) . ? O6 C30 1.257(4) . ? O7 C40 1.256(4) . ? O7 Cd2 2.280(3) 1_545 ? O8 C40 1.258(4) . ? O8 Cd2 2.449(2) 1_545 ? N1 C3 1.321(4) . ? N1 C1 1.379(4) . ? N2 C3 1.346(4) . ? N2 C2 1.372(4) . ? N2 C4 1.443(4) . ? N3 C13 1.310(4) . ? N3 C11 1.386(4) . ? N4 C13 1.352(4) . ? N4 C12 1.378(4) . ? N4 C14 1.423(4) . ? N5 C23 1.315(4) . ? N5 C22 1.376(4) . ? N6 C23 1.354(4) . ? N6 C21 1.389(4) . ? N6 C24 1.432(4) . ? N7 C33 1.323(4) . ? N7 C31 1.372(4) . ? N8 C33 1.346(4) . ? N8 C32 1.377(4) . ? N8 C34 1.434(4) . ? C1 C2 1.359(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C9 1.380(4) . ? C4 C5 1.390(4) . ? C5 C6 1.394(4) . ? C5 H5 0.9300 . ? C6 C7 1.396(5) . ? C6 C10 1.494(5) . ? C7 C8 1.373(5) . ? C7 H7 0.9300 . ? C8 C9 1.381(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 Cd2 2.673(3) 1_655 ? C11 C12 1.358(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 C19 1.404(4) . ? C15 C16 1.392(4) . ? C15 H15 0.9300 . ? C16 C17 1.402(4) . ? C16 C20 1.495(4) . ? C17 C18 1.381(4) . ? C17 H17 0.9300 . ? C18 C19 1.384(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 Cd1 2.690(3) 1_565 ? C21 C22 1.348(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.387(5) . ? C24 C29 1.389(5) . ? C25 C26 1.392(4) . ? C25 H25 0.9300 . ? C26 C27 1.400(5) . ? C26 C30 1.492(5) . ? C27 C28 1.384(5) . ? C27 H27 0.9300 . ? C28 C29 1.390(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 C32 1.358(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.387(5) . ? C34 C35 1.392(5) . ? C35 C36 1.384(4) . ? C35 H35 0.9300 . ? C36 C37 1.393(4) . ? C36 C40 1.501(4) . ? C37 C38 1.388(5) . ? C37 H37 0.9300 . ? C38 C39 1.385(5) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 Cd2 2.689(3) 1_545 ? OW1 H1W1 0.74(4) . ? OW1 H2W1 0.82(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 N1 Cd1 O4 138.13(9) . 1_545 ? N1 Cd1 N3 92.84(9) . . ? O4 Cd1 N3 83.10(9) 1_545 . ? N1 Cd1 O6 124.85(8) . . ? O4 Cd1 O6 96.99(8) 1_545 . ? N3 Cd1 O6 92.28(9) . . ? N1 Cd1 O5 102.28(8) . . ? O4 Cd1 O5 102.63(8) 1_545 . ? N3 Cd1 O5 148.20(8) . . ? O6 Cd1 O5 56.13(8) . . ? N1 Cd1 O3 89.77(8) . 1_545 ? O4 Cd1 O3 55.71(7) 1_545 1_545 ? N3 Cd1 O3 114.74(9) . 1_545 ? O6 Cd1 O3 135.75(8) . 1_545 ? O5 Cd1 O3 93.36(8) . 1_545 ? N1 Cd1 C20 114.33(10) . 1_545 ? O4 Cd1 C20 27.96(9) 1_545 1_545 ? N3 Cd1 C20 99.16(10) . 1_545 ? O6 Cd1 C20 118.87(8) . 1_545 ? O5 Cd1 C20 99.74(9) . 1_545 ? O3 Cd1 C20 27.77(8) 1_545 1_545 ? N1 Cd1 C30 116.50(9) . . ? O4 Cd1 C30 101.07(8) 1_545 . ? N3 Cd1 C30 120.06(9) . . ? O6 Cd1 C30 27.85(8) . . ? O5 Cd1 C30 28.29(8) . . ? O3 Cd1 C30 116.20(9) 1_545 . ? C20 Cd1 C30 111.73(9) 1_545 . ? N7 Cd2 O7 112.76(10) . 1_565 ? N7 Cd2 N5 87.49(10) . . ? O7 Cd2 N5 99.58(9) 1_565 . ? N7 Cd2 O2 145.15(9) . 1_455 ? O7 Cd2 O2 101.76(9) 1_565 1_455 ? N5 Cd2 O2 91.49(9) . 1_455 ? N7 Cd2 O1 91.18(9) . 1_455 ? O7 Cd2 O1 143.69(8) 1_565 1_455 ? N5 Cd2 O1 108.72(9) . 1_455 ? O2 Cd2 O1 56.30(8) 1_455 1_455 ? N7 Cd2 O8 84.64(9) . 1_565 ? O7 Cd2 O8 55.49(8) 1_565 1_565 ? N5 Cd2 O8 147.39(9) . 1_565 ? O2 Cd2 O8 112.56(8) 1_455 1_565 ? O1 Cd2 O8 103.05(8) 1_455 1_565 ? N7 Cd2 C10 118.31(10) . 1_455 ? O7 Cd2 C10 125.36(10) 1_565 1_455 ? N5 Cd2 C10 100.71(10) . 1_455 ? O2 Cd2 C10 28.16(9) 1_455 1_455 ? O1 Cd2 C10 28.15(9) 1_455 1_455 ? O8 Cd2 C10 110.88(9) 1_565 1_455 ? N7 Cd2 C40 98.06(10) . 1_565 ? O7 Cd2 C40 27.75(9) 1_565 1_565 ? N5 Cd2 C40 123.86(10) . 1_565 ? O2 Cd2 C40 111.12(9) 1_455 1_565 ? O1 Cd2 C40 126.82(9) 1_455 1_565 ? O8 Cd2 C40 27.85(8) 1_565 1_565 ? C10 Cd2 C40 123.61(10) 1_455 1_565 ? C10 O1 Cd2 88.73(19) . 1_655 ? C10 O2 Cd2 92.7(2) . 1_655 ? C20 O3 Cd1 87.16(19) . 1_565 ? C20 O4 Cd1 94.03(18) . 1_565 ? C30 O5 Cd1 90.67(19) . . ? C30 O6 Cd1 91.29(18) . . ? C40 O7 Cd2 94.6(2) . 1_545 ? C40 O8 Cd2 86.77(18) . 1_545 ? C3 N1 C1 105.8(3) . . ? C3 N1 Cd1 122.0(2) . . ? C1 N1 Cd1 129.6(2) . . ? C3 N2 C2 107.1(3) . . ? C3 N2 C4 123.7(3) . . ? C2 N2 C4 128.9(3) . . ? C13 N3 C11 105.8(3) . . ? C13 N3 Cd1 126.9(2) . . ? C11 N3 Cd1 124.5(2) . . ? C13 N4 C12 106.5(3) . . ? C13 N4 C14 125.6(3) . . ? C12 N4 C14 127.4(3) . . ? C23 N5 C22 105.7(3) . . ? C23 N5 Cd2 124.8(2) . . ? C22 N5 Cd2 129.1(2) . . ? C23 N6 C21 106.2(3) . . ? C23 N6 C24 125.6(3) . . ? C21 N6 C24 127.8(3) . . ? C33 N7 C31 105.8(3) . . ? C33 N7 Cd2 128.6(2) . . ? C31 N7 Cd2 125.5(2) . . ? C33 N8 C32 107.5(3) . . ? C33 N8 C34 126.1(3) . . ? C32 N8 C34 126.5(3) . . ? C2 C1 N1 109.3(3) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? C1 C2 N2 106.4(3) . . ? C1 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? N1 C3 N2 111.4(3) . . ? N1 C3 H3 124.3 . . ? N2 C3 H3 124.3 . . ? C9 C4 C5 122.1(3) . . ? C9 C4 N2 117.6(3) . . ? C5 C4 N2 120.3(3) . . ? C4 C5 C6 118.4(3) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C5 C6 C7 119.3(3) . . ? C5 C6 C10 121.3(3) . . ? C7 C6 C10 119.3(3) . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C4 C9 C8 118.9(3) . . ? C4 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? O1 C10 O2 122.3(3) . . ? O1 C10 C6 120.1(3) . . ? O2 C10 C6 117.6(3) . . ? O1 C10 Cd2 63.12(17) . 1_655 ? O2 C10 Cd2 59.18(17) . 1_655 ? C6 C10 Cd2 176.0(2) . 1_655 ? C12 C11 N3 109.1(3) . . ? C12 C11 H11 125.5 . . ? N3 C11 H11 125.5 . . ? C11 C12 N4 106.7(3) . . ? C11 C12 H12 126.7 . . ? N4 C12 H12 126.7 . . ? N3 C13 N4 111.9(3) . . ? N3 C13 H13 124.0 . . ? N4 C13 H13 124.0 . . ? C15 C14 C19 121.1(3) . . ? C15 C14 N4 120.0(3) . . ? C19 C14 N4 118.9(3) . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 C20 120.1(3) . . ? C17 C16 C20 120.0(3) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 119.1(3) . . ? C18 C19 H19 120.5 . . ? C14 C19 H19 120.5 . . ? O3 C20 O4 123.0(3) . . ? O3 C20 C16 120.3(3) . . ? O4 C20 C16 116.7(3) . . ? O3 C20 Cd1 65.07(17) . 1_565 ? O4 C20 Cd1 58.02(16) . 1_565 ? C16 C20 Cd1 173.9(2) . 1_565 ? C22 C21 N6 106.3(3) . . ? C22 C21 H21 126.9 . . ? N6 C21 H21 126.9 . . ? C21 C22 N5 110.1(3) . . ? C21 C22 H22 125.0 . . ? N5 C22 H22 125.0 . . ? N5 C23 N6 111.8(3) . . ? N5 C23 H23 124.1 . . ? N6 C23 H23 124.1 . . ? C25 C24 C29 121.3(3) . . ? C25 C24 N6 118.5(3) . . ? C29 C24 N6 120.2(3) . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 118.5(3) . . ? C25 C26 C30 119.9(3) . . ? C27 C26 C30 121.5(3) . . ? C28 C27 C26 121.0(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.3(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C24 C29 C28 118.7(3) . . ? C24 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? O6 C30 O5 121.9(3) . . ? O6 C30 C26 119.4(3) . . ? O5 C30 C26 118.6(3) . . ? O6 C30 Cd1 60.86(16) . . ? O5 C30 Cd1 61.04(16) . . ? C26 C30 Cd1 179.6(2) . . ? C32 C31 N7 110.0(3) . . ? C32 C31 H31 125.0 . . ? N7 C31 H31 125.0 . . ? C31 C32 N8 105.7(3) . . ? C31 C32 H32 127.1 . . ? N8 C32 H32 127.1 . . ? N7 C33 N8 111.0(3) . . ? N7 C33 H33 124.5 . . ? N8 C33 H33 124.5 . . ? C39 C34 C35 121.3(3) . . ? C39 C34 N8 119.7(3) . . ? C35 C34 N8 119.0(3) . . ? C36 C35 C34 119.1(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 119.8(3) . . ? C35 C36 C40 120.2(3) . . ? C37 C36 C40 119.8(3) . . ? C38 C37 C36 120.5(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 119.1(3) . . ? C38 C39 H39 120.4 . . ? C34 C39 H39 120.4 . . ? O7 C40 O8 122.7(3) . . ? O7 C40 C36 118.3(3) . . ? O8 C40 C36 119.0(3) . . ? O7 C40 Cd2 57.67(17) . 1_545 ? O8 C40 Cd2 65.39(17) . 1_545 ? C36 C40 Cd2 171.0(2) . 1_545 ? H1W1 OW1 H2W1 108(5) . . ? 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 N1 Cd1 O5 C30 -124.00(17) . . . . ? O4 Cd1 O5 C30 89.92(17) 1_545 . . . ? N3 Cd1 O5 C30 -7.4(2) . . . . ? O6 Cd1 O5 C30 -0.07(16) . . . . ? O3 Cd1 O5 C30 145.50(17) 1_545 . . . ? C20 Cd1 O5 C30 118.28(17) 1_545 . . . ? N1 Cd1 O6 C30 81.14(19) . . . . ? O4 Cd1 O6 C30 -100.49(17) 1_545 . . . ? N3 Cd1 O6 C30 176.19(17) . . . . ? O5 Cd1 O6 C30 0.07(16) . . . . ? O3 Cd1 O6 C30 -53.9(2) 1_545 . . . ? C20 Cd1 O6 C30 -82.04(18) 1_545 . . . ? O4 Cd1 N1 C3 -123.4(2) 1_545 . . . ? N3 Cd1 N1 C3 -40.5(3) . . . . ? O6 Cd1 N1 C3 54.2(3) . . . . ? O5 Cd1 N1 C3 111.3(2) . . . . ? O3 Cd1 N1 C3 -155.3(2) 1_545 . . . ? C20 Cd1 N1 C3 -141.9(2) 1_545 . . . ? C30 Cd1 N1 C3 85.3(3) . . . . ? O4 Cd1 N1 C1 35.5(3) 1_545 . . . ? N3 Cd1 N1 C1 118.3(3) . . . . ? O6 Cd1 N1 C1 -146.9(2) . . . . ? O5 Cd1 N1 C1 -89.8(3) . . . . ? O3 Cd1 N1 C1 3.6(3) 1_545 . . . ? C20 Cd1 N1 C1 16.9(3) 1_545 . . . ? C30 Cd1 N1 C1 -115.9(3) . . . . ? N1 Cd1 N3 C13 93.5(3) . . . . ? O4 Cd1 N3 C13 -128.4(3) 1_545 . . . ? O6 Cd1 N3 C13 -31.6(3) . . . . ? O5 Cd1 N3 C13 -25.5(3) . . . . ? O3 Cd1 N3 C13 -175.5(2) 1_545 . . . ? C20 Cd1 N3 C13 -151.3(2) 1_545 . . . ? C30 Cd1 N3 C13 -29.6(3) . . . . ? N1 Cd1 N3 C11 -107.7(2) . . . . ? O4 Cd1 N3 C11 30.4(2) 1_545 . . . ? O6 Cd1 N3 C11 127.2(2) . . . . ? O5 Cd1 N3 C11 133.3(2) . . . . ? O3 Cd1 N3 C11 -16.7(3) 1_545 . . . ? C20 Cd1 N3 C11 7.5(2) 1_545 . . . ? C30 Cd1 N3 C11 129.3(2) . . . . ? N7 Cd2 N5 C23 21.9(3) . . . . ? O7 Cd2 N5 C23 134.6(3) 1_565 . . . ? O2 Cd2 N5 C23 -123.2(3) 1_455 . . . ? O1 Cd2 N5 C23 -68.5(3) 1_455 . . . ? O8 Cd2 N5 C23 97.9(3) 1_565 . . . ? C10 Cd2 N5 C23 -96.4(3) 1_455 . . . ? C40 Cd2 N5 C23 119.9(3) 1_565 . . . ? N7 Cd2 N5 C22 -166.9(3) . . . . ? O7 Cd2 N5 C22 -54.3(3) 1_565 . . . ? O2 Cd2 N5 C22 47.9(3) 1_455 . . . ? O1 Cd2 N5 C22 102.7(3) 1_455 . . . ? O8 Cd2 N5 C22 -90.9(3) 1_565 . . . ? C10 Cd2 N5 C22 74.7(3) 1_455 . . . ? C40 Cd2 N5 C22 -68.9(3) 1_565 . . . ? O7 Cd2 N7 C33 154.9(3) 1_565 . . . ? N5 Cd2 N7 C33 -105.8(3) . . . . ? O2 Cd2 N7 C33 -16.8(4) 1_455 . . . ? O1 Cd2 N7 C33 2.9(3) 1_455 . . . ? O8 Cd2 N7 C33 105.9(3) 1_565 . . . ? C10 Cd2 N7 C33 -5.0(3) 1_455 . . . ? C40 Cd2 N7 C33 130.4(3) 1_565 . . . ? O7 Cd2 N7 C31 -29.6(3) 1_565 . . . ? N5 Cd2 N7 C31 69.7(3) . . . . ? O2 Cd2 N7 C31 158.7(2) 1_455 . . . ? O1 Cd2 N7 C31 178.4(3) 1_455 . . . ? O8 Cd2 N7 C31 -78.6(3) 1_565 . . . ? C10 Cd2 N7 C31 170.5(2) 1_455 . . . ? C40 Cd2 N7 C31 -54.1(3) 1_565 . . . ? C3 N1 C1 C2 0.2(4) . . . . ? Cd1 N1 C1 C2 -161.3(2) . . . . ? N1 C1 C2 N2 -0.1(4) . . . . ? C3 N2 C2 C1 0.0(3) . . . . ? C4 N2 C2 C1 -174.5(3) . . . . ? C1 N1 C3 N2 -0.2(4) . . . . ? Cd1 N1 C3 N2 163.03(19) . . . . ? C2 N2 C3 N1 0.2(4) . . . . ? C4 N2 C3 N1 174.9(3) . . . . ? C3 N2 C4 C9 -54.5(4) . . . . ? C2 N2 C4 C9 119.1(4) . . . . ? C3 N2 C4 C5 123.5(3) . . . . ? C2 N2 C4 C5 -62.8(4) . . . . ? C9 C4 C5 C6 0.6(4) . . . . ? N2 C4 C5 C6 -177.3(3) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C4 C5 C6 C10 179.4(3) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C10 C6 C7 C8 -179.6(3) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C5 C4 C9 C8 -1.5(5) . . . . ? N2 C4 C9 C8 176.5(3) . . . . ? C7 C8 C9 C4 1.3(5) . . . . ? Cd2 O1 C10 O2 -2.6(3) 1_655 . . . ? Cd2 O1 C10 C6 177.3(3) 1_655 . . . ? Cd2 O2 C10 O1 2.7(3) 1_655 . . . ? Cd2 O2 C10 C6 -177.2(2) 1_655 . . . ? C5 C6 C10 O1 -0.7(4) . . . . ? C7 C6 C10 O1 178.2(3) . . . . ? C5 C6 C10 O2 179.2(3) . . . . ? C7 C6 C10 O2 -1.9(4) . . . . ? C13 N3 C11 C12 0.6(4) . . . . ? Cd1 N3 C11 C12 -162.0(2) . . . . ? N3 C11 C12 N4 -0.8(4) . . . . ? C13 N4 C12 C11 0.7(3) . . . . ? C14 N4 C12 C11 172.5(3) . . . . ? C11 N3 C13 N4 -0.1(3) . . . . ? Cd1 N3 C13 N4 161.9(2) . . . . ? C12 N4 C13 N3 -0.4(3) . . . . ? C14 N4 C13 N3 -172.4(3) . . . . ? C13 N4 C14 C15 -31.5(4) . . . . ? C12 N4 C14 C15 158.2(3) . . . . ? C13 N4 C14 C19 146.9(3) . . . . ? C12 N4 C14 C19 -23.4(5) . . . . ? C19 C14 C15 C16 -3.6(4) . . . . ? N4 C14 C15 C16 174.8(3) . . . . ? C14 C15 C16 C17 1.5(4) . . . . ? C14 C15 C16 C20 178.7(3) . . . . ? C15 C16 C17 C18 2.2(4) . . . . ? C20 C16 C17 C18 -174.9(3) . . . . ? C16 C17 C18 C19 -3.9(5) . . . . ? C17 C18 C19 C14 1.8(5) . . . . ? C15 C14 C19 C18 2.0(5) . . . . ? N4 C14 C19 C18 -176.4(3) . . . . ? Cd1 O3 C20 O4 2.8(3) 1_565 . . . ? Cd1 O3 C20 C16 -176.7(3) 1_565 . . . ? Cd1 O4 C20 O3 -3.0(3) 1_565 . . . ? Cd1 O4 C20 C16 176.5(2) 1_565 . . . ? C15 C16 C20 O3 -13.9(4) . . . . ? C17 C16 C20 O3 163.2(3) . . . . ? C15 C16 C20 O4 166.5(3) . . . . ? C17 C16 C20 O4 -16.4(4) . . . . ? C23 N6 C21 C22 0.4(4) . . . . ? C24 N6 C21 C22 -173.0(3) . . . . ? N6 C21 C22 N5 -0.5(4) . . . . ? C23 N5 C22 C21 0.4(4) . . . . ? Cd2 N5 C22 C21 -172.0(2) . . . . ? C22 N5 C23 N6 -0.2(4) . . . . ? Cd2 N5 C23 N6 172.7(2) . . . . ? C21 N6 C23 N5 -0.1(4) . . . . ? C24 N6 C23 N5 173.5(3) . . . . ? C23 N6 C24 C25 -58.1(4) . . . . ? C21 N6 C24 C25 114.2(4) . . . . ? C23 N6 C24 C29 122.4(4) . . . . ? C21 N6 C24 C29 -65.3(5) . . . . ? C29 C24 C25 C26 1.1(5) . . . . ? N6 C24 C25 C26 -178.4(3) . . . . ? C24 C25 C26 C27 -0.8(4) . . . . ? C24 C25 C26 C30 176.7(3) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C30 C26 C27 C28 -177.6(3) . . . . ? C26 C27 C28 C29 0.8(5) . . . . ? C25 C24 C29 C28 -0.4(5) . . . . ? N6 C24 C29 C28 179.1(3) . . . . ? C27 C28 C29 C24 -0.5(5) . . . . ? Cd1 O6 C30 O5 -0.1(3) . . . . ? Cd1 O6 C30 C26 -179.7(2) . . . . ? Cd1 O5 C30 O6 0.1(3) . . . . ? Cd1 O5 C30 C26 179.7(2) . . . . ? C25 C26 C30 O6 -5.8(4) . . . . ? C27 C26 C30 O6 171.7(3) . . . . ? C25 C26 C30 O5 174.7(3) . . . . ? C27 C26 C30 O5 -7.9(4) . . . . ? C27 C26 C30 Cd1 36(32) . . . . ? N1 Cd1 C30 O6 -115.04(17) . . . . ? O4 Cd1 C30 O6 83.98(17) 1_545 . . . ? N3 Cd1 C30 O6 -4.4(2) . . . . ? O5 Cd1 C30 O6 -179.9(3) . . . . ? O3 Cd1 C30 O6 141.05(16) 1_545 . . . ? C20 Cd1 C30 O6 110.99(17) 1_545 . . . ? N1 Cd1 C30 O5 64.84(19) . . . . ? O4 Cd1 C30 O5 -96.14(17) 1_545 . . . ? N3 Cd1 C30 O5 175.49(15) . . . . ? O6 Cd1 C30 O5 179.9(3) . . . . ? O3 Cd1 C30 O5 -39.06(18) 1_545 . . . ? C20 Cd1 C30 O5 -69.13(18) 1_545 . . . ? C33 N7 C31 C32 -0.7(4) . . . . ? Cd2 N7 C31 C32 -177.0(2) . . . . ? N7 C31 C32 N8 0.5(4) . . . . ? C33 N8 C32 C31 -0.1(3) . . . . ? C34 N8 C32 C31 179.2(3) . . . . ? C31 N7 C33 N8 0.6(4) . . . . ? Cd2 N7 C33 N8 176.81(19) . . . . ? C32 N8 C33 N7 -0.3(4) . . . . ? C34 N8 C33 N7 -179.6(3) . . . . ? C33 N8 C34 C39 -133.4(3) . . . . ? C32 N8 C34 C39 47.5(4) . . . . ? C33 N8 C34 C35 48.8(4) . . . . ? C32 N8 C34 C35 -130.4(3) . . . . ? C39 C34 C35 C36 2.8(5) . . . . ? N8 C34 C35 C36 -179.3(3) . . . . ? C34 C35 C36 C37 -0.8(5) . . . . ? C34 C35 C36 C40 -176.5(3) . . . . ? C35 C36 C37 C38 -1.6(5) . . . . ? C40 C36 C37 C38 174.1(3) . . . . ? C36 C37 C38 C39 1.9(5) . . . . ? C37 C38 C39 C34 0.1(5) . . . . ? C35 C34 C39 C38 -2.5(5) . . . . ? N8 C34 C39 C38 179.7(3) . . . . ? Cd2 O7 C40 O8 -7.3(4) 1_545 . . . ? Cd2 O7 C40 C36 170.7(2) 1_545 . . . ? Cd2 O8 C40 O7 6.8(3) 1_545 . . . ? Cd2 O8 C40 C36 -171.2(3) 1_545 . . . ? C35 C36 C40 O7 33.9(4) . . . . ? C37 C36 C40 O7 -141.8(3) . . . . ? C35 C36 C40 O8 -148.1(3) . . . . ? C37 C36 C40 O8 36.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.257 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.184 # Attachment 'Compound 9.txt' data_9 _database_code_depnum_ccdc_archive 'CCDC 773585' #TrackingRef 'Compound 9.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 Cd3 N12 O15' _chemical_formula_sum 'C64 H56 Cd3 N12 O15' _chemical_formula_weight 1570.44 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.063(4) _cell_length_b 18.938(5) _cell_length_c 29.918(2) _cell_angle_alpha 90.000 _cell_angle_beta 99.625(3) _cell_angle_gamma 90.000 _cell_volume 6180(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.50 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3148 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7778 _exptl_absorpt_correction_T_max 0.8262 _exptl_absorpt_process_details SADABS _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' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32768 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11420 _reflns_number_gt 8650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Three restraints applied are DFIX and DANG option to fix the O-H distance and H-O-H angle in waters. Another seven restrains were added to fix the bond distance of O10-C64, C64- C63, C61-C62 and C62-O13 using DFIX instruction and O13-O11, O13-C61 and O14- C63 using DANG instruction. ; _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^)+(0.0828P)^2^+17.5382P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11420 _refine_ls_number_parameters 857 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.574 _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 Cd1 Cd 0.50278(7) -0.05264(3) 0.61111(2) 0.0208(2) Uani 1 1 d . . . Cd2 Cd 0.27156(7) 0.01864(3) 0.27228(2) 0.0199(2) Uani 1 1 d . . . Cd3 Cd -0.23700(6) 0.02667(3) -0.04634(2) 0.0198(2) Uani 1 1 d . . . O1 O -0.4982(8) -0.0705(3) -0.3161(2) 0.0333(18) Uani 1 1 d . . . O2 O -0.5506(7) -0.1758(4) -0.3458(2) 0.0348(18) Uani 1 1 d . . . O3 O -0.3181(7) -0.0453(3) 0.0063(2) 0.0300(17) Uani 1 1 d . . . O4 O -0.1531(7) 0.0127(4) 0.0365(2) 0.0338(18) Uani 1 1 d . . . O5 O -0.5752(6) 0.4414(3) 0.1174(2) 0.0224(14) Uani 1 1 d . . . O6 O -0.4802(6) 0.4534(3) 0.0580(2) 0.0211(14) Uani 1 1 d . . . O7 O 0.1053(6) 0.0323(3) 0.3147(2) 0.0229(15) Uani 1 1 d . . . O8 O 0.2760(6) -0.0212(3) 0.3465(2) 0.0216(14) Uani 1 1 d . . . O9 O 0.8067(8) -0.3974(3) 0.2915(3) 0.0372(19) Uani 1 1 d . . . O10 O 0.7290(7) -0.3615(3) 0.2226(2) 0.0307(17) Uani 1 1 d . . . O11 O 1.0753(8) -0.3805(4) 0.5448(3) 0.045(2) Uani 1 1 d D . . O12 O 1.1855(8) -0.4095(4) 0.6079(3) 0.046(2) Uani 1 1 d . . . O13 O 0.9459(18) -0.2989(13) 0.4670(7) 0.189(11) Uani 1 1 d D . . O14 O -0.088(2) 0.0881(9) 0.1828(5) 0.178(10) Uani 1 1 d D . . H14 H -0.0575 0.1248 0.1753 0.282 Uiso 1 1 calc R . . N1 N -0.3875(8) -0.0281(4) -0.0974(3) 0.0214(17) Uani 1 1 d . . . N2 N -0.5010(8) -0.0952(4) -0.1483(2) 0.0199(17) Uani 1 1 d . . . N3 N -0.3550(8) 0.1233(4) -0.0352(3) 0.0234(18) Uani 1 1 d . . . N4 N -0.4507(7) 0.2042(4) -0.0009(3) 0.0209(17) Uani 1 1 d . . . N5 N 0.1322(8) -0.0615(4) 0.2366(3) 0.0270(19) Uani 1 1 d . . . N6 N -0.0318(8) -0.1043(4) 0.1927(3) 0.0226(18) Uani 1 1 d . . . N7 N 0.4176(8) -0.0490(4) 0.2488(3) 0.0226(18) Uani 1 1 d . . . N8 N 0.5806(8) -0.1158(4) 0.2522(3) 0.0229(18) Uani 1 1 d . . . N9 N 0.1842(7) -0.0861(4) 0.5039(2) 0.0219(17) Uani 1 1 d . . . N10 N 0.3330(7) -0.0891(4) 0.5627(3) 0.0219(17) Uani 1 1 d . . . N11 N 0.6526(7) -0.1105(4) 0.5867(3) 0.0203(17) Uani 1 1 d . . . N12 N 0.8239(7) -0.1700(4) 0.5891(2) 0.0196(17) Uani 1 1 d . . . C1 C -0.5070(10) -0.0256(5) -0.0906(3) 0.026(2) Uani 1 1 d . . . H1 H -0.5352 0.0004 -0.0681 0.031 Uiso 1 1 calc R . . C2 C -0.5785(10) -0.0668(5) -0.1218(3) 0.027(2) Uani 1 1 d . . . H2 H -0.6626 -0.0741 -0.1246 0.032 Uiso 1 1 calc R . . C3 C -0.3871(9) -0.0690(5) -0.1323(3) 0.021(2) Uani 1 1 d . . . H3 H -0.3176 -0.0792 -0.1448 0.025 Uiso 1 1 calc R . . C4 C -0.5358(9) -0.1406(5) -0.1872(3) 0.021(2) Uani 1 1 d . . . C5 C -0.5208(9) -0.1167(5) -0.2294(3) 0.021(2) Uani 1 1 d . . . H5 H -0.4887 -0.0719 -0.2326 0.025 Uiso 1 1 calc R . . C6 C -0.5535(9) -0.1593(5) -0.2669(3) 0.023(2) Uani 1 1 d . . . C7 C -0.6035(9) -0.2251(5) -0.2613(3) 0.024(2) Uani 1 1 d . . . H7 H -0.6266 -0.2538 -0.2866 0.029 Uiso 1 1 calc R . . C8 C -0.6200(9) -0.2492(5) -0.2189(3) 0.026(2) Uani 1 1 d . . . H8 H -0.6548 -0.2933 -0.2159 0.031 Uiso 1 1 calc R . . C9 C -0.5840(10) -0.2071(5) -0.1810(3) 0.025(2) Uani 1 1 d . . . H9 H -0.5920 -0.2229 -0.1522 0.030 Uiso 1 1 calc R . . C10 C -0.5338(9) -0.1343(5) -0.3134(3) 0.024(2) Uani 1 1 d . . . C11 C -0.4053(9) 0.1374(5) 0.0004(3) 0.021(2) Uani 1 1 d . . . H11 H -0.4095 0.1055 0.0238 0.026 Uiso 1 1 calc R . . C12 C -0.3692(9) 0.1837(5) -0.0617(3) 0.025(2) Uani 1 1 d . . . H12 H -0.3423 0.1891 -0.0893 0.030 Uiso 1 1 calc R . . C13 C -0.4280(9) 0.2336(5) -0.0412(3) 0.022(2) Uani 1 1 d . . . H13 H -0.4492 0.2788 -0.0520 0.027 Uiso 1 1 calc R . . C14 C -0.5144(9) 0.2366(5) 0.0312(3) 0.020(2) Uani 1 1 d . . . C15 C -0.4901(9) 0.3058(5) 0.0431(3) 0.020(2) Uani 1 1 d . . . H15 H -0.4293 0.3302 0.0314 0.024 Uiso 1 1 calc R . . C16 C -0.5562(9) 0.3392(5) 0.0723(3) 0.0186(19) Uani 1 1 d . . . C17 C -0.6428(9) 0.3015(5) 0.0912(3) 0.024(2) Uani 1 1 d . . . H17 H -0.6842 0.3229 0.1122 0.029 Uiso 1 1 calc R . . C18 C -0.6669(9) 0.2323(5) 0.0788(3) 0.027(2) Uani 1 1 d . . . H18 H -0.7267 0.2076 0.0908 0.032 Uiso 1 1 calc R . . C19 C -0.6029(9) 0.1990(5) 0.0485(3) 0.023(2) Uani 1 1 d . . . H19 H -0.6195 0.1523 0.0401 0.028 Uiso 1 1 calc R . . C20 C -0.5360(9) 0.4156(5) 0.0832(3) 0.020(2) Uani 1 1 d . . . C21 C -0.2326(10) -0.0338(5) 0.0385(3) 0.024(2) Uani 1 1 d . . . C22 C -0.2262(9) -0.0794(5) 0.0799(3) 0.023(2) Uani 1 1 d . . . C23 C -0.1363(9) -0.0691(5) 0.1176(3) 0.024(2) Uani 1 1 d . . . H23 H -0.0807 -0.0323 0.1178 0.028 Uiso 1 1 calc R . . C24 C -0.1289(9) -0.1133(5) 0.1548(3) 0.021(2) Uani 1 1 d . . . C25 C -0.2110(9) -0.1670(5) 0.1555(3) 0.023(2) Uani 1 1 d . . . H25 H -0.2051 -0.1967 0.1805 0.028 Uiso 1 1 calc R . . C26 C -0.3039(9) -0.1768(5) 0.1182(3) 0.023(2) Uani 1 1 d . . . H26 H -0.3612 -0.2126 0.1186 0.028 Uiso 1 1 calc R . . C27 C -0.3108(9) -0.1336(5) 0.0809(3) 0.025(2) Uani 1 1 d . . . H27 H -0.3725 -0.1407 0.0561 0.030 Uiso 1 1 calc R . . C28 C 0.0599(10) -0.0563(5) 0.1974(3) 0.026(2) Uani 1 1 d . . . H28 H 0.0704 -0.0234 0.1752 0.032 Uiso 1 1 calc R . . C29 C -0.0151(10) -0.1427(5) 0.2322(3) 0.029(2) Uani 1 1 d . . . H29 H -0.0637 -0.1798 0.2392 0.034 Uiso 1 1 calc R . . C30 C 0.0856(10) -0.1163(5) 0.2587(3) 0.028(2) Uani 1 1 d . . . H30 H 0.1184 -0.1327 0.2875 0.033 Uiso 1 1 calc R . . C31 C 0.4192(10) -0.0762(5) 0.2058(3) 0.025(2) Uani 1 1 d . . . H31 H 0.3616 -0.0672 0.1800 0.030 Uiso 1 1 calc R . . C32 C 0.5200(10) -0.1184(5) 0.2078(3) 0.027(2) Uani 1 1 d . . . H32 H 0.5434 -0.1438 0.1841 0.032 Uiso 1 1 calc R . . C33 C 0.5147(9) -0.0746(4) 0.2758(3) 0.022(2) Uani 1 1 d . . . H33 H 0.5345 -0.0653 0.3067 0.026 Uiso 1 1 calc R . . C34 C 0.6808(9) -0.1594(5) 0.2724(3) 0.022(2) Uani 1 1 d . . . C35 C 0.6887(9) -0.2280(5) 0.2567(3) 0.021(2) Uani 1 1 d . . . H35 H 0.6351 -0.2435 0.2312 0.025 Uiso 1 1 calc R . . C36 C 0.7772(9) -0.2731(5) 0.2792(3) 0.022(2) Uani 1 1 d . . . C37 C 0.8596(10) -0.2491(5) 0.3157(3) 0.029(2) Uani 1 1 d . . . H37 H 0.9187 -0.2795 0.3309 0.034 Uiso 1 1 calc R . . C38 C 0.8544(10) -0.1802(5) 0.3295(3) 0.028(2) Uani 1 1 d . . . H38 H 0.9116 -0.1639 0.3536 0.034 Uiso 1 1 calc R . . C39 C 0.7653(9) -0.1347(5) 0.3081(3) 0.025(2) Uani 1 1 d . . . H39 H 0.7625 -0.0880 0.3176 0.030 Uiso 1 1 calc R . . C40 C 0.7732(9) -0.3486(5) 0.2636(3) 0.025(2) Uani 1 1 d . . . C41 C 0.1660(9) -0.0018(5) 0.3462(3) 0.022(2) Uani 1 1 d . . . C42 C 0.1051(9) -0.0209(5) 0.3865(3) 0.021(2) Uani 1 1 d . . . C43 C -0.0230(9) -0.0142(5) 0.3822(3) 0.022(2) Uani 1 1 d . . . H43 H -0.0684 0.0038 0.3557 0.026 Uiso 1 1 calc R . . C44 C -0.0808(10) -0.0344(5) 0.4176(3) 0.027(2) Uani 1 1 d . . . H44 H -0.1656 -0.0314 0.4146 0.032 Uiso 1 1 calc R . . C45 C -0.0130(9) -0.0589(5) 0.4574(3) 0.024(2) Uani 1 1 d . . . H45 H -0.0521 -0.0721 0.4814 0.029 Uiso 1 1 calc R . . C46 C 0.1137(9) -0.0640(5) 0.4618(3) 0.021(2) Uani 1 1 d . . . C47 C 0.1735(9) -0.0465(5) 0.4259(3) 0.022(2) Uani 1 1 d . . . H47 H 0.2579 -0.0520 0.4284 0.027 Uiso 1 1 calc R . . C48 C 0.2961(9) -0.0614(5) 0.5225(3) 0.020(2) Uani 1 1 d . . . H48 H 0.3410 -0.0289 0.5086 0.024 Uiso 1 1 calc R . . C49 C 0.1486(10) -0.1325(5) 0.5353(3) 0.027(2) Uani 1 1 d . . . H49 H 0.0753 -0.1574 0.5326 0.033 Uiso 1 1 calc R . . C50 C 0.2418(10) -0.1339(5) 0.5701(3) 0.027(2) Uani 1 1 d . . . H50 H 0.2440 -0.1616 0.5959 0.032 Uiso 1 1 calc R . . C51 C 0.6762(9) -0.1186(5) 0.5430(3) 0.021(2) Uani 1 1 d . . . H51 H 0.6275 -0.1013 0.5170 0.026 Uiso 1 1 calc R . . C52 C 0.7814(10) -0.1558(5) 0.5441(3) 0.028(2) Uani 1 1 d . . . H52 H 0.8174 -0.1690 0.5194 0.033 Uiso 1 1 calc R . . C53 C 0.7441(9) -0.1422(4) 0.6132(3) 0.020(2) Uani 1 1 d . . . H53 H 0.7521 -0.1448 0.6446 0.024 Uiso 1 1 calc R . . C54 C 0.9338(9) -0.2072(5) 0.6081(3) 0.022(2) Uani 1 1 d . . . C55 C 0.9986(9) -0.1843(5) 0.6489(3) 0.025(2) Uani 1 1 d . . . H55 H 0.9752 -0.1438 0.6628 0.030 Uiso 1 1 calc R . . C56 C 1.1001(9) -0.2236(5) 0.6688(4) 0.030(2) Uani 1 1 d . . . H56 H 1.1448 -0.2095 0.6965 0.036 Uiso 1 1 calc R . . C57 C 1.1343(10) -0.2830(5) 0.6477(4) 0.031(2) Uani 1 1 d . . . H57 H 1.2010 -0.3095 0.6614 0.038 Uiso 1 1 calc R . . C58 C 1.0693(10) -0.3035(5) 0.6058(4) 0.031(2) Uani 1 1 d . . . C59 C 0.9690(10) -0.2656(5) 0.5859(3) 0.025(2) Uani 1 1 d . . . H59 H 0.9254 -0.2791 0.5579 0.030 Uiso 1 1 calc R . . C60 C 1.1112(11) -0.3690(5) 0.5852(4) 0.036(3) Uani 1 1 d . . . C61 C 1.142(2) -0.279(2) 0.4342(11) 0.24(2) Uani 1 1 d D . . H61A H 1.2039 -0.2511 0.4526 0.362 Uiso 1 1 calc R . . H61B H 1.1441 -0.2698 0.4028 0.362 Uiso 1 1 calc R . . H61C H 1.1561 -0.3279 0.4406 0.362 Uiso 1 1 calc R . . C62 C 1.023(2) -0.2592(13) 0.4442(14) 0.22(7) Uani 1 1 d D . . H62A H 1.0357 -0.2150 0.4607 0.591 Uiso 1 1 calc R . . H62B H 0.9738 -0.2477 0.4151 0.591 Uiso 1 1 calc R . . C63 C -0.1839(16) 0.0330(8) 0.2455(6) 0.080(5) Uani 1 1 d D . . H63A H -0.2084 0.0457 0.2737 0.119 Uiso 1 1 calc R . . H63B H -0.1261 -0.0051 0.2503 0.119 Uiso 1 1 calc R . . H63C H -0.2546 0.0185 0.2243 0.119 Uiso 1 1 calc R . . C64 C -0.1239(15) 0.0974(8) 0.2262(5) 0.074(5) Uani 1 1 d D . . H64A H -0.1810 0.1366 0.2242 0.089 Uiso 1 1 calc R . . H64B H -0.0519 0.1106 0.2478 0.089 Uiso 1 1 calc R . . OW1 O -0.0873(10) -0.0530(5) -0.0563(4) 0.065(3) Uani 1 1 d D . . H2W1 H -0.020(8) -0.047(7) -0.039(4) 0.07(7) Uiso 1 1 d D . . H1W1 H -0.125(7) -0.086(3) -0.046(3) 0.07(2) 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 Cd1 0.0285(4) 0.0180(4) 0.0159(4) 0.0007(3) 0.0032(3) 0.0062(3) Cd2 0.0253(4) 0.0178(3) 0.0169(4) 0.0022(3) 0.0046(3) 0.0011(3) Cd3 0.0220(4) 0.0163(3) 0.0215(4) -0.0017(3) 0.0050(3) 0.0001(3) O1 0.063(6) 0.017(3) 0.020(4) 0.002(3) 0.010(4) 0.007(3) O2 0.043(5) 0.041(4) 0.019(4) -0.009(3) 0.002(3) -0.005(4) O3 0.043(5) 0.023(3) 0.021(4) 0.003(3) -0.003(3) -0.004(3) O4 0.027(4) 0.037(4) 0.035(4) 0.015(3) -0.003(3) -0.006(3) O5 0.028(4) 0.022(3) 0.018(3) -0.005(3) 0.006(3) -0.003(3) O6 0.021(4) 0.024(3) 0.019(3) 0.000(3) 0.004(3) -0.002(3) O7 0.031(4) 0.021(3) 0.017(3) 0.002(3) 0.004(3) 0.002(3) O8 0.023(4) 0.026(3) 0.017(3) 0.002(3) 0.005(3) 0.001(3) O9 0.055(5) 0.020(3) 0.040(4) 0.005(3) 0.016(4) 0.003(3) O10 0.037(4) 0.023(3) 0.031(4) -0.007(3) 0.003(3) 0.004(3) O11 0.051(5) 0.023(4) 0.072(6) -0.009(4) 0.041(5) -0.002(4) O12 0.057(6) 0.022(4) 0.072(6) 0.015(4) 0.043(5) 0.019(4) O13 0.121(17) 0.28(3) 0.178(19) -0.093(19) -0.015(14) 0.067(18) O14 0.35(3) 0.120(13) 0.101(13) -0.024(11) 0.050(16) 0.047(17) N1 0.031(5) 0.016(4) 0.018(4) 0.000(3) 0.006(4) -0.001(3) N2 0.031(5) 0.019(4) 0.011(4) -0.001(3) 0.004(3) -0.001(3) N3 0.028(5) 0.019(4) 0.025(4) -0.001(3) 0.009(4) 0.000(3) N4 0.023(4) 0.017(4) 0.023(4) -0.001(3) 0.004(3) -0.002(3) N5 0.030(5) 0.033(5) 0.018(4) 0.001(4) 0.003(4) -0.003(4) N6 0.027(5) 0.021(4) 0.021(4) 0.000(3) 0.005(4) 0.001(3) N7 0.032(5) 0.018(4) 0.018(4) -0.002(3) 0.004(4) -0.001(3) N8 0.029(5) 0.019(4) 0.022(4) -0.001(3) 0.008(4) 0.001(3) N9 0.023(4) 0.029(4) 0.015(4) 0.006(3) 0.007(3) -0.003(4) N10 0.025(5) 0.021(4) 0.021(4) 0.001(3) 0.008(4) 0.001(3) N11 0.026(5) 0.015(4) 0.020(4) 0.000(3) 0.003(3) -0.002(3) N12 0.024(4) 0.018(4) 0.016(4) -0.002(3) 0.003(3) 0.000(3) C1 0.033(6) 0.026(5) 0.020(5) 0.001(4) 0.010(4) -0.002(4) C2 0.024(5) 0.033(5) 0.024(5) -0.003(4) 0.004(4) -0.002(4) C3 0.023(5) 0.021(4) 0.019(5) 0.005(4) 0.007(4) -0.003(4) C4 0.021(5) 0.024(5) 0.017(5) -0.003(4) 0.001(4) 0.000(4) C5 0.026(5) 0.016(4) 0.023(5) 0.004(4) 0.005(4) 0.000(4) C6 0.021(5) 0.025(5) 0.021(5) 0.005(4) 0.001(4) 0.007(4) C7 0.026(6) 0.020(5) 0.023(5) -0.005(4) -0.003(4) 0.006(4) C8 0.020(5) 0.020(5) 0.036(6) -0.001(4) 0.000(4) 0.000(4) C9 0.032(6) 0.024(5) 0.019(5) 0.004(4) 0.004(4) -0.002(4) C10 0.022(5) 0.027(5) 0.022(5) 0.001(4) -0.003(4) 0.009(4) C11 0.021(5) 0.019(4) 0.023(5) 0.000(4) 0.002(4) -0.002(4) C12 0.030(6) 0.019(4) 0.030(5) 0.003(4) 0.011(5) 0.005(4) C13 0.033(6) 0.016(4) 0.020(5) 0.003(4) 0.009(4) -0.001(4) C14 0.028(5) 0.019(4) 0.015(4) 0.001(4) 0.005(4) 0.003(4) C15 0.020(5) 0.020(4) 0.020(5) 0.002(4) 0.004(4) -0.005(4) C16 0.023(5) 0.020(4) 0.012(4) -0.001(4) 0.000(4) 0.002(4) C17 0.029(6) 0.020(5) 0.028(5) -0.001(4) 0.015(4) 0.003(4) C18 0.022(5) 0.025(5) 0.036(6) 0.002(4) 0.011(5) -0.002(4) C19 0.030(6) 0.013(4) 0.026(5) 0.002(4) 0.004(4) 0.003(4) C20 0.018(5) 0.021(4) 0.018(5) -0.002(4) -0.002(4) 0.002(4) C21 0.028(6) 0.021(5) 0.023(5) 0.002(4) 0.007(5) 0.006(4) C22 0.021(5) 0.021(5) 0.025(5) 0.003(4) 0.003(4) 0.006(4) C23 0.027(6) 0.017(4) 0.029(5) -0.004(4) 0.009(4) -0.001(4) C24 0.023(5) 0.022(5) 0.017(5) -0.007(4) 0.000(4) 0.001(4) C25 0.028(6) 0.024(5) 0.019(5) -0.002(4) 0.008(4) 0.006(4) C26 0.017(5) 0.027(5) 0.026(5) -0.002(4) 0.008(4) -0.001(4) C27 0.022(5) 0.029(5) 0.023(5) -0.001(4) 0.001(4) 0.002(4) C28 0.033(6) 0.027(5) 0.018(5) 0.002(4) 0.004(4) -0.007(4) C29 0.033(6) 0.030(5) 0.022(5) 0.004(4) -0.001(4) -0.005(5) C30 0.035(6) 0.027(5) 0.022(5) 0.005(4) 0.004(5) 0.004(5) C31 0.034(6) 0.022(5) 0.019(5) 0.003(4) 0.005(4) -0.001(4) C32 0.041(6) 0.022(5) 0.020(5) -0.001(4) 0.009(5) -0.002(5) C33 0.030(6) 0.013(4) 0.021(5) -0.004(4) 0.004(4) 0.001(4) C34 0.023(5) 0.026(5) 0.019(5) 0.002(4) 0.009(4) 0.002(4) C35 0.021(5) 0.020(4) 0.020(5) -0.004(4) 0.003(4) -0.005(4) C36 0.026(5) 0.016(4) 0.026(5) 0.001(4) 0.011(4) 0.000(4) C37 0.031(6) 0.034(5) 0.023(5) 0.003(4) 0.010(5) 0.004(5) C38 0.025(6) 0.032(5) 0.027(6) -0.002(4) 0.002(4) -0.001(5) C39 0.030(6) 0.021(5) 0.025(5) -0.004(4) 0.004(4) -0.004(4) C40 0.025(6) 0.018(5) 0.034(6) 0.000(4) 0.014(5) -0.001(4) C41 0.027(6) 0.021(4) 0.019(5) -0.006(4) 0.008(4) -0.003(4) C42 0.023(5) 0.019(4) 0.020(5) -0.002(4) 0.003(4) -0.002(4) C43 0.025(5) 0.021(5) 0.019(5) 0.000(4) 0.003(4) 0.001(4) C44 0.021(5) 0.028(5) 0.033(6) -0.008(4) 0.008(4) -0.003(4) C45 0.025(5) 0.027(5) 0.021(5) -0.002(4) 0.008(4) -0.002(4) C46 0.023(5) 0.019(4) 0.022(5) -0.002(4) 0.004(4) -0.002(4) C47 0.018(5) 0.021(5) 0.026(5) -0.001(4) 0.000(4) -0.002(4) C48 0.017(5) 0.022(4) 0.022(5) 0.005(4) 0.006(4) -0.002(4) C49 0.028(6) 0.030(5) 0.025(5) 0.004(4) 0.007(4) -0.008(4) C50 0.035(6) 0.022(5) 0.028(6) 0.005(4) 0.017(5) 0.003(4) C51 0.028(5) 0.017(4) 0.017(5) -0.004(4) 0.001(4) -0.002(4) C52 0.039(6) 0.026(5) 0.020(5) -0.001(4) 0.010(5) -0.008(5) C53 0.028(5) 0.015(4) 0.018(5) -0.002(4) 0.005(4) -0.001(4) C54 0.023(5) 0.017(4) 0.028(5) 0.003(4) 0.008(4) 0.002(4) C55 0.024(5) 0.023(5) 0.030(6) -0.005(4) 0.009(4) 0.003(4) C56 0.020(5) 0.031(5) 0.038(6) 0.000(5) 0.003(5) 0.002(4) C57 0.024(6) 0.024(5) 0.048(7) 0.008(5) 0.013(5) 0.005(4) C58 0.029(6) 0.021(5) 0.050(7) -0.001(5) 0.023(5) -0.002(4) C59 0.029(6) 0.019(4) 0.030(5) 0.002(4) 0.014(5) -0.003(4) C60 0.046(7) 0.020(5) 0.052(8) -0.013(5) 0.035(6) -0.002(5) C61 0.08(2) 0.41(6) 0.22(4) 0.08(4) -0.01(2) 0.09(3) C62 0.18(3) 0.164(18) 0.25(16) 0.15(4) -0.15(7) -0.09(2) C63 0.071(12) 0.070(11) 0.092(13) -0.001(9) -0.002(10) 0.039(9) C64 0.072(11) 0.079(11) 0.082(11) -0.033(9) 0.005(9) 0.035(9) OW1 0.035(6) 0.033(5) 0.134(10) -0.015(6) 0.030(7) 0.004(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 Cd1 O1 2.205(7) 1_656 ? Cd1 N11 2.210(8) . ? Cd1 N10 2.279(8) . ? Cd1 O5 2.296(6) 4_666 ? Cd1 O6 2.488(6) 4_666 ? Cd1 C20 2.738(9) 4_666 ? Cd2 N7 2.264(8) . ? Cd2 O10 2.275(7) 2_655 ? Cd2 N5 2.295(8) . ? Cd2 O8 2.338(6) . ? Cd2 O7 2.418(7) . ? Cd2 O9 2.523(7) 2_655 ? Cd2 C41 2.696(9) . ? Cd2 C40 2.745(9) 2_655 ? Cd3 OW1 2.296(9) . ? Cd3 N3 2.303(8) . ? Cd3 N1 2.308(8) . ? Cd3 O12 2.351(8) 2_655 ? Cd3 O3 2.369(7) . ? Cd3 O11 2.503(8) 2_655 ? Cd3 O4 2.511(7) . ? O1 C10 1.278(12) . ? O1 Cd1 2.204(7) 1_454 ? O2 C10 1.237(11) . ? O3 C21 1.251(12) . ? O4 C21 1.253(12) . ? O5 C20 1.274(11) . ? O5 Cd1 2.296(6) 4_465 ? O6 C20 1.271(11) . ? O6 Cd1 2.488(6) 4_465 ? O7 C41 1.242(11) . ? O8 C41 1.269(12) . ? O9 C40 1.257(12) . ? O9 Cd2 2.523(7) 2_645 ? O10 C40 1.265(12) . ? O10 Cd2 2.275(7) 2_645 ? O11 C60 1.227(14) . ? O11 Cd3 2.503(8) 2_645 ? O12 C60 1.241(14) . ? O12 Cd3 2.351(8) 2_645 ? O13 C62 1.40(3) . ? O14 C64 1.432(17) . ? N1 C3 1.301(12) . ? N1 C1 1.372(13) . ? N2 C3 1.364(12) . ? N2 C2 1.371(12) . ? N2 C4 1.446(11) . ? N3 C11 1.311(12) . ? N3 C12 1.386(12) . ? N4 C11 1.359(11) . ? N4 C13 1.389(12) . ? N4 C14 1.423(12) . ? N5 C28 1.309(13) . ? N5 C30 1.378(13) . ? N6 C28 1.352(13) . ? N6 C29 1.372(12) . ? N6 C24 1.436(12) . ? N7 C33 1.324(13) . ? N7 C31 1.388(12) . ? N8 C33 1.347(12) . ? N8 C32 1.385(12) . ? N8 C34 1.432(12) . ? N9 C48 1.353(12) . ? N9 C49 1.391(12) . ? N9 C46 1.430(12) . ? N10 C48 1.314(12) . ? N10 C50 1.364(12) . ? N11 C53 1.321(12) . ? N11 C51 1.384(11) . ? N12 C53 1.337(12) . ? N12 C52 1.378(12) . ? N12 C54 1.437(12) . ? C1 C2 1.363(14) . ? C4 C5 1.377(13) . ? C4 C9 1.392(13) . ? C5 C6 1.381(13) . ? C6 C7 1.385(13) . ? C6 C10 1.520(13) . ? C7 C8 1.391(14) . ? C8 C9 1.388(13) . ? C12 C13 1.352(13) . ? C14 C15 1.371(12) . ? C14 C19 1.380(13) . ? C15 C16 1.383(13) . ? C16 C17 1.389(13) . ? C16 C20 1.492(12) . ? C17 C18 1.375(13) . ? C18 C19 1.390(13) . ? C20 Cd1 2.738(9) 4_465 ? C21 C22 1.504(13) . ? C22 C23 1.386(14) . ? C22 C27 1.393(14) . ? C23 C24 1.384(13) . ? C24 C25 1.366(13) . ? C25 C26 1.398(14) . ? C26 C27 1.376(13) . ? C29 C30 1.351(15) . ? C31 C32 1.364(14) . ? C34 C39 1.378(14) . ? C34 C35 1.389(13) . ? C35 C36 1.388(13) . ? C36 C37 1.376(14) . ? C36 C40 1.503(12) . ? C37 C38 1.373(14) . ? C38 C39 1.384(14) . ? C40 Cd2 2.745(9) 2_645 ? C41 C42 1.519(13) . ? C42 C47 1.378(13) . ? C42 C43 1.407(13) . ? C43 C44 1.380(13) . ? C44 C45 1.378(14) . ? C45 C46 1.389(13) . ? C46 C47 1.392(13) . ? C49 C50 1.338(15) . ? C51 C52 1.355(14) . ? C54 C55 1.378(14) . ? C54 C59 1.379(13) . ? C55 C56 1.395(14) . ? C56 C57 1.373(14) . ? C57 C58 1.392(15) . ? C58 C59 1.371(15) . ? C58 C60 1.492(13) . ? C61 C62 1.44(3) . ? C63 C64 1.545(19) . ? 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 Cd1 N11 112.2(3) 1_656 . ? O1 Cd1 N10 116.2(3) 1_656 . ? N11 Cd1 N10 102.9(3) . . ? O1 Cd1 O5 89.8(2) 1_656 4_666 ? N11 Cd1 O5 142.6(2) . 4_666 ? N10 Cd1 O5 92.8(3) . 4_666 ? O1 Cd1 O6 139.4(2) 1_656 4_666 ? N11 Cd1 O6 91.3(2) . 4_666 ? N10 Cd1 O6 88.0(2) . 4_666 ? O5 Cd1 O6 55.2(2) 4_666 4_666 ? O1 Cd1 C20 114.9(3) 1_656 4_666 ? N11 Cd1 C20 117.2(3) . 4_666 ? N10 Cd1 C20 91.3(3) . 4_666 ? O5 Cd1 C20 27.6(2) 4_666 4_666 ? O6 Cd1 C20 27.6(2) 4_666 4_666 ? N7 Cd2 O10 126.5(3) . 2_655 ? N7 Cd2 N5 86.6(3) . . ? O10 Cd2 N5 133.0(3) 2_655 . ? N7 Cd2 O8 102.1(3) . . ? O10 Cd2 O8 104.9(2) 2_655 . ? N5 Cd2 O8 97.7(3) . . ? N7 Cd2 O7 150.3(2) . . ? O10 Cd2 O7 81.2(2) 2_655 . ? N5 Cd2 O7 78.7(3) . . ? O8 Cd2 O7 55.4(2) . . ? N7 Cd2 O9 107.1(3) . 2_655 ? O10 Cd2 O9 54.3(2) 2_655 2_655 ? N5 Cd2 O9 86.9(3) . 2_655 ? O8 Cd2 O9 150.6(2) . 2_655 ? O7 Cd2 O9 97.7(2) . 2_655 ? N7 Cd2 C41 127.1(3) . . ? O10 Cd2 C41 94.7(3) 2_655 . ? N5 Cd2 C41 86.4(3) . . ? O8 Cd2 C41 28.1(3) . . ? O7 Cd2 C41 27.4(3) . . ? O9 Cd2 C41 124.7(3) 2_655 . ? N7 Cd2 C40 119.2(3) . 2_655 ? O10 Cd2 C40 27.2(3) 2_655 2_655 ? N5 Cd2 C40 111.1(3) . 2_655 ? O8 Cd2 C40 129.8(3) . 2_655 ? O7 Cd2 C40 90.2(2) . 2_655 ? O9 Cd2 C40 27.2(3) 2_655 2_655 ? C41 Cd2 C40 112.2(3) . 2_655 ? OW1 Cd3 N3 168.2(3) . . ? OW1 Cd3 N1 94.3(4) . . ? N3 Cd3 N1 95.1(3) . . ? OW1 Cd3 O12 87.8(3) . 2_655 ? N3 Cd3 O12 85.5(3) . 2_655 ? N1 Cd3 O12 87.4(3) . 2_655 ? OW1 Cd3 O3 94.0(3) . . ? N3 Cd3 O3 94.3(3) . . ? N1 Cd3 O3 82.5(2) . . ? O12 Cd3 O3 169.9(3) 2_655 . ? OW1 Cd3 O11 86.3(3) . 2_655 ? N3 Cd3 O11 82.0(3) . 2_655 ? N1 Cd3 O11 139.6(3) . 2_655 ? O12 Cd3 O11 52.2(3) 2_655 2_655 ? O3 Cd3 O11 137.8(3) . 2_655 ? OW1 Cd3 O4 84.5(4) . . ? N3 Cd3 O4 93.8(3) . . ? N1 Cd3 O4 135.4(2) . . ? O12 Cd3 O4 136.8(3) 2_655 . ? O3 Cd3 O4 53.3(2) . . ? O11 Cd3 O4 84.9(3) 2_655 . ? C10 O1 Cd1 105.1(6) . 1_454 ? C21 O3 Cd3 95.1(6) . . ? C21 O4 Cd3 88.5(6) . . ? C20 O5 Cd1 95.9(5) . 4_465 ? C20 O6 Cd1 87.2(5) . 4_465 ? C41 O7 Cd2 88.9(6) . . ? C41 O8 Cd2 91.9(5) . . ? C40 O9 Cd2 86.3(6) . 2_645 ? C40 O10 Cd2 97.6(6) . 2_645 ? C60 O11 Cd3 89.6(7) . 2_645 ? C60 O12 Cd3 96.5(7) . 2_645 ? C3 N1 C1 105.7(8) . . ? C3 N1 Cd3 134.4(7) . . ? C1 N1 Cd3 119.6(6) . . ? C3 N2 C2 106.5(8) . . ? C3 N2 C4 127.2(8) . . ? C2 N2 C4 126.1(8) . . ? C11 N3 C12 105.9(8) . . ? C11 N3 Cd3 127.4(6) . . ? C12 N3 Cd3 125.9(6) . . ? C11 N4 C13 106.2(8) . . ? C11 N4 C14 127.2(8) . . ? C13 N4 C14 126.5(8) . . ? C28 N5 C30 105.4(8) . . ? C28 N5 Cd2 129.1(7) . . ? C30 N5 Cd2 123.5(6) . . ? C28 N6 C29 106.1(8) . . ? C28 N6 C24 127.6(8) . . ? C29 N6 C24 126.3(8) . . ? C33 N7 C31 107.2(8) . . ? C33 N7 Cd2 124.4(6) . . ? C31 N7 Cd2 128.2(7) . . ? C33 N8 C32 107.7(8) . . ? C33 N8 C34 124.2(8) . . ? C32 N8 C34 127.0(8) . . ? C48 N9 C49 106.5(8) . . ? C48 N9 C46 126.1(8) . . ? C49 N9 C46 127.3(8) . . ? C48 N10 C50 105.8(8) . . ? C48 N10 Cd1 123.9(6) . . ? C50 N10 Cd1 129.7(6) . . ? C53 N11 C51 105.5(8) . . ? C53 N11 Cd1 124.7(6) . . ? C51 N11 Cd1 129.7(6) . . ? C53 N12 C52 107.5(8) . . ? C53 N12 C54 124.9(8) . . ? C52 N12 C54 127.6(8) . . ? C2 C1 N1 110.1(9) . . ? C1 C2 N2 105.8(9) . . ? N1 C3 N2 111.9(9) . . ? C5 C4 C9 121.8(9) . . ? C5 C4 N2 119.0(8) . . ? C9 C4 N2 119.2(8) . . ? C4 C5 C6 119.8(9) . . ? C5 C6 C7 119.0(9) . . ? C5 C6 C10 120.3(8) . . ? C7 C6 C10 120.7(9) . . ? C6 C7 C8 121.4(9) . . ? C9 C8 C7 119.6(9) . . ? C8 C9 C4 118.4(9) . . ? O2 C10 O1 123.9(9) . . ? O2 C10 C6 119.6(9) . . ? O1 C10 C6 116.4(8) . . ? N3 C11 N4 111.8(8) . . ? C13 C12 N3 109.6(8) . . ? C12 C13 N4 106.5(8) . . ? C15 C14 C19 121.2(9) . . ? C15 C14 N4 119.3(8) . . ? C19 C14 N4 119.5(8) . . ? C14 C15 C16 119.9(9) . . ? C15 C16 C17 119.7(8) . . ? C15 C16 C20 120.4(8) . . ? C17 C16 C20 119.8(8) . . ? C18 C17 C16 119.7(9) . . ? C17 C18 C19 120.8(9) . . ? C14 C19 C18 118.7(9) . . ? O6 C20 O5 121.6(8) . . ? O6 C20 C16 119.1(8) . . ? O5 C20 C16 119.2(8) . . ? O6 C20 Cd1 65.2(5) . 4_465 ? O5 C20 Cd1 56.5(4) . 4_465 ? C16 C20 Cd1 174.9(6) . 4_465 ? O3 C21 O4 122.2(9) . . ? O3 C21 C22 117.4(9) . . ? O4 C21 C22 120.4(9) . . ? C23 C22 C27 118.7(9) . . ? C23 C22 C21 121.2(9) . . ? C27 C22 C21 120.1(9) . . ? C24 C23 C22 120.5(9) . . ? C25 C24 C23 120.8(9) . . ? C25 C24 N6 119.2(8) . . ? C23 C24 N6 120.0(9) . . ? C24 C25 C26 119.2(9) . . ? C27 C26 C25 120.2(9) . . ? C26 C27 C22 120.5(9) . . ? N5 C28 N6 112.2(8) . . ? C30 C29 N6 106.8(9) . . ? C29 C30 N5 109.6(9) . . ? C32 C31 N7 108.2(9) . . ? C31 C32 N8 106.5(8) . . ? N7 C33 N8 110.3(8) . . ? C39 C34 C35 120.5(9) . . ? C39 C34 N8 120.5(8) . . ? C35 C34 N8 118.9(9) . . ? C36 C35 C34 119.3(9) . . ? C37 C36 C35 120.2(9) . . ? C37 C36 C40 122.9(9) . . ? C35 C36 C40 116.9(9) . . ? C38 C37 C36 119.8(10) . . ? C37 C38 C39 121.1(10) . . ? C34 C39 C38 119.0(9) . . ? O9 C40 O10 121.6(9) . . ? O9 C40 C36 120.1(9) . . ? O10 C40 C36 118.1(9) . . ? O9 C40 Cd2 66.5(5) . 2_645 ? O10 C40 Cd2 55.2(5) . 2_645 ? C36 C40 Cd2 170.7(7) . 2_645 ? O7 C41 O8 123.5(8) . . ? O7 C41 C42 118.0(9) . . ? O8 C41 C42 118.5(8) . . ? O7 C41 Cd2 63.7(5) . . ? O8 C41 Cd2 60.1(5) . . ? C42 C41 Cd2 174.3(6) . . ? C47 C42 C43 120.7(9) . . ? C47 C42 C41 120.6(9) . . ? C43 C42 C41 118.7(8) . . ? C44 C43 C42 119.6(9) . . ? C45 C44 C43 120.2(10) . . ? C44 C45 C46 119.9(9) . . ? C45 C46 C47 121.0(9) . . ? C45 C46 N9 119.7(8) . . ? C47 C46 N9 119.3(9) . . ? C42 C47 C46 118.7(9) . . ? N10 C48 N9 111.2(8) . . ? C50 C49 N9 105.6(9) . . ? C49 C50 N10 110.9(9) . . ? C52 C51 N11 109.5(8) . . ? C51 C52 N12 106.0(8) . . ? N11 C53 N12 111.5(8) . . ? C55 C54 C59 122.1(9) . . ? C55 C54 N12 118.4(8) . . ? C59 C54 N12 119.4(9) . . ? C54 C55 C56 118.2(9) . . ? C57 C56 C55 120.3(10) . . ? C56 C57 C58 120.2(10) . . ? C59 C58 C57 120.2(9) . . ? C59 C58 C60 122.7(11) . . ? C57 C58 C60 117.1(10) . . ? C58 C59 C54 119.0(10) . . ? O11 C60 O12 120.4(9) . . ? O11 C60 C58 118.8(11) . . ? O12 C60 C58 120.7(11) . . ? O13 C62 C61 128(3) . . ? O14 C64 C63 116.3(14) . . ? 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 OW1 Cd3 O3 C21 74.8(6) . . . . ? N3 Cd3 O3 C21 -96.8(6) . . . . ? N1 Cd3 O3 C21 168.6(6) . . . . ? O12 Cd3 O3 C21 174.7(13) 2_655 . . . ? O11 Cd3 O3 C21 -14.0(7) 2_655 . . . ? O4 Cd3 O3 C21 -5.3(5) . . . . ? OW1 Cd3 O4 C21 -94.0(6) . . . . ? N3 Cd3 O4 C21 97.7(6) . . . . ? N1 Cd3 O4 C21 -3.4(7) . . . . ? O12 Cd3 O4 C21 -174.8(5) 2_655 . . . ? O3 Cd3 O4 C21 5.2(5) . . . . ? O11 Cd3 O4 C21 179.3(6) 2_655 . . . ? N7 Cd2 O7 C41 42.6(8) . . . . ? O10 Cd2 O7 C41 -118.5(6) 2_655 . . . ? N5 Cd2 O7 C41 104.3(6) . . . . ? O8 Cd2 O7 C41 -3.4(5) . . . . ? O9 Cd2 O7 C41 -170.4(5) 2_655 . . . ? C40 Cd2 O7 C41 -144.2(6) 2_655 . . . ? N7 Cd2 O8 C41 -155.3(5) . . . . ? O10 Cd2 O8 C41 71.3(5) 2_655 . . . ? N5 Cd2 O8 C41 -67.1(6) . . . . ? O7 Cd2 O8 C41 3.4(5) . . . . ? O9 Cd2 O8 C41 30.4(8) 2_655 . . . ? C40 Cd2 O8 C41 58.8(6) 2_655 . . . ? OW1 Cd3 N1 C3 -24.6(9) . . . . ? N3 Cd3 N1 C3 148.3(8) . . . . ? O12 Cd3 N1 C3 63.0(8) 2_655 . . . ? O3 Cd3 N1 C3 -118.1(9) . . . . ? O11 Cd3 N1 C3 64.7(10) 2_655 . . . ? O4 Cd3 N1 C3 -111.1(8) . . . . ? OW1 Cd3 N1 C1 148.4(7) . . . . ? N3 Cd3 N1 C1 -38.7(7) . . . . ? O12 Cd3 N1 C1 -124.0(7) 2_655 . . . ? O3 Cd3 N1 C1 54.9(7) . . . . ? O11 Cd3 N1 C1 -122.3(7) 2_655 . . . ? O4 Cd3 N1 C1 61.9(8) . . . . ? OW1 Cd3 N3 C11 -111.2(19) . . . . ? N1 Cd3 N3 C11 106.0(8) . . . . ? O12 Cd3 N3 C11 -167.0(8) 2_655 . . . ? O3 Cd3 N3 C11 23.2(8) . . . . ? O11 Cd3 N3 C11 -114.5(8) 2_655 . . . ? O4 Cd3 N3 C11 -30.3(8) . . . . ? OW1 Cd3 N3 C12 57(2) . . . . ? N1 Cd3 N3 C12 -85.8(8) . . . . ? O12 Cd3 N3 C12 1.2(8) 2_655 . . . ? O3 Cd3 N3 C12 -168.6(8) . . . . ? O11 Cd3 N3 C12 53.7(8) 2_655 . . . ? O4 Cd3 N3 C12 137.9(8) . . . . ? N7 Cd2 N5 C28 -102.0(9) . . . . ? O10 Cd2 N5 C28 37.4(10) 2_655 . . . ? O8 Cd2 N5 C28 156.2(9) . . . . ? O7 Cd2 N5 C28 103.9(9) . . . . ? O9 Cd2 N5 C28 5.3(9) 2_655 . . . ? C41 Cd2 N5 C28 130.4(9) . . . . ? C40 Cd2 N5 C28 18.0(10) 2_655 . . . ? N7 Cd2 N5 C30 96.9(8) . . . . ? O10 Cd2 N5 C30 -123.7(7) 2_655 . . . ? O8 Cd2 N5 C30 -4.9(8) . . . . ? O7 Cd2 N5 C30 -57.3(8) . . . . ? O9 Cd2 N5 C30 -155.8(8) 2_655 . . . ? C41 Cd2 N5 C30 -30.7(8) . . . . ? C40 Cd2 N5 C30 -143.1(8) 2_655 . . . ? O10 Cd2 N7 C33 89.9(8) 2_655 . . . ? N5 Cd2 N7 C33 -126.5(8) . . . . ? O8 Cd2 N7 C33 -29.3(8) . . . . ? O7 Cd2 N7 C33 -66.6(10) . . . . ? O9 Cd2 N7 C33 147.8(7) 2_655 . . . ? C41 Cd2 N7 C33 -43.6(9) . . . . ? C40 Cd2 N7 C33 121.2(7) 2_655 . . . ? O10 Cd2 N7 C31 -95.9(8) 2_655 . . . ? N5 Cd2 N7 C31 47.8(8) . . . . ? O8 Cd2 N7 C31 144.9(7) . . . . ? O7 Cd2 N7 C31 107.6(8) . . . . ? O9 Cd2 N7 C31 -37.9(8) 2_655 . . . ? C41 Cd2 N7 C31 130.7(7) . . . . ? C40 Cd2 N7 C31 -64.6(8) 2_655 . . . ? O1 Cd1 N10 C48 153.6(7) 1_656 . . . ? N11 Cd1 N10 C48 -83.4(7) . . . . ? O5 Cd1 N10 C48 62.5(7) 4_666 . . . ? O6 Cd1 N10 C48 7.5(7) 4_666 . . . ? C20 Cd1 N10 C48 34.9(7) 4_666 . . . ? O1 Cd1 N10 C50 -16.0(9) 1_656 . . . ? N11 Cd1 N10 C50 107.0(8) . . . . ? O5 Cd1 N10 C50 -107.2(8) 4_666 . . . ? O6 Cd1 N10 C50 -162.2(8) 4_666 . . . ? C20 Cd1 N10 C50 -134.7(8) 4_666 . . . ? O1 Cd1 N11 C53 -11.1(8) 1_656 . . . ? N10 Cd1 N11 C53 -136.7(7) . . . . ? O5 Cd1 N11 C53 110.7(7) 4_666 . . . ? O6 Cd1 N11 C53 135.0(7) 4_666 . . . ? C20 Cd1 N11 C53 125.0(7) 4_666 . . . ? O1 Cd1 N11 C51 172.7(7) 1_656 . . . ? N10 Cd1 N11 C51 47.1(8) . . . . ? O5 Cd1 N11 C51 -65.5(9) 4_666 . . . ? O6 Cd1 N11 C51 -41.2(8) 4_666 . . . ? C20 Cd1 N11 C51 -51.2(8) 4_666 . . . ? C3 N1 C1 C2 0.9(11) . . . . ? Cd3 N1 C1 C2 -173.9(6) . . . . ? N1 C1 C2 N2 0.1(11) . . . . ? C3 N2 C2 C1 -0.9(10) . . . . ? C4 N2 C2 C1 -177.5(8) . . . . ? C1 N1 C3 N2 -1.5(10) . . . . ? Cd3 N1 C3 N2 172.2(6) . . . . ? C2 N2 C3 N1 1.6(10) . . . . ? C4 N2 C3 N1 178.1(8) . . . . ? C3 N2 C4 C5 -61.0(13) . . . . ? C2 N2 C4 C5 114.8(11) . . . . ? C3 N2 C4 C9 119.3(10) . . . . ? C2 N2 C4 C9 -64.8(13) . . . . ? C9 C4 C5 C6 -0.4(15) . . . . ? N2 C4 C5 C6 180.0(8) . . . . ? C4 C5 C6 C7 1.4(14) . . . . ? C4 C5 C6 C10 -178.2(9) . . . . ? C5 C6 C7 C8 -0.8(15) . . . . ? C10 C6 C7 C8 178.8(9) . . . . ? C6 C7 C8 C9 -0.9(15) . . . . ? C7 C8 C9 C4 2.0(15) . . . . ? C5 C4 C9 C8 -1.4(15) . . . . ? N2 C4 C9 C8 178.3(9) . . . . ? Cd1 O1 C10 O2 6.2(12) 1_454 . . . ? Cd1 O1 C10 C6 -175.0(7) 1_454 . . . ? C5 C6 C10 O2 172.0(9) . . . . ? C7 C6 C10 O2 -7.6(14) . . . . ? C5 C6 C10 O1 -6.8(14) . . . . ? C7 C6 C10 O1 173.6(9) . . . . ? C12 N3 C11 N4 -0.7(11) . . . . ? Cd3 N3 C11 N4 169.4(6) . . . . ? C13 N4 C11 N3 0.9(11) . . . . ? C14 N4 C11 N3 178.0(9) . . . . ? C11 N3 C12 C13 0.2(11) . . . . ? Cd3 N3 C12 C13 -170.1(7) . . . . ? N3 C12 C13 N4 0.4(12) . . . . ? C11 N4 C13 C12 -0.8(11) . . . . ? C14 N4 C13 C12 -177.8(9) . . . . ? C11 N4 C14 C15 139.8(10) . . . . ? C13 N4 C14 C15 -43.8(14) . . . . ? C11 N4 C14 C19 -42.9(14) . . . . ? C13 N4 C14 C19 133.6(10) . . . . ? C19 C14 C15 C16 -0.9(14) . . . . ? N4 C14 C15 C16 176.3(8) . . . . ? C14 C15 C16 C17 3.1(14) . . . . ? C14 C15 C16 C20 -176.3(8) . . . . ? C15 C16 C17 C18 -3.7(15) . . . . ? C20 C16 C17 C18 175.7(9) . . . . ? C16 C17 C18 C19 2.0(15) . . . . ? C15 C14 C19 C18 -0.7(15) . . . . ? N4 C14 C19 C18 -178.0(9) . . . . ? C17 C18 C19 C14 0.2(15) . . . . ? Cd1 O6 C20 O5 3.1(9) 4_465 . . . ? Cd1 O6 C20 C16 -177.0(8) 4_465 . . . ? Cd1 O5 C20 O6 -3.4(10) 4_465 . . . ? Cd1 O5 C20 C16 176.7(7) 4_465 . . . ? C15 C16 C20 O6 16.2(13) . . . . ? C17 C16 C20 O6 -163.2(9) . . . . ? C15 C16 C20 O5 -163.8(9) . . . . ? C17 C16 C20 O5 16.8(13) . . . . ? Cd3 O3 C21 O4 10.0(10) . . . . ? Cd3 O3 C21 C22 -168.5(7) . . . . ? Cd3 O4 C21 O3 -9.4(10) . . . . ? Cd3 O4 C21 C22 169.1(8) . . . . ? O3 C21 C22 C23 -178.4(9) . . . . ? O4 C21 C22 C23 3.1(14) . . . . ? O3 C21 C22 C27 2.2(14) . . . . ? O4 C21 C22 C27 -176.4(9) . . . . ? C27 C22 C23 C24 1.9(14) . . . . ? C21 C22 C23 C24 -177.5(9) . . . . ? C22 C23 C24 C25 -1.1(14) . . . . ? C22 C23 C24 N6 176.9(8) . . . . ? C28 N6 C24 C25 177.3(9) . . . . ? C29 N6 C24 C25 -3.8(14) . . . . ? C28 N6 C24 C23 -0.8(15) . . . . ? C29 N6 C24 C23 178.1(9) . . . . ? C23 C24 C25 C26 -0.5(14) . . . . ? N6 C24 C25 C26 -178.6(8) . . . . ? C24 C25 C26 C27 1.3(14) . . . . ? C25 C26 C27 C22 -0.5(14) . . . . ? C23 C22 C27 C26 -1.1(14) . . . . ? C21 C22 C27 C26 178.4(9) . . . . ? C30 N5 C28 N6 0.5(12) . . . . ? Cd2 N5 C28 N6 -163.3(6) . . . . ? C29 N6 C28 N5 -0.3(12) . . . . ? C24 N6 C28 N5 178.8(9) . . . . ? C28 N6 C29 C30 -0.1(11) . . . . ? C24 N6 C29 C30 -179.1(9) . . . . ? N6 C29 C30 N5 0.4(12) . . . . ? C28 N5 C30 C29 -0.5(12) . . . . ? Cd2 N5 C30 C29 164.4(7) . . . . ? C33 N7 C31 C32 -0.2(11) . . . . ? Cd2 N7 C31 C32 -175.3(6) . . . . ? N7 C31 C32 N8 -0.9(11) . . . . ? C33 N8 C32 C31 1.6(10) . . . . ? C34 N8 C32 C31 170.0(9) . . . . ? C31 N7 C33 N8 1.3(11) . . . . ? Cd2 N7 C33 N8 176.6(6) . . . . ? C32 N8 C33 N7 -1.9(11) . . . . ? C34 N8 C33 N7 -170.6(8) . . . . ? C33 N8 C34 C39 -41.7(14) . . . . ? C32 N8 C34 C39 151.7(9) . . . . ? C33 N8 C34 C35 135.8(9) . . . . ? C32 N8 C34 C35 -30.8(14) . . . . ? C39 C34 C35 C36 4.6(14) . . . . ? N8 C34 C35 C36 -172.8(8) . . . . ? C34 C35 C36 C37 -2.8(14) . . . . ? C34 C35 C36 C40 174.0(8) . . . . ? C35 C36 C37 C38 -0.3(15) . . . . ? C40 C36 C37 C38 -176.9(9) . . . . ? C36 C37 C38 C39 1.7(15) . . . . ? C35 C34 C39 C38 -3.3(14) . . . . ? N8 C34 C39 C38 174.1(9) . . . . ? C37 C38 C39 C34 0.1(15) . . . . ? Cd2 O9 C40 O10 -3.3(9) 2_645 . . . ? Cd2 O9 C40 C36 172.7(8) 2_645 . . . ? Cd2 O10 C40 O9 3.7(10) 2_645 . . . ? Cd2 O10 C40 C36 -172.4(7) 2_645 . . . ? C37 C36 C40 O9 28.7(14) . . . . ? C35 C36 C40 O9 -148.0(9) . . . . ? C37 C36 C40 O10 -155.2(9) . . . . ? C35 C36 C40 O10 28.1(13) . . . . ? Cd2 O7 C41 O8 6.3(9) . . . . ? Cd2 O7 C41 C42 -173.9(7) . . . . ? Cd2 O8 C41 O7 -6.5(9) . . . . ? Cd2 O8 C41 C42 173.7(7) . . . . ? N7 Cd2 C41 O7 -155.2(5) . . . . ? O10 Cd2 C41 O7 60.6(5) 2_655 . . . ? N5 Cd2 C41 O7 -72.2(5) . . . . ? O8 Cd2 C41 O7 174.0(9) . . . . ? O9 Cd2 C41 O7 11.5(6) 2_655 . . . ? C40 Cd2 C41 O7 39.2(6) 2_655 . . . ? N7 Cd2 C41 O8 30.9(6) . . . . ? O10 Cd2 C41 O8 -113.3(5) 2_655 . . . ? N5 Cd2 C41 O8 113.8(5) . . . . ? O7 Cd2 C41 O8 -174.0(9) . . . . ? O9 Cd2 C41 O8 -162.4(5) 2_655 . . . ? C40 Cd2 C41 O8 -134.8(5) 2_655 . . . ? O7 C41 C42 C47 -167.6(8) . . . . ? O8 C41 C42 C47 12.2(13) . . . . ? O7 C41 C42 C43 14.4(12) . . . . ? O8 C41 C42 C43 -165.7(8) . . . . ? C47 C42 C43 C44 -0.9(14) . . . . ? C41 C42 C43 C44 177.0(8) . . . . ? C42 C43 C44 C45 2.0(14) . . . . ? C43 C44 C45 C46 -0.6(14) . . . . ? C44 C45 C46 C47 -1.9(14) . . . . ? C44 C45 C46 N9 176.8(9) . . . . ? C48 N9 C46 C45 -143.2(9) . . . . ? C49 N9 C46 C45 31.5(14) . . . . ? C48 N9 C46 C47 35.6(13) . . . . ? C49 N9 C46 C47 -149.8(9) . . . . ? C43 C42 C47 C46 -1.5(13) . . . . ? C41 C42 C47 C46 -179.4(8) . . . . ? C45 C46 C47 C42 3.0(14) . . . . ? N9 C46 C47 C42 -175.8(8) . . . . ? C50 N10 C48 N9 0.5(10) . . . . ? Cd1 N10 C48 N9 -171.3(6) . . . . ? C49 N9 C48 N10 0.5(11) . . . . ? C46 N9 C48 N10 176.0(8) . . . . ? C48 N9 C49 C50 -1.2(11) . . . . ? C46 N9 C49 C50 -176.7(9) . . . . ? N9 C49 C50 N10 1.6(11) . . . . ? C48 N10 C50 C49 -1.3(11) . . . . ? Cd1 N10 C50 C49 169.8(7) . . . . ? C53 N11 C51 C52 0.5(10) . . . . ? Cd1 N11 C51 C52 177.3(6) . . . . ? N11 C51 C52 N12 -0.7(10) . . . . ? C53 N12 C52 C51 0.6(10) . . . . ? C54 N12 C52 C51 -178.9(8) . . . . ? C51 N11 C53 N12 -0.2(10) . . . . ? Cd1 N11 C53 N12 -177.1(5) . . . . ? C52 N12 C53 N11 -0.2(10) . . . . ? C54 N12 C53 N11 179.2(8) . . . . ? C53 N12 C54 C55 -36.3(13) . . . . ? C52 N12 C54 C55 143.0(9) . . . . ? C53 N12 C54 C59 141.5(9) . . . . ? C52 N12 C54 C59 -39.1(13) . . . . ? C59 C54 C55 C56 -2.4(15) . . . . ? N12 C54 C55 C56 175.4(9) . . . . ? C54 C55 C56 C57 0.7(15) . . . . ? C55 C56 C57 C58 1.4(15) . . . . ? C56 C57 C58 C59 -1.7(15) . . . . ? C56 C57 C58 C60 -179.4(9) . . . . ? C57 C58 C59 C54 0.0(14) . . . . ? C60 C58 C59 C54 177.6(9) . . . . ? C55 C54 C59 C58 2.1(14) . . . . ? N12 C54 C59 C58 -175.6(8) . . . . ? Cd3 O11 C60 O12 -10.9(10) 2_645 . . . ? Cd3 O11 C60 C58 165.8(9) 2_645 . . . ? Cd3 O12 C60 O11 11.7(11) 2_645 . . . ? Cd3 O12 C60 C58 -165.0(8) 2_645 . . . ? C59 C58 C60 O11 18.1(15) . . . . ? C57 C58 C60 O11 -164.2(10) . . . . ? C59 C58 C60 O12 -165.2(10) . . . . ? C57 C58 C60 O12 12.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.306 _refine_diff_density_min -1.777 _refine_diff_density_rms 0.174