# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #=========================================================== data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 872129' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H28.50 Cd N8 O10.25' _chemical_formula_sum 'C23 H28.50 Cd N8 O10.25' _chemical_formula_weight 693.44 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 8.0773(3) _cell_length_b 21.0490(7) _cell_length_c 34.7351(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5905.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4602 _cell_measurement_theta_min 3.0817 _cell_measurement_theta_max 29.2436 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97753 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22059 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5208 _reflns_number_gt 3554 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For O4W, O5W, O6W and O7W, some anisotropic displacement ellipsoids were rather elongated, which led us to use the ISOR restraints. ; _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^)+(0.0570P)^2^+9.5666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5208 _refine_ls_number_parameters 397 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.067 _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 Cd1 Cd 0.19551(5) 0.161065(17) 0.528326(12) 0.03896(17) Uani 1 1 d . . . C1 C 0.3836(9) 0.5155(3) 0.54766(18) 0.0563(17) Uani 1 1 d . . . H1 H 0.3276 0.5113 0.5244 0.068 Uiso 1 1 calc R . . C2 C 0.4397(8) 0.4615(3) 0.56516(18) 0.0539(17) Uani 1 1 d . . . H2 H 0.4246 0.4221 0.5536 0.065 Uiso 1 1 calc R . . C3 C 0.5184(7) 0.4662(2) 0.59990(16) 0.0379(13) Uani 1 1 d . . . C4 C 0.5419(8) 0.5258(3) 0.61494(18) 0.0539(17) Uani 1 1 d . . . H4 H 0.5966 0.5311 0.6383 0.065 Uiso 1 1 calc R . . C5 C 0.4841(8) 0.5774(3) 0.59517(18) 0.0511(16) Uani 1 1 d . . . H5 H 0.5018 0.6174 0.6057 0.061 Uiso 1 1 calc R . . C6 C 0.5775(7) 0.4086(3) 0.61980(17) 0.0405(14) Uani 1 1 d . . . C7 C 0.6587(7) 0.3462(3) 0.66313(17) 0.0434(14) Uani 1 1 d . . . C8 C 0.7021(8) 0.3191(3) 0.70083(18) 0.0546(17) Uani 1 1 d . . . C9 C 0.7645(12) 0.3588(4) 0.7287(2) 0.089(3) Uani 1 1 d . . . H9 H 0.7802 0.4018 0.7238 0.107 Uiso 1 1 calc R . . C10 C 0.8035(13) 0.3325(5) 0.7644(2) 0.107(4) Uani 1 1 d . . . H10 H 0.8464 0.3594 0.7831 0.128 Uiso 1 1 calc R . . C11 C 0.7239(12) 0.2359(5) 0.7466(3) 0.091(3) Uani 1 1 d . . . H11 H 0.7100 0.1931 0.7523 0.109 Uiso 1 1 calc R . . C12 C 0.6792(9) 0.2563(4) 0.7102(2) 0.070(2) Uani 1 1 d . . . H12 H 0.6345 0.2280 0.6924 0.084 Uiso 1 1 calc R . . C13 C 0.7411(7) 0.2573(3) 0.61590(19) 0.0450(15) Uani 1 1 d . . . H13A H 0.8180 0.2664 0.5952 0.054 Uiso 1 1 calc R . . H13B H 0.8034 0.2390 0.6370 0.054 Uiso 1 1 calc R . . C14 C 0.5517(8) 0.2061(3) 0.56837(18) 0.0478(15) Uani 1 1 d . . . H14 H 0.5823 0.2298 0.5469 0.057 Uiso 1 1 calc R . . C15 C 0.4375(9) 0.1429(3) 0.6050(2) 0.0621(19) Uani 1 1 d . . . H15 H 0.3681 0.1108 0.6138 0.074 Uiso 1 1 calc R . . C16 C 0.3842(7) 0.1291(3) 0.46494(16) 0.0390(13) Uani 1 1 d . . . C17 C 0.6287(7) 0.2248(2) 0.43481(17) 0.0378(13) Uani 1 1 d . . . C18 C 0.5980(6) 0.1622(2) 0.41556(15) 0.0344(12) Uani 1 1 d . . . C19 C 0.4895(7) 0.1165(2) 0.43049(15) 0.0343(12) Uani 1 1 d . . . C20 C 0.4684(7) 0.0595(2) 0.41057(18) 0.0458(15) Uani 1 1 d . . . H20 H 0.3968 0.0287 0.4202 0.055 Uiso 1 1 calc R . . C21 C 0.5525(8) 0.0483(3) 0.37682(18) 0.0521(16) Uani 1 1 d . . . H21 H 0.5368 0.0102 0.3637 0.062 Uiso 1 1 calc R . . C22 C 0.6586(8) 0.0927(3) 0.36249(19) 0.0540(17) Uani 1 1 d . . . H22 H 0.7162 0.0846 0.3398 0.065 Uiso 1 1 calc R . . C23 C 0.6809(7) 0.1496(3) 0.38151(17) 0.0435(14) Uani 1 1 d . . . H23 H 0.7524 0.1799 0.3713 0.052 Uiso 1 1 calc R . . N1 N 0.4043(6) 0.5738(2) 0.56189(13) 0.0407(11) Uani 1 1 d . . . N2 N 0.6053(6) 0.4048(2) 0.65801(14) 0.0471(12) Uani 1 1 d . . . N3 N 0.6120(6) 0.3566(2) 0.60055(13) 0.0409(11) Uani 1 1 d . . . N4 N 0.6649(6) 0.3165(2) 0.62865(14) 0.0412(11) Uani 1 1 d . . . N5 N 0.7835(10) 0.2720(5) 0.7734(2) 0.094(2) Uani 1 1 d . . . N6 N 0.6195(6) 0.2120(2) 0.60271(14) 0.0405(11) Uani 1 1 d . . . N7 N 0.5430(7) 0.1717(3) 0.62756(16) 0.0664(16) Uani 1 1 d . . . N8 N 0.4362(6) 0.1627(2) 0.56831(15) 0.0482(12) Uani 1 1 d . . . O1 O 0.3392(5) 0.18458(19) 0.47210(11) 0.0475(10) Uani 1 1 d . . . O2 O 0.3389(6) 0.0835(2) 0.48562(14) 0.0661(13) Uani 1 1 d . . . O3 O 0.6904(5) 0.22662(18) 0.46814(12) 0.0506(11) Uani 1 1 d . . . O4 O 0.5988(5) 0.27434(17) 0.41610(12) 0.0488(10) Uani 1 1 d . . . O1W O 0.3185(7) -0.0579(3) 0.47426(16) 0.0903(17) Uani 1 1 d . . . H1A H 0.4167 -0.0730 0.4719 0.135 Uiso 1 1 d R . . H1B H 0.3279 -0.0192 0.4805 0.135 Uiso 1 1 d R . . O2W O -0.0789(6) 0.1550(2) 0.50584(17) 0.0872(17) Uani 1 1 d . . . H2A H -0.1465 0.1815 0.4952 0.131 Uiso 1 1 d R . . H2B H -0.0899 0.1201 0.4935 0.131 Uiso 1 1 d R . . O3W O 0.9213(7) 0.2029(2) 0.83591(14) 0.0861(17) Uani 1 1 d . . . H3A H 0.8766 0.2257 0.8186 0.129 Uiso 1 1 d R . . H3B H 0.9746 0.1734 0.8247 0.129 Uiso 1 1 d R . . O4W O 0.4367(11) 0.4870(3) 0.71316(19) 0.143(3) Uani 1 1 d U . . H4B H 0.5449 0.5115 0.7080 0.214 Uiso 1 1 d R . . H4A H 0.4422 0.4488 0.7047 0.214 Uiso 1 1 d R . . O5W O 0.7368(16) 0.0834(6) 0.8137(4) 0.244(6) Uani 1 1 d U . . H5A H 0.8364 0.0890 0.8065 0.366 Uiso 1 1 d R . . H5B H 0.6942 0.0555 0.7991 0.366 Uiso 1 1 d R . . O6W O 1.0836(18) 0.1112(5) 0.7936(4) 0.121(4) Uani 0.50 1 d PU . . H6A H 1.0836 0.0966 0.7727 0.181 Uiso 0.50 1 d PR . . H6B H 1.1905 0.0946 0.8034 0.181 Uiso 0.50 1 d PR . . O7W O 1.396(3) 0.0693(9) 0.7993(6) 0.194(8) Uani 0.50 1 d PU . . H7A H 1.4785 0.0850 0.8105 0.292 Uiso 0.50 1 d PR . . H7B H 1.3894 0.0845 0.7768 0.292 Uiso 0.50 1 d PR . . O8W O 1.589(4) -0.0020(11) 0.7717(7) 0.123(10) Uani 0.25 1 d P . . H8A H 1.4984 0.0124 0.7750 0.184 Uiso 0.25 1 d PR . . H8B H 1.5727 -0.0335 0.7529 0.184 Uiso 0.25 1 d PR . . 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 0.0525(3) 0.0317(2) 0.0327(3) 0.00136(18) 0.0058(2) 0.00362(18) C1 0.088(5) 0.044(4) 0.036(4) -0.002(3) -0.019(4) 0.002(3) C2 0.080(5) 0.033(3) 0.049(4) -0.004(3) -0.013(4) 0.005(3) C3 0.041(3) 0.035(3) 0.037(3) 0.002(2) 0.002(3) 0.006(2) C4 0.071(4) 0.048(4) 0.043(4) -0.007(3) -0.017(3) 0.013(3) C5 0.075(4) 0.035(3) 0.043(4) -0.008(3) -0.012(3) 0.004(3) C6 0.041(3) 0.036(3) 0.045(4) 0.002(3) -0.002(3) 0.008(3) C7 0.051(4) 0.046(3) 0.034(3) -0.002(3) -0.007(3) 0.009(3) C8 0.061(4) 0.065(4) 0.038(4) 0.002(3) -0.003(3) 0.022(3) C9 0.139(8) 0.077(5) 0.050(5) -0.016(4) -0.028(5) 0.029(5) C10 0.151(10) 0.123(9) 0.047(5) -0.030(5) -0.033(5) 0.040(7) C11 0.114(7) 0.096(6) 0.062(6) 0.028(5) -0.005(5) 0.015(5) C12 0.092(6) 0.071(5) 0.045(4) 0.008(4) -0.011(4) 0.009(4) C13 0.044(3) 0.040(3) 0.051(4) 0.001(3) 0.001(3) 0.006(3) C14 0.055(4) 0.055(4) 0.033(4) 0.010(3) 0.003(3) 0.005(3) C15 0.073(5) 0.053(4) 0.061(5) 0.023(3) -0.015(4) -0.017(3) C16 0.047(3) 0.038(3) 0.032(3) -0.003(3) -0.001(3) -0.001(3) C17 0.038(3) 0.034(3) 0.042(4) -0.004(3) -0.005(3) -0.002(2) C18 0.040(3) 0.032(3) 0.031(3) 0.000(2) -0.008(3) 0.004(2) C19 0.041(3) 0.031(3) 0.031(3) 0.000(2) 0.002(3) 0.007(2) C20 0.053(4) 0.032(3) 0.053(4) -0.003(3) 0.001(3) -0.002(3) C21 0.066(4) 0.043(3) 0.047(4) -0.013(3) 0.000(3) 0.003(3) C22 0.066(4) 0.059(4) 0.037(4) -0.003(3) 0.009(3) 0.014(3) C23 0.048(4) 0.043(3) 0.040(4) 0.006(3) 0.008(3) 0.002(3) N1 0.051(3) 0.035(2) 0.036(3) 0.000(2) 0.001(2) 0.003(2) N2 0.058(3) 0.046(3) 0.037(3) -0.001(2) -0.008(3) 0.007(2) N3 0.044(3) 0.038(3) 0.040(3) 0.004(2) -0.001(2) 0.004(2) N4 0.043(3) 0.038(2) 0.043(3) 0.004(2) -0.001(2) 0.004(2) N5 0.123(6) 0.114(6) 0.046(4) 0.009(4) -0.010(4) 0.044(5) N6 0.044(3) 0.036(2) 0.042(3) 0.005(2) 0.002(2) 0.004(2) N7 0.079(4) 0.067(4) 0.053(4) 0.023(3) -0.015(3) -0.027(3) N8 0.055(3) 0.043(3) 0.047(3) 0.007(2) -0.002(2) -0.001(2) O1 0.062(3) 0.041(2) 0.039(2) -0.0067(18) 0.004(2) 0.0076(19) O2 0.090(3) 0.050(3) 0.058(3) 0.013(2) 0.032(3) 0.002(2) O3 0.065(3) 0.043(2) 0.044(3) -0.0034(19) -0.018(2) -0.0045(19) O4 0.062(3) 0.033(2) 0.052(3) 0.0017(19) -0.013(2) -0.0014(19) O1W 0.085(4) 0.072(3) 0.114(5) 0.002(3) 0.012(3) 0.011(3) O2W 0.082(4) 0.076(3) 0.104(4) 0.002(3) -0.034(3) 0.019(3) O3W 0.118(5) 0.087(4) 0.054(3) 0.003(3) -0.013(3) 0.035(3) O4W 0.199(7) 0.131(5) 0.099(5) -0.016(4) -0.001(5) 0.048(5) O5W 0.265(9) 0.231(9) 0.237(9) -0.012(7) -0.004(7) 0.021(8) O6W 0.167(9) 0.080(6) 0.115(8) -0.007(6) 0.037(7) 0.003(6) O7W 0.202(11) 0.197(11) 0.184(11) -0.008(9) -0.037(9) -0.006(9) O8W 0.15(3) 0.11(2) 0.11(2) 0.051(16) 0.016(18) 0.012(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.319(4) 7_655 ? Cd1 O1 2.325(4) . ? Cd1 O2W 2.354(5) . ? Cd1 O3 2.368(4) 3_456 ? Cd1 N8 2.389(5) . ? Cd1 O4 2.487(4) 3_456 ? Cd1 O2 2.492(4) . ? C1 N1 1.335(7) . ? C1 C2 1.365(8) . ? C1 H1 0.9300 . ? C2 C3 1.367(8) . ? C2 H2 0.9300 . ? C3 C4 1.373(8) . ? C3 C6 1.476(7) . ? C4 C5 1.367(8) . ? C4 H4 0.9300 . ? C5 N1 1.326(7) . ? C5 H5 0.9300 . ? C6 N3 1.312(7) . ? C6 N2 1.348(7) . ? C7 N2 1.319(7) . ? C7 N4 1.352(7) . ? C7 C8 1.471(8) . ? C8 C12 1.374(9) . ? C8 C9 1.374(10) . ? C9 C10 1.394(12) . ? C9 H9 0.9300 . ? C10 N5 1.322(12) . ? C10 H10 0.9300 . ? C11 N5 1.292(11) . ? C11 C12 1.383(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N6 1.444(7) . ? C13 N4 1.457(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N8 1.305(7) . ? C14 N6 1.318(7) . ? C14 H14 0.9300 . ? C15 N7 1.307(8) . ? C15 N8 1.341(8) . ? C15 H15 0.9300 . ? C16 O1 1.247(7) . ? C16 O2 1.255(7) . ? C16 C19 1.492(7) . ? C17 O4 1.252(6) . ? C17 O3 1.261(6) . ? C17 C18 1.499(7) . ? C18 C23 1.385(8) . ? C18 C19 1.401(7) . ? C19 C20 1.396(7) . ? C20 C21 1.375(8) . ? C20 H20 0.9300 . ? C21 C22 1.362(9) . ? C21 H21 0.9300 . ? C22 C23 1.380(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? N1 Cd1 2.319(4) 7_665 ? N3 N4 1.360(6) . ? N6 N7 1.359(7) . ? O3 Cd1 2.368(4) 3_556 ? O4 Cd1 2.487(4) 3_556 ? O1W H1A 0.8586 . ? O1W H1B 0.8446 . ? O2W H2A 0.8618 . ? O2W H2B 0.8575 . ? O3W H3A 0.8500 . ? O3W H3B 0.8500 . ? O4W H4B 1.0304 . ? O4W H4A 0.8573 . ? O5W H5A 0.8500 . ? O5W H5B 0.8499 . ? O6W H6A 0.7883 . ? O6W H6B 0.9922 . ? O7W H7A 0.8375 . ? O7W H7B 0.8470 . ? O8W H8A 0.8043 . ? O8W H8B 0.9385 . ? 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 O1 139.83(15) 7_655 . ? N1 Cd1 O2W 78.28(18) 7_655 . ? O1 Cd1 O2W 101.71(18) . . ? N1 Cd1 O3 139.31(15) 7_655 3_456 ? O1 Cd1 O3 80.77(14) . 3_456 ? O2W Cd1 O3 93.12(16) . 3_456 ? N1 Cd1 N8 90.12(16) 7_655 . ? O1 Cd1 N8 94.53(16) . . ? O2W Cd1 N8 163.72(19) . . ? O3 Cd1 N8 88.25(15) 3_456 . ? N1 Cd1 O4 86.18(14) 7_655 3_456 ? O1 Cd1 O4 133.82(13) . 3_456 ? O2W Cd1 O4 89.49(17) . 3_456 ? O3 Cd1 O4 53.73(13) 3_456 3_456 ? N8 Cd1 O4 78.25(16) . 3_456 ? N1 Cd1 O2 86.66(15) 7_655 . ? O1 Cd1 O2 53.67(13) . . ? O2W Cd1 O2 101.82(19) . . ? O3 Cd1 O2 133.91(14) 3_456 . ? N8 Cd1 O2 88.72(17) . . ? O4 Cd1 O2 165.10(15) 3_456 . ? N1 C1 C2 124.0(6) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 119.2(5) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 117.8(5) . . ? C2 C3 C6 120.3(5) . . ? C4 C3 C6 121.9(5) . . ? C5 C4 C3 119.2(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 124.0(5) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N3 C6 N2 114.6(5) . . ? N3 C6 C3 121.0(5) . . ? N2 C6 C3 124.3(5) . . ? N2 C7 N4 109.0(5) . . ? N2 C7 C8 124.1(5) . . ? N4 C7 C8 126.9(5) . . ? C12 C8 C9 117.9(7) . . ? C12 C8 C7 123.5(6) . . ? C9 C8 C7 118.5(7) . . ? C8 C9 C10 117.9(9) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N5 C10 C9 124.4(8) . . ? N5 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N5 C11 C12 124.9(9) . . ? N5 C11 H11 117.5 . . ? C12 C11 H11 117.5 . . ? C8 C12 C11 118.7(8) . . ? C8 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? N6 C13 N4 111.9(5) . . ? N6 C13 H13A 109.2 . . ? N4 C13 H13A 109.2 . . ? N6 C13 H13B 109.2 . . ? N4 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N8 C14 N6 111.4(5) . . ? N8 C14 H14 124.3 . . ? N6 C14 H14 124.3 . . ? N7 C15 N8 115.5(6) . . ? N7 C15 H15 122.2 . . ? N8 C15 H15 122.2 . . ? O1 C16 O2 121.2(5) . . ? O1 C16 C19 119.5(5) . . ? O2 C16 C19 119.2(5) . . ? O4 C17 O3 121.8(5) . . ? O4 C17 C18 118.0(5) . . ? O3 C17 C18 120.1(5) . . ? C23 C18 C19 119.2(5) . . ? C23 C18 C17 118.0(5) . . ? C19 C18 C17 122.8(5) . . ? C20 C19 C18 118.9(5) . . ? C20 C19 C16 118.8(5) . . ? C18 C19 C16 122.1(5) . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.3(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.8(5) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C5 N1 C1 115.8(5) . . ? C5 N1 Cd1 124.2(4) . 7_665 ? C1 N1 Cd1 119.9(4) . 7_665 ? C7 N2 C6 104.1(5) . . ? C6 N3 N4 102.7(5) . . ? C7 N4 N3 109.7(4) . . ? C7 N4 C13 132.8(5) . . ? N3 N4 C13 116.4(5) . . ? C11 N5 C10 116.2(7) . . ? C14 N6 N7 109.1(5) . . ? C14 N6 C13 129.2(5) . . ? N7 N6 C13 121.4(5) . . ? C15 N7 N6 101.9(5) . . ? C14 N8 C15 102.1(5) . . ? C14 N8 Cd1 126.4(4) . . ? C15 N8 Cd1 123.7(4) . . ? C16 O1 Cd1 96.5(3) . . ? C16 O2 Cd1 88.5(3) . . ? C17 O3 Cd1 94.9(3) . 3_556 ? C17 O4 Cd1 89.5(3) . 3_556 ? H1A O1W H1B 107.4 . . ? Cd1 O2W H2A 134.7 . . ? Cd1 O2W H2B 108.1 . . ? H2A O2W H2B 105.9 . . ? H3A O3W H3B 107.7 . . ? H4B O4W H4A 111.4 . . ? H5A O5W H5B 107.7 . . ? H6A O6W H6B 100.2 . . ? H7A O7W H7B 109.2 . . ? H8A O8W H8B 103.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.8(11) . . . . ? C1 C2 C3 C4 -2.1(10) . . . . ? C1 C2 C3 C6 178.9(6) . . . . ? C2 C3 C4 C5 1.1(9) . . . . ? C6 C3 C4 C5 -179.9(6) . . . . ? C3 C4 C5 N1 0.4(10) . . . . ? C2 C3 C6 N3 24.9(9) . . . . ? C4 C3 C6 N3 -154.1(6) . . . . ? C2 C3 C6 N2 -157.2(6) . . . . ? C4 C3 C6 N2 23.9(9) . . . . ? N2 C7 C8 C12 146.9(7) . . . . ? N4 C7 C8 C12 -32.6(10) . . . . ? N2 C7 C8 C9 -31.2(10) . . . . ? N4 C7 C8 C9 149.4(7) . . . . ? C12 C8 C9 C10 1.2(12) . . . . ? C7 C8 C9 C10 179.4(8) . . . . ? C8 C9 C10 N5 -0.4(16) . . . . ? C9 C8 C12 C11 -1.7(11) . . . . ? C7 C8 C12 C11 -179.8(7) . . . . ? N5 C11 C12 C8 1.5(14) . . . . ? O4 C17 C18 C23 58.2(7) . . . . ? O3 C17 C18 C23 -118.4(6) . . . . ? O4 C17 C18 C19 -121.6(6) . . . . ? O3 C17 C18 C19 61.8(7) . . . . ? C23 C18 C19 C20 0.1(8) . . . . ? C17 C18 C19 C20 179.9(5) . . . . ? C23 C18 C19 C16 -174.1(5) . . . . ? C17 C18 C19 C16 5.7(8) . . . . ? O1 C16 C19 C20 -145.8(5) . . . . ? O2 C16 C19 C20 32.4(8) . . . . ? O1 C16 C19 C18 28.5(8) . . . . ? O2 C16 C19 C18 -153.4(6) . . . . ? C18 C19 C20 C21 -0.1(8) . . . . ? C16 C19 C20 C21 174.3(5) . . . . ? C19 C20 C21 C22 0.4(9) . . . . ? C20 C21 C22 C23 -0.9(10) . . . . ? C21 C22 C23 C18 0.9(9) . . . . ? C19 C18 C23 C22 -0.6(8) . . . . ? C17 C18 C23 C22 179.7(5) . . . . ? C4 C5 N1 C1 -0.8(10) . . . . ? C4 C5 N1 Cd1 179.7(5) . . . 7_665 ? C2 C1 N1 C5 -0.3(10) . . . . ? C2 C1 N1 Cd1 179.2(6) . . . 7_665 ? N4 C7 N2 C6 0.9(7) . . . . ? C8 C7 N2 C6 -178.6(6) . . . . ? N3 C6 N2 C7 -0.8(7) . . . . ? C3 C6 N2 C7 -178.9(5) . . . . ? N2 C6 N3 N4 0.4(6) . . . . ? C3 C6 N3 N4 178.5(5) . . . . ? N2 C7 N4 N3 -0.8(7) . . . . ? C8 C7 N4 N3 178.7(6) . . . . ? N2 C7 N4 C13 166.7(6) . . . . ? C8 C7 N4 C13 -13.9(10) . . . . ? C6 N3 N4 C7 0.2(6) . . . . ? C6 N3 N4 C13 -169.5(5) . . . . ? N6 C13 N4 C7 116.9(7) . . . . ? N6 C13 N4 N3 -76.3(6) . . . . ? C12 C11 N5 C10 -0.6(15) . . . . ? C9 C10 N5 C11 0.1(16) . . . . ? N8 C14 N6 N7 -1.6(7) . . . . ? N8 C14 N6 C13 -174.7(5) . . . . ? N4 C13 N6 C14 85.6(7) . . . . ? N4 C13 N6 N7 -86.7(6) . . . . ? N8 C15 N7 N6 -2.1(8) . . . . ? C14 N6 N7 C15 2.2(7) . . . . ? C13 N6 N7 C15 175.8(5) . . . . ? N6 C14 N8 C15 0.3(7) . . . . ? N6 C14 N8 Cd1 149.9(4) . . . . ? N7 C15 N8 C14 1.2(8) . . . . ? N7 C15 N8 Cd1 -149.5(5) . . . . ? N1 Cd1 N8 C14 -173.3(5) 7_655 . . . ? O1 Cd1 N8 C14 46.6(5) . . . . ? O2W Cd1 N8 C14 -129.1(6) . . . . ? O3 Cd1 N8 C14 -34.0(5) 3_456 . . . ? O4 Cd1 N8 C14 -87.2(5) 3_456 . . . ? O2 Cd1 N8 C14 100.0(5) . . . . ? N1 Cd1 N8 C15 -29.8(5) 7_655 . . . ? O1 Cd1 N8 C15 -169.8(5) . . . . ? O2W Cd1 N8 C15 14.4(9) . . . . ? O3 Cd1 N8 C15 109.6(5) 3_456 . . . ? O4 Cd1 N8 C15 56.3(5) 3_456 . . . ? O2 Cd1 N8 C15 -116.4(5) . . . . ? O2 C16 O1 Cd1 3.4(6) . . . . ? C19 C16 O1 Cd1 -178.5(4) . . . . ? N1 Cd1 O1 C16 -12.3(4) 7_655 . . . ? O2W Cd1 O1 C16 -98.0(3) . . . . ? O3 Cd1 O1 C16 170.7(3) 3_456 . . . ? N8 Cd1 O1 C16 83.3(3) . . . . ? O4 Cd1 O1 C16 161.3(3) 3_456 . . . ? O2 Cd1 O1 C16 -1.8(3) . . . . ? O1 C16 O2 Cd1 -3.1(6) . . . . ? C19 C16 O2 Cd1 178.8(5) . . . . ? N1 Cd1 O2 C16 175.0(4) 7_655 . . . ? O1 Cd1 O2 C16 1.8(3) . . . . ? O2W Cd1 O2 C16 97.7(4) . . . . ? O3 Cd1 O2 C16 -8.5(5) 3_456 . . . ? N8 Cd1 O2 C16 -94.8(4) . . . . ? O4 Cd1 O2 C16 -123.6(5) 3_456 . . . ? O4 C17 O3 Cd1 2.1(6) . . . 3_556 ? C18 C17 O3 Cd1 178.6(4) . . . 3_556 ? O3 C17 O4 Cd1 -2.0(6) . . . 3_556 ? C18 C17 O4 Cd1 -178.6(5) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.842 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.090 #=========================================================== data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 872130' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H16 Cd N8 O4' _chemical_formula_sum 'C23 H16 Cd N8 O4' _chemical_formula_weight 580.84 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 _symmetry_space_group_name_hall '-P 2yn' 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 10.2045(3) _cell_length_b 16.3187(6) _cell_length_c 13.9348(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.700(3) _cell_angle_gamma 90.00 _cell_volume 2287.31(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2659 _cell_measurement_theta_min 2.8979 _cell_measurement_theta_max 29.0750 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7733 _exptl_absorpt_correction_T_max 0.8168 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8951 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4168 _reflns_number_gt 3126 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0243P)^2^+0.4716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4168 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 -0.08269(3) 0.100438(18) 0.49248(2) 0.03195(11) Uani 1 1 d . . . C1 C -0.3204(4) -0.2302(3) -0.0789(3) 0.0450(11) Uani 1 1 d . . . H1 H -0.2911 -0.2671 -0.1215 0.054 Uiso 1 1 calc R . . C2 C -0.2766(4) -0.1503(3) -0.0794(3) 0.0435(11) Uani 1 1 d . . . H2 H -0.2189 -0.1342 -0.1210 0.052 Uiso 1 1 calc R . . C3 C -0.3200(4) -0.0948(3) -0.0172(3) 0.0345(10) Uani 1 1 d . . . C4 C -0.4066(4) -0.1216(3) 0.0417(3) 0.0422(11) Uani 1 1 d . . . H4 H -0.4386 -0.0856 0.0840 0.051 Uiso 1 1 calc R . . C5 C -0.4451(4) -0.2021(3) 0.0373(3) 0.0421(10) Uani 1 1 d . . . H5 H -0.5045 -0.2191 0.0772 0.051 Uiso 1 1 calc R . . C6 C -0.2701(4) -0.0101(3) -0.0156(3) 0.0370(10) Uani 1 1 d . . . C7 C -0.1734(4) 0.0953(3) -0.0561(3) 0.0337(9) Uani 1 1 d . . . C8 C -0.0964(4) 0.1499(3) -0.1093(3) 0.0348(10) Uani 1 1 d . . . C9 C -0.0011(5) 0.1156(3) -0.1561(3) 0.0534(12) Uani 1 1 d . . . H9 H 0.0144 0.0594 -0.1534 0.064 Uiso 1 1 calc R . . C10 C 0.0710(5) 0.1664(4) -0.2071(4) 0.0659(15) Uani 1 1 d . . . H10 H 0.1336 0.1421 -0.2394 0.079 Uiso 1 1 calc R . . C11 C -0.0351(5) 0.2787(3) -0.1690(3) 0.0562(13) Uani 1 1 d . . . H11 H -0.0474 0.3351 -0.1723 0.067 Uiso 1 1 calc R . . C12 C -0.1156(4) 0.2337(3) -0.1177(3) 0.0433(11) Uani 1 1 d . . . H12 H -0.1810 0.2593 -0.0894 0.052 Uiso 1 1 calc R . . C13 C -0.2090(5) 0.1824(3) 0.0891(3) 0.0485(12) Uani 1 1 d . . . H13A H -0.1611 0.2252 0.0615 0.058 Uiso 1 1 calc R . . H13B H -0.2947 0.2040 0.0980 0.058 Uiso 1 1 calc R . . C14 C 0.0185(4) 0.1066(3) 0.2808(3) 0.0514(12) Uani 1 1 d . . . H14 H 0.0990 0.0829 0.3083 0.062 Uiso 1 1 calc R . . C15 C -0.1734(4) 0.1540(2) 0.2675(3) 0.0347(10) Uani 1 1 d . . . H15 H -0.2561 0.1709 0.2796 0.042 Uiso 1 1 calc R . . C16 C 0.2013(4) 0.0914(2) 0.5540(3) 0.0329(9) Uani 1 1 d . . . C17 C 0.6934(4) 0.0778(3) 0.5672(3) 0.0355(10) Uani 1 1 d . . . C18 C 0.5737(3) 0.0629(3) 0.6143(3) 0.0342(10) Uani 1 1 d . . . C19 C 0.5856(4) 0.0202(3) 0.7011(3) 0.0403(11) Uani 1 1 d . . . H19 H 0.6691 0.0032 0.7322 0.048 Uiso 1 1 calc R . . C20 C 0.4741(4) 0.0024(3) 0.7423(3) 0.0424(11) Uani 1 1 d . . . H20 H 0.4831 -0.0251 0.8015 0.051 Uiso 1 1 calc R . . C21 C 0.3504(4) 0.0257(2) 0.6952(3) 0.0363(10) Uani 1 1 d . . . H21 H 0.2755 0.0125 0.7219 0.044 Uiso 1 1 calc R . . C22 C 0.3361(3) 0.0689(2) 0.6081(3) 0.0309(9) Uani 1 1 d . . . C23 C 0.4487(4) 0.0870(2) 0.5685(3) 0.0333(10) Uani 1 1 d . . . H23 H 0.4400 0.1159 0.5102 0.040 Uiso 1 1 calc R . . N1 N -0.4025(3) -0.2577(2) -0.0208(2) 0.0395(8) Uani 1 1 d . . . N2 N -0.2000(3) 0.0181(2) -0.0831(2) 0.0368(8) Uani 1 1 d . . . N3 N -0.2908(3) 0.0445(2) 0.0509(2) 0.0420(9) Uani 1 1 d . . . N4 N -0.2279(3) 0.1121(2) 0.0234(2) 0.0389(8) Uani 1 1 d . . . N5 N 0.0579(4) 0.2471(3) -0.2137(3) 0.0590(11) Uani 1 1 d . . . N6 N -0.1348(3) 0.1569(2) 0.1819(2) 0.0377(8) Uani 1 1 d . . . N7 N -0.0099(4) 0.1259(3) 0.1888(3) 0.0597(12) Uani 1 1 d . . . N8 N -0.0785(3) 0.1238(2) 0.3329(2) 0.0349(8) Uani 1 1 d . . . O1 O 0.1049(2) 0.04543(17) 0.56944(19) 0.0380(7) Uani 1 1 d . . . O2 O 0.1858(2) 0.15139(18) 0.4995(2) 0.0443(7) Uani 1 1 d . . . O3 O 0.6798(2) 0.11066(19) 0.4856(2) 0.0432(7) Uani 1 1 d . . . O4 O 0.8057(2) 0.0560(2) 0.6129(2) 0.0502(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 Cd1 0.02855(16) 0.03223(18) 0.03631(17) 0.00329(14) 0.00901(12) 0.00569(14) C1 0.059(3) 0.035(3) 0.046(3) -0.006(2) 0.021(2) -0.002(2) C2 0.051(3) 0.038(3) 0.046(3) 0.003(2) 0.023(2) -0.007(2) C3 0.033(2) 0.032(2) 0.037(2) 0.008(2) 0.0054(18) -0.0002(19) C4 0.044(2) 0.034(3) 0.051(3) -0.002(2) 0.012(2) 0.003(2) C5 0.034(2) 0.042(3) 0.053(3) 0.003(2) 0.0149(19) -0.002(2) C6 0.038(2) 0.034(2) 0.038(2) 0.002(2) 0.0046(19) 0.002(2) C7 0.034(2) 0.033(2) 0.034(2) 0.003(2) 0.0051(18) 0.001(2) C8 0.037(2) 0.031(2) 0.036(2) -0.0028(19) 0.0036(18) -0.001(2) C9 0.061(3) 0.039(3) 0.064(3) -0.008(2) 0.020(2) -0.002(3) C10 0.059(3) 0.070(4) 0.077(4) -0.006(3) 0.035(3) -0.003(3) C11 0.076(3) 0.035(3) 0.062(3) -0.001(2) 0.023(3) -0.009(3) C12 0.051(3) 0.035(3) 0.047(3) 0.000(2) 0.019(2) 0.001(2) C13 0.075(3) 0.028(3) 0.041(2) -0.002(2) 0.005(2) 0.005(2) C14 0.036(2) 0.072(4) 0.047(3) 0.003(3) 0.011(2) 0.015(2) C15 0.033(2) 0.032(2) 0.041(2) -0.0034(19) 0.0120(18) 0.0066(19) C16 0.027(2) 0.026(2) 0.046(2) -0.012(2) 0.0041(18) 0.0020(19) C17 0.031(2) 0.036(3) 0.040(2) -0.010(2) 0.0085(18) -0.0018(19) C18 0.027(2) 0.041(3) 0.035(2) -0.009(2) 0.0079(17) 0.0019(19) C19 0.030(2) 0.050(3) 0.040(2) -0.005(2) 0.0025(18) 0.007(2) C20 0.037(2) 0.054(3) 0.036(2) 0.005(2) 0.0057(19) 0.005(2) C21 0.030(2) 0.038(3) 0.044(2) -0.008(2) 0.0152(18) -0.0007(19) C22 0.0233(19) 0.031(2) 0.040(2) -0.0017(19) 0.0071(16) 0.0006(18) C23 0.030(2) 0.035(3) 0.034(2) -0.0051(19) 0.0022(17) -0.0018(18) N1 0.040(2) 0.033(2) 0.047(2) 0.0019(17) 0.0144(17) -0.0011(17) N2 0.0428(19) 0.029(2) 0.0393(19) 0.0016(16) 0.0097(16) -0.0029(17) N3 0.053(2) 0.031(2) 0.045(2) 0.0044(17) 0.0154(17) 0.0031(18) N4 0.051(2) 0.029(2) 0.0365(19) -0.0001(16) 0.0080(16) -0.0006(17) N5 0.061(3) 0.057(3) 0.065(3) -0.004(2) 0.028(2) -0.017(2) N6 0.045(2) 0.036(2) 0.0336(19) 0.0015(16) 0.0095(16) 0.0066(17) N7 0.048(2) 0.090(4) 0.045(2) 0.009(2) 0.0215(18) 0.019(2) N8 0.0324(17) 0.037(2) 0.0367(19) 0.0013(16) 0.0103(15) 0.0047(16) O1 0.0217(13) 0.0364(17) 0.0567(18) -0.0020(14) 0.0086(12) -0.0035(13) O2 0.0349(16) 0.0341(18) 0.0623(19) 0.0046(16) 0.0039(14) 0.0004(14) O3 0.0336(15) 0.058(2) 0.0394(17) -0.0003(15) 0.0101(12) 0.0016(14) O4 0.0247(15) 0.073(2) 0.0551(18) 0.0058(17) 0.0119(13) 0.0081(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.220(2) . ? Cd1 N8 2.263(3) . ? Cd1 O4 2.299(3) 1_455 ? Cd1 N1 2.357(3) 2_455 ? Cd1 O3 2.415(2) 1_455 ? Cd1 O1 2.529(3) 3_556 ? Cd1 C17 2.692(4) 1_455 ? C1 N1 1.337(5) . ? C1 C2 1.379(6) . ? C1 H1 0.9300 . ? C2 C3 1.378(6) . ? C2 H2 0.9300 . ? C3 C4 1.375(5) . ? C3 C6 1.471(6) . ? C4 C5 1.370(6) . ? C4 H4 0.9300 . ? C5 N1 1.337(5) . ? C5 H5 0.9300 . ? C6 N3 1.329(5) . ? C6 N2 1.354(5) . ? C7 N2 1.329(5) . ? C7 N4 1.350(5) . ? C7 C8 1.469(5) . ? C8 C9 1.377(6) . ? C8 C12 1.382(6) . ? C9 C10 1.383(7) . ? C9 H9 0.9300 . ? C10 N5 1.325(6) . ? C10 H10 0.9300 . ? C11 N5 1.325(6) . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N6 1.445(5) . ? C13 N4 1.459(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N7 1.304(5) . ? C14 N8 1.352(5) . ? C14 H14 0.9300 . ? C15 N8 1.310(4) . ? C15 N6 1.318(5) . ? C15 H15 0.9300 . ? C16 O2 1.233(5) . ? C16 O1 1.283(4) . ? C16 C22 1.499(5) . ? C17 O3 1.244(5) . ? C17 O4 1.265(4) . ? C17 C18 1.500(5) . ? C17 Cd1 2.692(4) 1_655 ? C18 C23 1.384(5) . ? C18 C19 1.385(5) . ? C19 C20 1.388(5) . ? C19 H19 0.9300 . ? C20 C21 1.375(5) . ? C20 H20 0.9300 . ? C21 C22 1.390(5) . ? C21 H21 0.9300 . ? C22 C23 1.388(5) . ? C23 H23 0.9300 . ? N1 Cd1 2.357(3) 2_445 ? N3 N4 1.364(5) . ? N6 N7 1.359(4) . ? O1 Cd1 2.529(3) 3_556 ? O3 Cd1 2.415(2) 1_655 ? O4 Cd1 2.299(3) 1_655 ? 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 N8 112.65(11) . . ? O1 Cd1 O4 90.72(9) . 1_455 ? N8 Cd1 O4 149.78(10) . 1_455 ? O1 Cd1 N1 113.00(10) . 2_455 ? N8 Cd1 N1 90.65(12) . 2_455 ? O4 Cd1 N1 97.70(12) 1_455 2_455 ? O1 Cd1 O3 145.59(10) . 1_455 ? N8 Cd1 O3 97.72(10) . 1_455 ? O4 Cd1 O3 55.50(9) 1_455 1_455 ? N1 Cd1 O3 81.17(11) 2_455 1_455 ? O1 Cd1 O1 78.73(9) . 3_556 ? N8 Cd1 O1 80.72(10) . 3_556 ? O4 Cd1 O1 85.71(10) 1_455 3_556 ? N1 Cd1 O1 167.62(9) 2_455 3_556 ? O3 Cd1 O1 91.14(9) 1_455 3_556 ? O1 Cd1 C17 118.47(11) . 1_455 ? N8 Cd1 C17 124.12(11) . 1_455 ? O4 Cd1 C17 27.98(10) 1_455 1_455 ? N1 Cd1 C17 89.29(12) 2_455 1_455 ? O3 Cd1 C17 27.52(10) 1_455 1_455 ? O1 Cd1 C17 88.25(10) 3_556 1_455 ? N1 C1 C2 123.9(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.7(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 118.2(4) . . ? C4 C3 C6 123.1(4) . . ? C2 C3 C6 118.6(4) . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.9(4) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N3 C6 N2 114.9(4) . . ? N3 C6 C3 123.0(4) . . ? N2 C6 C3 122.1(4) . . ? N2 C7 N4 109.4(3) . . ? N2 C7 C8 122.3(4) . . ? N4 C7 C8 128.3(4) . . ? C9 C8 C12 117.6(4) . . ? C9 C8 C7 118.1(4) . . ? C12 C8 C7 124.2(4) . . ? C8 C9 C10 118.6(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N5 C10 C9 125.2(5) . . ? N5 C10 H10 117.4 . . ? C9 C10 H10 117.4 . . ? N5 C11 C12 124.8(5) . . ? N5 C11 H11 117.6 . . ? C12 C11 H11 117.6 . . ? C8 C12 C11 118.6(4) . . ? C8 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? N6 C13 N4 109.2(3) . . ? N6 C13 H13A 109.8 . . ? N4 C13 H13A 109.8 . . ? N6 C13 H13B 109.8 . . ? N4 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N7 C14 N8 114.6(4) . . ? N7 C14 H14 122.7 . . ? N8 C14 H14 122.7 . . ? N8 C15 N6 110.2(3) . . ? N8 C15 H15 124.9 . . ? N6 C15 H15 124.9 . . ? O2 C16 O1 123.0(3) . . ? O2 C16 C22 121.0(4) . . ? O1 C16 C22 116.0(4) . . ? O3 C17 O4 122.3(4) . . ? O3 C17 C18 119.8(3) . . ? O4 C17 C18 118.0(4) . . ? O3 C17 Cd1 63.8(2) . 1_655 ? O4 C17 Cd1 58.5(2) . 1_655 ? C18 C17 Cd1 176.5(3) . 1_655 ? C23 C18 C19 119.0(4) . . ? C23 C18 C17 120.5(4) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 119.7(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 118.9(3) . . ? C23 C22 C16 120.0(3) . . ? C21 C22 C16 121.0(3) . . ? C18 C23 C22 121.1(4) . . ? C18 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C5 N1 C1 116.1(4) . . ? C5 N1 Cd1 121.9(3) . 2_445 ? C1 N1 Cd1 119.7(3) . 2_445 ? C7 N2 C6 103.5(3) . . ? C6 N3 N4 102.1(3) . . ? C7 N4 N3 110.2(3) . . ? C7 N4 C13 130.3(4) . . ? N3 N4 C13 118.5(3) . . ? C10 N5 C11 115.2(4) . . ? C15 N6 N7 110.0(3) . . ? C15 N6 C13 128.9(4) . . ? N7 N6 C13 121.0(3) . . ? C14 N7 N6 102.1(3) . . ? C15 N8 C14 103.1(3) . . ? C15 N8 Cd1 127.8(3) . . ? C14 N8 Cd1 129.0(3) . . ? C16 O1 Cd1 107.8(2) . . ? C16 O1 Cd1 121.3(2) . 3_556 ? Cd1 O1 Cd1 101.27(9) . 3_556 ? C17 O3 Cd1 88.7(2) . 1_655 ? C17 O4 Cd1 93.5(2) . 1_655 ? 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 C1 C2 C3 -0.5(7) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C1 C2 C3 C6 178.2(4) . . . . ? C2 C3 C4 C5 0.8(6) . . . . ? C6 C3 C4 C5 -178.2(4) . . . . ? C3 C4 C5 N1 0.7(6) . . . . ? C4 C3 C6 N3 8.8(6) . . . . ? C2 C3 C6 N3 -170.2(4) . . . . ? C4 C3 C6 N2 -170.6(4) . . . . ? C2 C3 C6 N2 10.4(6) . . . . ? N2 C7 C8 C9 -30.3(5) . . . . ? N4 C7 C8 C9 150.2(4) . . . . ? N2 C7 C8 C12 148.1(4) . . . . ? N4 C7 C8 C12 -31.4(6) . . . . ? C12 C8 C9 C10 1.0(6) . . . . ? C7 C8 C9 C10 179.4(4) . . . . ? C8 C9 C10 N5 1.3(8) . . . . ? C9 C8 C12 C11 -2.4(6) . . . . ? C7 C8 C12 C11 179.3(4) . . . . ? N5 C11 C12 C8 1.9(7) . . . . ? O3 C17 C18 C23 -1.4(6) . . . . ? O4 C17 C18 C23 178.6(4) . . . . ? O3 C17 C18 C19 174.5(4) . . . . ? O4 C17 C18 C19 -5.5(6) . . . . ? C23 C18 C19 C20 -0.6(6) . . . . ? C17 C18 C19 C20 -176.5(4) . . . . ? C18 C19 C20 C21 1.6(7) . . . . ? C19 C20 C21 C22 -1.8(6) . . . . ? C20 C21 C22 C23 1.1(6) . . . . ? C20 C21 C22 C16 177.3(4) . . . . ? O2 C16 C22 C23 -30.0(6) . . . . ? O1 C16 C22 C23 151.0(4) . . . . ? O2 C16 C22 C21 153.8(4) . . . . ? O1 C16 C22 C21 -25.1(6) . . . . ? C19 C18 C23 C22 -0.2(6) . . . . ? C17 C18 C23 C22 175.8(4) . . . . ? C21 C22 C23 C18 0.0(6) . . . . ? C16 C22 C23 C18 -176.3(4) . . . . ? C4 C5 N1 C1 -1.9(6) . . . . ? C4 C5 N1 Cd1 160.9(3) . . . 2_445 ? C2 C1 N1 C5 1.8(6) . . . . ? C2 C1 N1 Cd1 -161.4(3) . . . 2_445 ? N4 C7 N2 C6 -1.0(4) . . . . ? C8 C7 N2 C6 179.4(3) . . . . ? N3 C6 N2 C7 1.0(4) . . . . ? C3 C6 N2 C7 -179.6(3) . . . . ? N2 C6 N3 N4 -0.5(4) . . . . ? C3 C6 N3 N4 -179.9(3) . . . . ? N2 C7 N4 N3 0.8(4) . . . . ? C8 C7 N4 N3 -179.6(3) . . . . ? N2 C7 N4 C13 168.7(3) . . . . ? C8 C7 N4 C13 -11.8(7) . . . . ? C6 N3 N4 C7 -0.2(4) . . . . ? C6 N3 N4 C13 -169.7(3) . . . . ? N6 C13 N4 C7 -109.1(5) . . . . ? N6 C13 N4 N3 57.9(5) . . . . ? C9 C10 N5 C11 -1.9(8) . . . . ? C12 C11 N5 C10 0.3(7) . . . . ? N8 C15 N6 N7 1.4(5) . . . . ? N8 C15 N6 C13 177.1(4) . . . . ? N4 C13 N6 C15 -114.5(5) . . . . ? N4 C13 N6 N7 60.8(5) . . . . ? N8 C14 N7 N6 -0.6(5) . . . . ? C15 N6 N7 C14 -0.5(5) . . . . ? C13 N6 N7 C14 -176.6(4) . . . . ? N6 C15 N8 C14 -1.6(5) . . . . ? N6 C15 N8 Cd1 -178.7(3) . . . . ? N7 C14 N8 C15 1.4(5) . . . . ? N7 C14 N8 Cd1 178.4(3) . . . . ? O1 Cd1 N8 C15 178.6(3) . . . . ? O4 Cd1 N8 C15 40.6(5) 1_455 . . . ? N1 Cd1 N8 C15 -66.0(3) 2_455 . . . ? O3 Cd1 N8 C15 15.1(3) 1_455 . . . ? O1 Cd1 N8 C15 105.0(3) 3_556 . . . ? C17 Cd1 N8 C15 23.5(4) 1_455 . . . ? O1 Cd1 N8 C14 2.3(4) . . . . ? O4 Cd1 N8 C14 -135.8(4) 1_455 . . . ? N1 Cd1 N8 C14 117.6(4) 2_455 . . . ? O3 Cd1 N8 C14 -161.2(4) 1_455 . . . ? O1 Cd1 N8 C14 -71.3(4) 3_556 . . . ? C17 Cd1 N8 C14 -152.8(3) 1_455 . . . ? O2 C16 O1 Cd1 -4.6(5) . . . . ? C22 C16 O1 Cd1 174.3(3) . . . . ? O2 C16 O1 Cd1 111.2(4) . . . 3_556 ? C22 C16 O1 Cd1 -69.9(4) . . . 3_556 ? N8 Cd1 O1 C16 53.5(3) . . . . ? O4 Cd1 O1 C16 -146.2(2) 1_455 . . . ? N1 Cd1 O1 C16 -47.5(3) 2_455 . . . ? O3 Cd1 O1 C16 -156.4(2) 1_455 . . . ? O1 Cd1 O1 C16 128.4(3) 3_556 . . . ? C17 Cd1 O1 C16 -149.9(2) 1_455 . . . ? N8 Cd1 O1 Cd1 -74.85(13) . . . 3_556 ? O4 Cd1 O1 Cd1 85.48(11) 1_455 . . 3_556 ? N1 Cd1 O1 Cd1 -175.84(10) 2_455 . . 3_556 ? O3 Cd1 O1 Cd1 75.22(19) 1_455 . . 3_556 ? O1 Cd1 O1 Cd1 0.0 3_556 . . 3_556 ? C17 Cd1 O1 Cd1 81.75(13) 1_455 . . 3_556 ? O4 C17 O3 Cd1 0.0(4) . . . 1_655 ? C18 C17 O3 Cd1 179.9(3) . . . 1_655 ? O3 C17 O4 Cd1 0.0(4) . . . 1_655 ? C18 C17 O4 Cd1 -179.9(3) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.565 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.084 #========================================================== data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 872131' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H16 Cd N8 O5' _chemical_formula_sum 'C23 H16 Cd N8 O5' _chemical_formula_weight 596.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1097(5) _cell_length_b 9.5613(5) _cell_length_c 14.6922(7) _cell_angle_alpha 88.285(4) _cell_angle_beta 86.169(4) _cell_angle_gamma 64.289(5) _cell_volume 1150.42(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3745 _cell_measurement_theta_min 2.7734 _cell_measurement_theta_max 29.1407 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98641 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7353 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.34 _reflns_number_total 4179 _reflns_number_gt 3707 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0284P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4179 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Cd1 Cd -0.03843(2) 0.05727(2) 0.877836(14) 0.02749(9) Uani 1 1 d . . . C1 C -0.0420(4) -0.2714(4) 0.2782(2) 0.0400(8) Uani 1 1 d . . . H1 H 0.0190 -0.3463 0.2347 0.048 Uiso 1 1 calc R . . C2 C -0.1083(4) -0.3163(4) 0.3542(2) 0.0417(8) Uani 1 1 d . . . H2 H -0.0931 -0.4187 0.3607 0.050 Uiso 1 1 calc R . . C3 C -0.1970(4) -0.2084(4) 0.42018(19) 0.0368(8) Uani 1 1 d . . . C4 C -0.2134(4) -0.0589(4) 0.4070(2) 0.0450(9) Uani 1 1 d . . . H4 H -0.2703 0.0169 0.4507 0.054 Uiso 1 1 calc R . . C5 C -0.1451(4) -0.0228(4) 0.3288(2) 0.0416(8) Uani 1 1 d . . . H5A H -0.1583 0.0788 0.3209 0.050 Uiso 1 1 calc R . . C6 C -0.2699(4) -0.2540(4) 0.5011(2) 0.0380(8) Uani 1 1 d . . . C7 C -0.3546(4) -0.3848(4) 0.5890(2) 0.0372(8) Uani 1 1 d . . . C8 C -0.3994(4) -0.5073(4) 0.62568(19) 0.0363(8) Uani 1 1 d . . . C9 C -0.3047(5) -0.6586(4) 0.5974(2) 0.0499(9) Uani 1 1 d . . . H9 H -0.2143 -0.6825 0.5568 0.060 Uiso 1 1 calc R . . C10 C -0.3474(5) -0.7732(5) 0.6308(3) 0.0582(10) Uani 1 1 d . . . H10 H -0.2837 -0.8742 0.6107 0.070 Uiso 1 1 calc R . . C11 C -0.5633(5) -0.6031(5) 0.7154(2) 0.0478(9) Uani 1 1 d . . . H11 H -0.6525 -0.5828 0.7563 0.057 Uiso 1 1 calc R . . C12 C -0.5332(4) -0.4793(4) 0.6853(2) 0.0399(8) Uani 1 1 d . . . H12 H -0.6017 -0.3789 0.7047 0.048 Uiso 1 1 calc R . . C13 C -0.4256(4) -0.2033(5) 0.7254(2) 0.0451(9) Uani 1 1 d . . . H13A H -0.5202 -0.1034 0.7286 0.054 Uiso 1 1 calc R . . H13B H -0.4541 -0.2781 0.7586 0.054 Uiso 1 1 calc R . . C14 C -0.2831(4) -0.0652(4) 0.7937(2) 0.0340(7) Uani 1 1 d . . . H14 H -0.3668 0.0347 0.7911 0.041 Uiso 1 1 calc R . . C15 C -0.0614(4) -0.2580(4) 0.8142(2) 0.0438(8) Uani 1 1 d . . . H15 H 0.0448 -0.3171 0.8310 0.053 Uiso 1 1 calc R . . C16 C -0.1924(3) 0.3635(3) 0.91796(19) 0.0289(7) Uani 1 1 d . . . C17 C -0.7249(3) 0.8363(3) 0.9186(2) 0.0289(7) Uani 1 1 d . . . C18 C -0.5577(3) 0.7510(3) 0.95243(18) 0.0254(6) Uani 1 1 d . . . C19 C -0.5023(3) 0.8204(3) 1.01410(19) 0.0303(7) Uani 1 1 d . . . H19 H -0.5711 0.9187 1.0365 0.036 Uiso 1 1 calc R . . C20 C -0.3448(4) 0.7449(4) 1.0429(2) 0.0321(7) Uani 1 1 d . . . C21 C -0.2436(3) 0.5968(4) 1.01118(19) 0.0302(7) Uani 1 1 d . . . H21 H -0.1382 0.5453 1.0307 0.036 Uiso 1 1 calc R . . C22 C -0.2993(3) 0.5253(3) 0.95032(19) 0.0273(7) Uani 1 1 d . . . C23 C -0.4561(3) 0.6021(3) 0.92110(18) 0.0263(6) Uani 1 1 d . . . H23 H -0.4936 0.5539 0.8804 0.032 Uiso 1 1 calc R . . N1 N -0.0609(3) -0.1264(3) 0.26378(16) 0.0347(6) Uani 1 1 d . . . N2 N -0.2846(3) -0.3895(3) 0.50645(17) 0.0399(7) Uani 1 1 d . . . N3 N -0.3263(4) -0.1655(3) 0.57432(17) 0.0440(7) Uani 1 1 d . . . N4 N -0.3806(3) -0.2512(3) 0.63074(16) 0.0394(7) Uani 1 1 d . . . N5 N -0.4735(4) -0.7493(4) 0.6898(2) 0.0528(8) Uani 1 1 d . . . N6 N -0.2909(3) -0.1923(3) 0.76664(16) 0.0339(6) Uani 1 1 d . . . N7 N -0.1485(4) -0.3185(3) 0.7786(2) 0.0481(7) Uani 1 1 d . . . N8 N -0.1392(3) -0.1016(3) 0.82465(17) 0.0343(6) Uani 1 1 d . . . O1 O -0.0475(2) 0.2981(2) 0.94173(14) 0.0394(5) Uani 1 1 d . . . O2 O -0.2515(2) 0.2979(2) 0.86850(14) 0.0360(5) Uani 1 1 d . . . O3 O -0.7552(2) 0.8038(3) 0.84320(14) 0.0403(5) Uani 1 1 d . . . O4 O -0.8315(2) 0.9447(2) 0.96870(13) 0.0331(5) Uani 1 1 d . . . O5 O -0.2947(3) 0.8190(3) 1.10301(15) 0.0462(6) Uani 1 1 d . . . H5 H -0.2004 0.7629 1.1152 0.069 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 0.02616(13) 0.02441(14) 0.02988(14) -0.00091(9) -0.00170(9) -0.00900(10) C1 0.048(2) 0.037(2) 0.0347(18) -0.0031(15) 0.0066(15) -0.0187(17) C2 0.055(2) 0.041(2) 0.0352(18) 0.0040(16) 0.0016(16) -0.0275(18) C3 0.0457(19) 0.049(2) 0.0240(16) 0.0020(15) -0.0005(14) -0.0282(18) C4 0.058(2) 0.042(2) 0.0311(18) -0.0063(16) 0.0126(16) -0.0197(18) C5 0.053(2) 0.0335(19) 0.0389(19) 0.0013(16) 0.0004(16) -0.0192(17) C6 0.0461(19) 0.049(2) 0.0249(16) -0.0013(15) 0.0015(14) -0.0269(18) C7 0.0386(18) 0.051(2) 0.0297(17) -0.0004(15) -0.0026(14) -0.0265(17) C8 0.0445(19) 0.047(2) 0.0258(16) 0.0041(15) -0.0054(15) -0.0274(17) C9 0.055(2) 0.052(2) 0.044(2) -0.0030(18) 0.0066(17) -0.025(2) C10 0.070(3) 0.043(2) 0.062(2) -0.0009(19) -0.001(2) -0.025(2) C11 0.050(2) 0.056(3) 0.046(2) 0.0053(18) -0.0015(17) -0.031(2) C12 0.0406(19) 0.044(2) 0.0420(19) 0.0018(16) -0.0040(16) -0.0244(17) C13 0.051(2) 0.069(3) 0.0297(17) -0.0085(17) 0.0061(15) -0.041(2) C14 0.0376(18) 0.0319(18) 0.0323(17) -0.0013(14) -0.0009(14) -0.0150(15) C15 0.0412(19) 0.035(2) 0.056(2) -0.0010(17) -0.0076(17) -0.0162(17) C16 0.0259(16) 0.0239(16) 0.0314(16) 0.0054(13) 0.0048(13) -0.0069(14) C17 0.0209(15) 0.0275(17) 0.0355(17) 0.0079(14) 0.0001(13) -0.0087(14) C18 0.0195(14) 0.0268(16) 0.0267(15) 0.0032(13) 0.0030(12) -0.0078(13) C19 0.0264(16) 0.0229(16) 0.0377(17) -0.0033(13) 0.0071(13) -0.0080(14) C20 0.0298(16) 0.0348(18) 0.0337(17) -0.0030(14) 0.0020(14) -0.0163(15) C21 0.0205(14) 0.0324(18) 0.0354(17) 0.0052(14) -0.0021(13) -0.0094(14) C22 0.0221(15) 0.0276(17) 0.0286(15) 0.0045(13) 0.0034(12) -0.0083(13) C23 0.0239(15) 0.0295(17) 0.0248(15) 0.0027(13) 0.0023(12) -0.0115(13) N1 0.0355(14) 0.0390(17) 0.0299(14) 0.0049(12) 0.0002(12) -0.0170(13) N2 0.0521(17) 0.0473(18) 0.0296(14) -0.0008(13) 0.0028(13) -0.0307(15) N3 0.0581(18) 0.054(2) 0.0331(15) -0.0015(14) 0.0051(14) -0.0377(17) N4 0.0518(17) 0.0569(19) 0.0244(13) -0.0043(13) 0.0056(12) -0.0383(16) N5 0.062(2) 0.047(2) 0.0556(19) 0.0082(16) 0.0000(17) -0.0308(17) N6 0.0393(15) 0.0408(17) 0.0299(14) -0.0028(12) 0.0009(12) -0.0252(14) N7 0.0518(18) 0.0354(17) 0.0613(19) -0.0069(15) -0.0015(15) -0.0227(16) N8 0.0353(15) 0.0327(16) 0.0375(14) -0.0003(12) -0.0049(12) -0.0169(13) O1 0.0239(11) 0.0312(13) 0.0518(14) -0.0020(11) -0.0052(10) -0.0010(10) O2 0.0302(11) 0.0307(12) 0.0420(12) -0.0017(10) -0.0024(10) -0.0083(10) O3 0.0295(12) 0.0457(14) 0.0373(12) -0.0022(11) -0.0064(10) -0.0078(11) O4 0.0207(10) 0.0304(12) 0.0369(12) 0.0008(10) 0.0032(9) -0.0011(9) O5 0.0362(12) 0.0464(15) 0.0577(14) -0.0143(12) -0.0072(11) -0.0178(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.2327(19) 1_645 ? Cd1 N8 2.267(3) . ? Cd1 O2 2.285(2) . ? Cd1 N1 2.402(2) 2_556 ? Cd1 O1 2.479(2) . ? Cd1 O4 2.4798(19) 2_467 ? Cd1 C16 2.705(3) . ? C1 N1 1.333(4) . ? C1 C2 1.379(4) . ? C1 H1 0.9300 . ? C2 C3 1.375(5) . ? C2 H2 0.9300 . ? C3 C4 1.380(5) . ? C3 C6 1.470(4) . ? C4 C5 1.376(4) . ? C4 H4 0.9300 . ? C5 N1 1.335(4) . ? C5 H5A 0.9300 . ? C6 N3 1.319(4) . ? C6 N2 1.358(4) . ? C7 N2 1.325(4) . ? C7 N4 1.353(4) . ? C7 C8 1.475(4) . ? C8 C12 1.383(4) . ? C8 C9 1.383(5) . ? C9 C10 1.381(5) . ? C9 H9 0.9300 . ? C10 N5 1.332(5) . ? C10 H10 0.9300 . ? C11 N5 1.327(5) . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N6 1.449(4) . ? C13 N4 1.453(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N8 1.312(4) . ? C14 N6 1.321(4) . ? C14 H14 0.9300 . ? C15 N7 1.307(4) . ? C15 N8 1.357(4) . ? C15 H15 0.9300 . ? C16 O2 1.258(4) . ? C16 O1 1.260(3) . ? C16 C22 1.498(4) . ? C17 O3 1.239(3) . ? C17 O4 1.279(3) . ? C17 C18 1.493(4) . ? C18 C19 1.380(4) . ? C18 C23 1.391(4) . ? C19 C20 1.387(4) . ? C19 H19 0.9300 . ? C20 O5 1.364(4) . ? C20 C21 1.386(4) . ? C21 C22 1.387(4) . ? C21 H21 0.9300 . ? C22 C23 1.384(4) . ? C23 H23 0.9300 . ? N1 Cd1 2.402(2) 2_556 ? N3 N4 1.363(3) . ? N6 N7 1.353(4) . ? O4 Cd1 2.2327(19) 1_465 ? O4 Cd1 2.4798(19) 2_467 ? O5 H5 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 N8 115.39(9) 1_645 . ? O4 Cd1 O2 135.26(8) 1_645 . ? N8 Cd1 O2 103.18(9) . . ? O4 Cd1 N1 109.08(8) 1_645 2_556 ? N8 Cd1 N1 99.61(9) . 2_556 ? O2 Cd1 N1 84.64(8) . 2_556 ? O4 Cd1 O1 82.58(7) 1_645 . ? N8 Cd1 O1 156.89(8) . . ? O2 Cd1 O1 55.08(7) . . ? N1 Cd1 O1 86.94(8) 2_556 . ? O4 Cd1 O4 74.94(7) 1_645 2_467 ? N8 Cd1 O4 90.35(8) . 2_467 ? O2 Cd1 O4 83.38(7) . 2_467 ? N1 Cd1 O4 165.90(8) 2_556 2_467 ? O1 Cd1 O4 80.12(7) . 2_467 ? O4 Cd1 C16 108.45(9) 1_645 . ? N8 Cd1 C16 129.74(9) . . ? O2 Cd1 C16 27.60(8) . . ? N1 Cd1 C16 87.82(9) 2_556 . ? O1 Cd1 C16 27.70(8) . . ? O4 Cd1 C16 78.12(8) 2_467 . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 117.5(3) . . ? C2 C3 C6 120.1(3) . . ? C4 C3 C6 122.4(3) . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? N3 C6 N2 114.9(3) . . ? N3 C6 C3 122.2(3) . . ? N2 C6 C3 122.9(3) . . ? N2 C7 N4 109.4(3) . . ? N2 C7 C8 123.6(3) . . ? N4 C7 C8 127.0(3) . . ? C12 C8 C9 117.9(3) . . ? C12 C8 C7 123.7(3) . . ? C9 C8 C7 118.4(3) . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N5 C10 C9 124.6(4) . . ? N5 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? N5 C11 C12 124.4(3) . . ? N5 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C11 C12 C8 118.7(3) . . ? C11 C12 H12 120.6 . . ? C8 C12 H12 120.6 . . ? N6 C13 N4 110.1(3) . . ? N6 C13 H13A 109.6 . . ? N4 C13 H13A 109.6 . . ? N6 C13 H13B 109.6 . . ? N4 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? N8 C14 N6 109.6(3) . . ? N8 C14 H14 125.2 . . ? N6 C14 H14 125.2 . . ? N7 C15 N8 114.3(3) . . ? N7 C15 H15 122.9 . . ? N8 C15 H15 122.9 . . ? O2 C16 O1 122.6(3) . . ? O2 C16 C22 118.6(3) . . ? O1 C16 C22 118.8(3) . . ? O2 C16 Cd1 57.27(15) . . ? O1 C16 Cd1 66.11(16) . . ? C22 C16 Cd1 169.54(19) . . ? O3 C17 O4 122.2(3) . . ? O3 C17 C18 120.0(3) . . ? O4 C17 C18 117.8(3) . . ? C19 C18 C23 119.6(3) . . ? C19 C18 C17 120.1(3) . . ? C23 C18 C17 120.3(3) . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O5 C20 C21 121.9(3) . . ? O5 C20 C19 118.5(3) . . ? C21 C20 C19 119.6(3) . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 C16 119.7(3) . . ? C21 C22 C16 120.3(3) . . ? C22 C23 C18 120.1(3) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? C1 N1 C5 116.8(3) . . ? C1 N1 Cd1 120.3(2) . 2_556 ? C5 N1 Cd1 122.8(2) . 2_556 ? C7 N2 C6 103.4(3) . . ? C6 N3 N4 102.3(3) . . ? C7 N4 N3 109.9(2) . . ? C7 N4 C13 130.8(3) . . ? N3 N4 C13 118.2(3) . . ? C11 N5 C10 115.8(3) . . ? C14 N6 N7 110.7(3) . . ? C14 N6 C13 127.5(3) . . ? N7 N6 C13 121.8(3) . . ? C15 N7 N6 102.1(3) . . ? C14 N8 C15 103.4(3) . . ? C14 N8 Cd1 128.8(2) . . ? C15 N8 Cd1 127.7(2) . . ? C16 O1 Cd1 86.19(18) . . ? C16 O2 Cd1 95.14(17) . . ? C17 O4 Cd1 102.93(17) . 1_465 ? C17 O4 Cd1 132.19(18) . 2_467 ? Cd1 O4 Cd1 105.06(7) 1_465 2_467 ? C20 O5 H5 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 C1 C2 C3 -1.0(5) . . . . ? C1 C2 C3 C4 -0.8(5) . . . . ? C1 C2 C3 C6 179.4(3) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C6 C3 C4 C5 -178.7(3) . . . . ? C3 C4 C5 N1 -0.6(5) . . . . ? C2 C3 C6 N3 165.7(3) . . . . ? C4 C3 C6 N3 -14.1(5) . . . . ? C2 C3 C6 N2 -14.4(5) . . . . ? C4 C3 C6 N2 165.8(3) . . . . ? N2 C7 C8 C12 -147.1(3) . . . . ? N4 C7 C8 C12 31.0(5) . . . . ? N2 C7 C8 C9 31.3(5) . . . . ? N4 C7 C8 C9 -150.6(3) . . . . ? C12 C8 C9 C10 -0.8(5) . . . . ? C7 C8 C9 C10 -179.2(3) . . . . ? C8 C9 C10 N5 -0.8(6) . . . . ? N5 C11 C12 C8 -1.2(5) . . . . ? C9 C8 C12 C11 1.7(5) . . . . ? C7 C8 C12 C11 -179.9(3) . . . . ? O4 Cd1 C16 O2 -168.02(16) 1_645 . . . ? N8 Cd1 C16 O2 -18.1(2) . . . . ? N1 Cd1 C16 O2 82.59(17) 2_556 . . . ? O1 Cd1 C16 O2 170.2(3) . . . . ? O4 Cd1 C16 O2 -98.51(17) 2_467 . . . ? O4 Cd1 C16 O1 21.83(18) 1_645 . . . ? N8 Cd1 C16 O1 171.74(15) . . . . ? O2 Cd1 C16 O1 -170.2(3) . . . . ? N1 Cd1 C16 O1 -87.56(17) 2_556 . . . ? O4 Cd1 C16 O1 91.34(16) 2_467 . . . ? O4 Cd1 C16 C22 -98.6(12) 1_645 . . . ? N8 Cd1 C16 C22 51.3(12) . . . . ? O2 Cd1 C16 C22 69.4(12) . . . . ? N1 Cd1 C16 C22 152.0(12) 2_556 . . . ? O1 Cd1 C16 C22 -120.4(12) . . . . ? O4 Cd1 C16 C22 -29.1(12) 2_467 . . . ? O3 C17 C18 C19 154.1(3) . . . . ? O4 C17 C18 C19 -24.1(4) . . . . ? O3 C17 C18 C23 -25.0(4) . . . . ? O4 C17 C18 C23 156.9(3) . . . . ? C23 C18 C19 C20 1.9(4) . . . . ? C17 C18 C19 C20 -177.2(3) . . . . ? C18 C19 C20 O5 179.1(3) . . . . ? C18 C19 C20 C21 -1.6(4) . . . . ? O5 C20 C21 C22 179.8(3) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C20 C21 C22 C16 -178.1(3) . . . . ? O2 C16 C22 C23 -3.8(4) . . . . ? O1 C16 C22 C23 176.7(3) . . . . ? Cd1 C16 C22 C23 -67.5(13) . . . . ? O2 C16 C22 C21 174.5(3) . . . . ? O1 C16 C22 C21 -5.1(4) . . . . ? Cd1 C16 C22 C21 110.7(12) . . . . ? C21 C22 C23 C18 0.2(4) . . . . ? C16 C22 C23 C18 178.5(2) . . . . ? C19 C18 C23 C22 -1.2(4) . . . . ? C17 C18 C23 C22 177.9(3) . . . . ? C2 C1 N1 C5 1.9(5) . . . . ? C2 C1 N1 Cd1 -174.1(3) . . . 2_556 ? C4 C5 N1 C1 -1.1(5) . . . . ? C4 C5 N1 Cd1 174.7(3) . . . 2_556 ? N4 C7 N2 C6 0.1(3) . . . . ? C8 C7 N2 C6 178.6(3) . . . . ? N3 C6 N2 C7 -0.3(4) . . . . ? C3 C6 N2 C7 179.9(3) . . . . ? N2 C6 N3 N4 0.3(4) . . . . ? C3 C6 N3 N4 -179.9(3) . . . . ? N2 C7 N4 N3 0.0(4) . . . . ? C8 C7 N4 N3 -178.3(3) . . . . ? N2 C7 N4 C13 -167.5(3) . . . . ? C8 C7 N4 C13 14.1(6) . . . . ? C6 N3 N4 C7 -0.2(4) . . . . ? C6 N3 N4 C13 169.1(3) . . . . ? N6 C13 N4 C7 111.6(4) . . . . ? N6 C13 N4 N3 -55.1(4) . . . . ? C12 C11 N5 C10 -0.3(5) . . . . ? C9 C10 N5 C11 1.4(6) . . . . ? N8 C14 N6 N7 -0.6(4) . . . . ? N8 C14 N6 C13 -177.8(3) . . . . ? N4 C13 N6 C14 111.6(4) . . . . ? N4 C13 N6 N7 -65.3(4) . . . . ? N8 C15 N7 N6 -0.6(4) . . . . ? C14 N6 N7 C15 0.7(4) . . . . ? C13 N6 N7 C15 178.1(3) . . . . ? N6 C14 N8 C15 0.2(3) . . . . ? N6 C14 N8 Cd1 177.99(18) . . . . ? N7 C15 N8 C14 0.3(4) . . . . ? N7 C15 N8 Cd1 -177.6(2) . . . . ? O4 Cd1 N8 C14 158.3(2) 1_645 . . . ? O2 Cd1 N8 C14 1.6(3) . . . . ? N1 Cd1 N8 C14 -85.1(3) 2_556 . . . ? O1 Cd1 N8 C14 19.9(4) . . . . ? O4 Cd1 N8 C14 84.9(3) 2_467 . . . ? C16 Cd1 N8 C14 10.1(3) . . . . ? O4 Cd1 N8 C15 -24.4(3) 1_645 . . . ? O2 Cd1 N8 C15 178.9(3) . . . . ? N1 Cd1 N8 C15 92.2(3) 2_556 . . . ? O1 Cd1 N8 C15 -162.8(2) . . . . ? O4 Cd1 N8 C15 -97.8(3) 2_467 . . . ? C16 Cd1 N8 C15 -172.6(2) . . . . ? O2 C16 O1 Cd1 -9.8(3) . . . . ? C22 C16 O1 Cd1 169.7(2) . . . . ? O4 Cd1 O1 C16 -159.16(17) 1_645 . . . ? N8 Cd1 O1 C16 -16.4(3) . . . . ? O2 Cd1 O1 C16 5.55(16) . . . . ? N1 Cd1 O1 C16 91.14(17) 2_556 . . . ? O4 Cd1 O1 C16 -83.24(17) 2_467 . . . ? O1 C16 O2 Cd1 10.7(3) . . . . ? C22 C16 O2 Cd1 -168.8(2) . . . . ? O4 Cd1 O2 C16 16.2(2) 1_645 . . . ? N8 Cd1 O2 C16 165.79(17) . . . . ? N1 Cd1 O2 C16 -95.57(18) 2_556 . . . ? O1 Cd1 O2 C16 -5.57(16) . . . . ? O4 Cd1 O2 C16 76.99(17) 2_467 . . . ? O3 C17 O4 Cd1 -7.5(3) . . . 1_465 ? C18 C17 O4 Cd1 170.6(2) . . . 1_465 ? O3 C17 O4 Cd1 117.1(3) . . . 2_467 ? C18 C17 O4 Cd1 -64.8(3) . . . 2_467 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O1 0.82 2.18 2.854(3) 138.9 2_567 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.598 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.072 #========================================================== data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 872132' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H56 Cd5 N16 Na2 O34' _chemical_formula_sum 'C66 H56 Cd5 N16 Na2 O34' _chemical_formula_weight 2225.25 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2255(4) _cell_length_b 11.5675(3) _cell_length_c 15.6687(4) _cell_angle_alpha 94.647(2) _cell_angle_beta 110.543(3) _cell_angle_gamma 92.245(3) _cell_volume 1893.96(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8009 _cell_measurement_theta_min 3.1444 _cell_measurement_theta_max 29.1853 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95613 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12105 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6897 _reflns_number_gt 6156 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For O3W, O3WA, O3WB, O4W, O4WA and O4WB, some anisotropic displacement ellipsoids were rather elongated, which led us to use the ISOR restraints. ; _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^)+(0.0391P)^2^+2.4743P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6897 _refine_ls_number_parameters 601 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _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 0.0000 -0.5000 0.5000 0.02951(10) Uani 1 2 d S . . Cd2 Cd 0.76643(2) -0.00224(2) 0.482409(16) 0.02533(8) Uani 1 1 d . . . Cd3 Cd 0.64380(2) 0.15250(2) 0.262856(17) 0.03133(9) Uani 1 1 d . . . Na1 Na 0.59215(14) 0.06479(14) 0.61893(11) 0.0389(4) Uani 1 1 d . . . C1 C 0.0844(4) -0.3650(4) 0.3523(3) 0.0373(9) Uani 1 1 d . . . H1 H 0.1498 -0.3313 0.4045 0.045 Uiso 1 1 calc R . . C2 C 0.0835(4) -0.3386(4) 0.2676(3) 0.0379(9) Uani 1 1 d . . . H2 H 0.1482 -0.2897 0.2630 0.045 Uiso 1 1 calc R . . C3 C -0.0147(4) -0.3860(3) 0.1903(2) 0.0310(8) Uani 1 1 d . . . C4 C -0.1082(4) -0.4577(4) 0.2003(3) 0.0486(11) Uani 1 1 d . . . H4 H -0.1765 -0.4901 0.1493 0.058 Uiso 1 1 calc R . . C5 C -0.0988(5) -0.4809(4) 0.2876(3) 0.0534(12) Uani 1 1 d . . . H5 H -0.1621 -0.5301 0.2939 0.064 Uiso 1 1 calc R . . C6 C -0.0196(4) -0.3651(3) 0.0970(3) 0.0323(8) Uani 1 1 d . . . C7 C 0.0317(4) -0.3221(4) -0.0133(3) 0.0356(9) Uani 1 1 d . . . C8 C 0.1055(4) -0.2834(4) -0.0692(3) 0.0377(9) Uani 1 1 d . . . C9 C 0.0490(4) -0.2425(4) -0.1541(3) 0.0408(10) Uani 1 1 d . . . H9 H -0.0385 -0.2353 -0.1776 0.049 Uiso 1 1 calc R . . C10 C 0.1238(4) -0.2131(4) -0.2027(3) 0.0386(9) Uani 1 1 d . . . H10 H 0.0844 -0.1887 -0.2605 0.046 Uiso 1 1 calc R . . C11 C 0.3045(4) -0.2535(5) -0.0891(3) 0.0589(14) Uani 1 1 d . . . H11 H 0.3928 -0.2554 -0.0657 0.071 Uiso 1 1 calc R . . C12 C 0.2359(4) -0.2880(5) -0.0369(3) 0.0597(14) Uani 1 1 d . . . H12 H 0.2774 -0.3142 0.0199 0.072 Uiso 1 1 calc R . . C13 C -0.1846(4) -0.3941(4) -0.1369(3) 0.0446(10) Uani 1 1 d . . . H13A H -0.2301 -0.4684 -0.1405 0.053 Uiso 1 1 calc R . . H13B H -0.1427 -0.3999 -0.1815 0.053 Uiso 1 1 calc R . . C14 C -0.3388(4) -0.1394(4) -0.1846(3) 0.0491(11) Uani 1 1 d . . . H14 H -0.3424 -0.0610 -0.1937 0.059 Uiso 1 1 calc R . . C15 C -0.4000(4) -0.3110(4) -0.1754(3) 0.0431(10) Uani 1 1 d . . . H15 H -0.4481 -0.3783 -0.1756 0.052 Uiso 1 1 calc R . . C16 C 0.4944(4) -0.4808(3) 0.6162(2) 0.0304(8) Uani 1 1 d . . . H16 H 0.4562 -0.5473 0.6281 0.036 Uiso 1 1 calc R . . C17 C 0.6190(4) -0.4794(3) 0.6196(3) 0.0330(8) Uani 1 1 d . . . H17 H 0.6659 -0.5436 0.6367 0.040 Uiso 1 1 calc R . . C18 C 0.6740(3) -0.3830(3) 0.5977(2) 0.0297(8) Uani 1 1 d . . . H18 H 0.7576 -0.3830 0.5993 0.036 Uiso 1 1 calc R . . C19 C 0.6054(3) -0.2856(3) 0.5731(2) 0.0234(7) Uani 1 1 d . . . C20 C 0.4820(3) -0.2835(3) 0.5754(2) 0.0230(7) Uani 1 1 d . . . C21 C 0.4258(3) -0.3829(3) 0.5949(2) 0.0247(7) Uani 1 1 d . . . C22 C 0.2902(3) -0.3880(3) 0.5924(2) 0.0268(8) Uani 1 1 d . . . C23 C 0.4078(3) -0.1769(3) 0.5567(2) 0.0256(7) Uani 1 1 d . . . C24 C 0.6640(3) -0.1881(3) 0.5396(2) 0.0259(7) Uani 1 1 d . . . C25 C 1.0865(4) -0.0431(3) 0.3241(3) 0.0313(8) Uani 1 1 d . . . C26 C 0.8222(3) -0.0399(3) 0.3250(2) 0.0306(8) Uani 1 1 d . . . C27 C 0.6075(4) -0.0991(4) 0.1492(3) 0.0479(11) Uani 1 1 d . . . C28 C 0.7445(4) -0.0849(4) 0.1533(3) 0.0388(9) Uani 1 1 d . . . C29 C 0.7676(4) -0.0959(4) 0.0721(3) 0.0509(12) Uani 1 1 d . . . H29 H 0.6996 -0.1126 0.0170 0.061 Uiso 1 1 calc R . . C30 C 0.8901(4) -0.0824(4) 0.0716(3) 0.0498(11) Uani 1 1 d . . . H30 H 0.9039 -0.0847 0.0164 0.060 Uiso 1 1 calc R . . C31 C 0.9915(4) -0.0657(4) 0.1532(3) 0.0407(10) Uani 1 1 d . . . H31 H 1.0741 -0.0598 0.1526 0.049 Uiso 1 1 calc R . . C32 C 0.9725(3) -0.0574(3) 0.2367(2) 0.0297(8) Uani 1 1 d . . . C33 C 0.8476(3) -0.0632(3) 0.2371(2) 0.0293(8) Uani 1 1 d . . . N1 N -0.0045(3) -0.4367(3) 0.3624(2) 0.0364(7) Uani 1 1 d . . . N2 N 0.0794(3) -0.3224(3) 0.0768(2) 0.0344(7) Uani 1 1 d . . . N3 N -0.1243(3) -0.3947(3) 0.0258(2) 0.0407(8) Uani 1 1 d . . . N4 N -0.0899(3) -0.3665(3) -0.0454(2) 0.0400(8) Uani 1 1 d . . . N5 N 0.2500(3) -0.2175(3) -0.1717(2) 0.0393(8) Uani 1 1 d . . . N6 N -0.2743(3) -0.3033(3) -0.1574(2) 0.0394(8) Uani 1 1 d . . . N7 N -0.2334(3) -0.1930(3) -0.1632(3) 0.0472(9) Uani 1 1 d . . . N8 N -0.4445(3) -0.2115(3) -0.1925(2) 0.0421(8) Uani 1 1 d . . . O1 O 0.2201(2) -0.4774(2) 0.55307(18) 0.0349(6) Uani 1 1 d . . . O2 O 0.2540(2) -0.3026(2) 0.62990(19) 0.0367(6) Uani 1 1 d . . . O3 O 0.3222(2) -0.1736(2) 0.48052(18) 0.0349(6) Uani 1 1 d . . . O4 O 0.4310(3) -0.0959(2) 0.62178(17) 0.0316(6) Uani 1 1 d . . . O5 O 0.5971(2) -0.1038(2) 0.50929(17) 0.0300(6) Uani 1 1 d . . . O6 O 0.7745(3) -0.1918(2) 0.5409(2) 0.0394(7) Uani 1 1 d . . . O7 O 0.7935(3) -0.1211(3) 0.36292(19) 0.0447(7) Uani 1 1 d . . . O8 O 0.8225(2) 0.0655(2) 0.35513(16) 0.0314(6) Uani 1 1 d . . . O9 O 0.5708(3) -0.0268(3) 0.1978(2) 0.0489(7) Uani 1 1 d . . . O10 O 0.5391(3) -0.1809(4) 0.0989(3) 0.0820(13) Uani 1 1 d . . . O11 O 1.0630(2) -0.0451(2) 0.39689(17) 0.0373(6) Uani 1 1 d . . . O12 O 1.1942(3) -0.0316(3) 0.31940(19) 0.0432(7) Uani 1 1 d . . . O1W O 0.0153(3) -0.6892(3) 0.4432(2) 0.0536(8) Uani 1 1 d . . . O2W O 0.6828(6) -0.3341(4) 0.3229(4) 0.1192(19) Uani 1 1 d . . . O3WA O 0.446(2) -0.1820(18) 0.2741(15) 0.066(5) Uani 0.25 1 d PU . . O3W O 0.463(2) -0.2221(19) 0.3070(15) 0.086(7) Uani 0.25 1 d PU . . O3WB O 0.3785(17) -0.1598(13) 0.2329(11) 0.048(3) Uani 0.25 1 d PU . . O3WC O 0.3118(16) -0.1433(13) 0.1576(19) 0.098(7) Uani 0.25 1 d P . . O4W O 0.5664(13) -0.4812(10) 0.1683(8) 0.126(4) Uani 0.50 1 d PU . . O4WA O 0.4644(17) -0.4344(13) 0.1488(11) 0.065(4) Uani 0.25 1 d PU . . O4WB O 0.382(2) -0.3990(16) 0.1718(13) 0.098(6) Uani 0.25 1 d PU . . O5W O 0.6031(6) -0.3765(5) 0.0253(4) 0.1196(18) 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 0.0247(2) 0.0438(2) 0.02481(19) 0.01104(15) 0.01261(15) 0.00698(16) Cd2 0.02000(14) 0.03197(15) 0.02691(14) 0.00920(10) 0.01036(11) 0.00415(11) Cd3 0.02116(15) 0.04827(18) 0.02787(15) 0.01074(11) 0.01102(11) 0.00561(12) Na1 0.0280(8) 0.0464(9) 0.0446(9) 0.0102(7) 0.0142(7) 0.0059(7) C1 0.036(2) 0.045(2) 0.030(2) 0.0096(16) 0.0088(17) -0.0029(18) C2 0.037(2) 0.042(2) 0.037(2) 0.0115(17) 0.0157(18) -0.0043(18) C3 0.036(2) 0.035(2) 0.0294(19) 0.0095(15) 0.0177(17) 0.0076(17) C4 0.049(3) 0.067(3) 0.026(2) 0.0089(19) 0.0105(19) -0.016(2) C5 0.049(3) 0.078(3) 0.035(2) 0.013(2) 0.018(2) -0.020(2) C6 0.034(2) 0.037(2) 0.031(2) 0.0127(15) 0.0154(17) 0.0068(17) C7 0.032(2) 0.048(2) 0.033(2) 0.0190(17) 0.0166(17) 0.0117(18) C8 0.037(2) 0.051(2) 0.034(2) 0.0162(17) 0.0208(18) 0.0095(19) C9 0.029(2) 0.062(3) 0.040(2) 0.0232(19) 0.0178(18) 0.017(2) C10 0.037(2) 0.055(3) 0.031(2) 0.0181(18) 0.0184(18) 0.0120(19) C11 0.030(2) 0.110(4) 0.040(3) 0.032(3) 0.011(2) 0.006(3) C12 0.037(3) 0.108(4) 0.037(2) 0.034(3) 0.011(2) 0.007(3) C13 0.046(3) 0.051(3) 0.037(2) 0.0084(18) 0.0133(19) 0.012(2) C14 0.039(3) 0.053(3) 0.052(3) 0.009(2) 0.011(2) 0.011(2) C15 0.033(2) 0.053(3) 0.041(2) 0.0114(19) 0.0097(18) 0.000(2) C16 0.031(2) 0.0289(19) 0.036(2) 0.0144(15) 0.0151(16) 0.0034(16) C17 0.032(2) 0.0288(19) 0.042(2) 0.0112(16) 0.0154(17) 0.0120(16) C18 0.0215(19) 0.034(2) 0.035(2) 0.0057(15) 0.0106(15) 0.0072(15) C19 0.0217(18) 0.0257(17) 0.0247(17) 0.0024(13) 0.0104(14) 0.0043(14) C20 0.0204(17) 0.0292(18) 0.0206(16) 0.0054(13) 0.0079(13) 0.0047(14) C21 0.0232(18) 0.0267(18) 0.0259(17) 0.0053(13) 0.0102(14) 0.0026(14) C22 0.0255(19) 0.033(2) 0.0263(18) 0.0151(15) 0.0113(15) 0.0036(16) C23 0.0181(18) 0.0290(19) 0.038(2) 0.0130(15) 0.0181(16) 0.0032(14) C24 0.0252(19) 0.0283(18) 0.0278(18) 0.0040(14) 0.0137(15) 0.0025(15) C25 0.024(2) 0.035(2) 0.035(2) 0.0069(15) 0.0090(16) 0.0087(16) C26 0.0192(18) 0.046(2) 0.0263(18) 0.0060(16) 0.0071(15) 0.0066(16) C27 0.027(2) 0.071(3) 0.038(2) -0.004(2) 0.0049(19) -0.002(2) C28 0.031(2) 0.049(2) 0.033(2) -0.0046(17) 0.0095(17) 0.0054(18) C29 0.041(3) 0.079(3) 0.025(2) -0.007(2) 0.0048(18) 0.005(2) C30 0.047(3) 0.075(3) 0.029(2) -0.005(2) 0.017(2) 0.009(2) C31 0.036(2) 0.054(3) 0.037(2) 0.0005(18) 0.0196(18) 0.0112(19) C32 0.026(2) 0.032(2) 0.0313(19) 0.0032(15) 0.0101(16) 0.0066(15) C33 0.0246(19) 0.036(2) 0.0268(18) 0.0002(14) 0.0085(15) 0.0033(15) N1 0.0368(19) 0.047(2) 0.0270(16) 0.0083(14) 0.0125(14) -0.0025(15) N2 0.0333(18) 0.0442(19) 0.0322(17) 0.0134(14) 0.0171(14) 0.0082(15) N3 0.037(2) 0.058(2) 0.0333(18) 0.0140(15) 0.0182(16) 0.0072(17) N4 0.038(2) 0.060(2) 0.0291(17) 0.0155(15) 0.0168(15) 0.0099(17) N5 0.0316(19) 0.059(2) 0.0322(17) 0.0142(15) 0.0156(15) 0.0040(16) N6 0.036(2) 0.047(2) 0.0357(18) 0.0115(14) 0.0111(15) 0.0082(16) N7 0.033(2) 0.052(2) 0.057(2) 0.0137(17) 0.0150(17) 0.0079(17) N8 0.0238(18) 0.061(2) 0.0405(19) 0.0153(16) 0.0077(15) 0.0092(17) O1 0.0245(14) 0.0363(15) 0.0445(15) 0.0033(12) 0.0135(12) -0.0035(12) O2 0.0249(14) 0.0393(15) 0.0505(16) 0.0017(12) 0.0198(13) 0.0014(12) O3 0.0215(14) 0.0409(15) 0.0418(15) 0.0170(12) 0.0072(12) 0.0079(11) O4 0.0381(16) 0.0288(13) 0.0384(14) 0.0070(11) 0.0255(12) 0.0066(11) O5 0.0257(14) 0.0326(14) 0.0364(14) 0.0136(11) 0.0142(11) 0.0053(11) O6 0.0283(15) 0.0391(15) 0.0637(19) 0.0155(13) 0.0295(14) 0.0084(12) O7 0.0461(18) 0.0514(18) 0.0421(16) 0.0112(13) 0.0220(14) -0.0033(14) O8 0.0270(14) 0.0419(15) 0.0268(13) 0.0035(11) 0.0106(11) 0.0110(11) O9 0.0300(16) 0.063(2) 0.0528(18) -0.0083(15) 0.0174(14) -0.0026(14) O10 0.043(2) 0.104(3) 0.080(3) -0.044(2) 0.0123(19) -0.023(2) O11 0.0258(14) 0.0557(17) 0.0282(14) 0.0062(12) 0.0061(11) 0.0066(12) O12 0.0246(15) 0.0618(19) 0.0440(16) 0.0101(13) 0.0113(12) 0.0107(13) O1W 0.0321(17) 0.0477(18) 0.075(2) -0.0069(15) 0.0144(15) 0.0075(14) O2W 0.136(5) 0.077(3) 0.147(5) 0.019(3) 0.054(4) -0.023(3) O3WA 0.083(9) 0.070(9) 0.061(9) -0.006(7) 0.046(7) 0.010(7) O3W 0.108(11) 0.075(10) 0.075(10) -0.011(7) 0.035(8) 0.023(8) O3WB 0.045(7) 0.065(7) 0.042(6) -0.001(5) 0.027(5) 0.010(6) O3WC 0.044(9) 0.057(9) 0.21(2) -0.045(12) 0.076(13) -0.018(8) O4W 0.138(8) 0.120(7) 0.121(7) -0.001(6) 0.058(6) -0.056(6) O4WA 0.057(7) 0.056(7) 0.081(8) 0.027(6) 0.020(6) -0.010(6) O4WB 0.119(10) 0.074(8) 0.085(9) 0.034(7) 0.012(7) -0.003(8) O5W 0.111(4) 0.135(5) 0.108(4) 0.008(3) 0.035(3) 0.007(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.310(3) 2_546 ? Cd1 O1 2.310(3) . ? Cd1 N1 2.317(3) . ? Cd1 N1 2.317(3) 2_546 ? Cd1 O1W 2.330(3) 2_546 ? Cd1 O1W 2.330(3) . ? Cd2 O11 2.180(3) 2_756 ? Cd2 O7 2.346(3) . ? Cd2 O5 2.374(2) . ? Cd2 O3 2.417(3) 2_656 ? Cd2 O6 2.437(3) . ? Cd2 O8 2.466(2) . ? Cd2 O4 2.613(3) 2_656 ? Cd2 C24 2.754(3) . ? Cd2 C26 2.755(3) . ? Cd2 Na1 3.4339(15) . ? Cd2 Na1 3.7878(16) 2_656 ? Cd3 O9 2.225(3) . ? Cd3 O2 2.274(3) 2_656 ? Cd3 N8 2.280(3) 2 ? Cd3 N5 2.308(3) 2_655 ? Cd3 O8 2.342(2) . ? Cd3 O4 2.370(2) 2_656 ? Na1 O3WA 2.238(18) 2_656 ? Na1 O3W 2.30(2) 2_656 ? Na1 O12 2.311(3) 2_756 ? Na1 O3WB 2.393(14) 2_656 ? Na1 O5 2.445(3) 2_656 ? Na1 O3 2.492(3) 2_656 ? Na1 O5 2.508(3) . ? Na1 O4 2.556(3) . ? Na1 Na1 3.723(3) 2_656 ? Na1 Cd2 3.7878(16) 2_656 ? C1 N1 1.333(5) . ? C1 C2 1.382(5) . ? C1 H1 0.9300 . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.372(6) . ? C3 C6 1.482(5) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 N1 1.321(5) . ? C5 H5 0.9300 . ? C6 N3 1.315(5) . ? C6 N2 1.345(5) . ? C7 N2 1.322(5) . ? C7 N4 1.343(5) . ? C7 C8 1.483(5) . ? C8 C12 1.375(6) . ? C8 C9 1.388(5) . ? C9 C10 1.368(5) . ? C9 H9 0.9300 . ? C10 N5 1.331(5) . ? C10 H10 0.9300 . ? C11 N5 1.332(5) . ? C11 C12 1.376(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N4 1.455(5) . ? C13 N6 1.459(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N7 1.307(6) . ? C14 N8 1.386(6) . ? C14 H14 0.9300 . ? C15 N8 1.283(5) . ? C15 N6 1.335(5) . ? C15 H15 0.9300 . ? C16 C17 1.380(5) . ? C16 C21 1.391(5) . ? C16 H16 0.9300 . ? C17 C18 1.377(5) . ? C17 H17 0.9300 . ? C18 C19 1.393(5) . ? C18 H18 0.9300 . ? C19 C20 1.400(5) . ? C19 C24 1.504(5) . ? C20 C21 1.396(5) . ? C20 C23 1.507(5) . ? C21 C22 1.508(5) . ? C22 O1 1.249(4) . ? C22 O2 1.262(4) . ? C23 O3 1.247(4) . ? C23 O4 1.275(4) . ? C24 O6 1.236(4) . ? C24 O5 1.274(4) . ? C25 O12 1.239(4) . ? C25 O11 1.260(4) . ? C25 C32 1.503(5) . ? C26 O7 1.241(5) . ? C26 O8 1.270(5) . ? C26 C33 1.509(5) . ? C27 O10 1.226(5) . ? C27 O9 1.262(5) . ? C27 C28 1.518(6) . ? C28 C29 1.382(6) . ? C28 C33 1.408(5) . ? C29 C30 1.381(6) . ? C29 H29 0.9300 . ? C30 C31 1.373(6) . ? C30 H30 0.9300 . ? C31 C32 1.394(5) . ? C31 H31 0.9300 . ? C32 C33 1.403(5) . ? N3 N4 1.361(4) . ? N5 Cd3 2.308(3) 2_655 ? N6 N7 1.361(5) . ? N8 Cd3 2.280(3) 2 ? O2 Cd3 2.274(3) 2_656 ? O3 Cd2 2.417(3) 2_656 ? O3 Na1 2.492(3) 2_656 ? O4 Cd3 2.370(2) 2_656 ? O4 Cd2 2.613(3) 2_656 ? O5 Na1 2.445(3) 2_656 ? O11 Cd2 2.180(3) 2_756 ? O12 Na1 2.311(3) 2_756 ? O3WA O3W 0.70(2) . ? O3WA O3WB 0.87(2) . ? O3WA Na1 2.238(18) 2_656 ? O3W O3WB 1.48(3) . ? O3W Na1 2.30(2) 2_656 ? O3WB O3WC 1.19(3) . ? O3WB Na1 2.393(14) 2_656 ? O4W O4WA 1.236(19) . ? O4WA O4WB 1.18(2) . ? 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 180.000(1) 2_546 . ? O1 Cd1 N1 90.90(11) 2_546 . ? O1 Cd1 N1 89.10(11) . . ? O1 Cd1 N1 89.10(11) 2_546 2_546 ? O1 Cd1 N1 90.90(11) . 2_546 ? N1 Cd1 N1 180.000(1) . 2_546 ? O1 Cd1 O1W 87.77(10) 2_546 2_546 ? O1 Cd1 O1W 92.23(10) . 2_546 ? N1 Cd1 O1W 90.86(12) . 2_546 ? N1 Cd1 O1W 89.14(12) 2_546 2_546 ? O1 Cd1 O1W 92.23(10) 2_546 . ? O1 Cd1 O1W 87.77(10) . . ? N1 Cd1 O1W 89.14(12) . . ? N1 Cd1 O1W 90.86(12) 2_546 . ? O1W Cd1 O1W 180.000(1) 2_546 . ? O11 Cd2 O7 116.29(10) 2_756 . ? O11 Cd2 O5 115.38(9) 2_756 . ? O7 Cd2 O5 103.12(9) . . ? O11 Cd2 O3 88.83(9) 2_756 2_656 ? O7 Cd2 O3 144.37(9) . 2_656 ? O5 Cd2 O3 86.27(8) . 2_656 ? O11 Cd2 O6 84.73(10) 2_756 . ? O7 Cd2 O6 79.01(9) . . ? O5 Cd2 O6 54.14(8) . . ? O3 Cd2 O6 130.93(8) 2_656 . ? O11 Cd2 O8 104.20(9) 2_756 . ? O7 Cd2 O8 54.07(9) . . ? O5 Cd2 O8 140.35(8) . . ? O3 Cd2 O8 97.16(8) 2_656 . ? O6 Cd2 O8 131.58(8) . . ? O11 Cd2 O4 138.75(9) 2_756 2_656 ? O7 Cd2 O4 95.65(9) . 2_656 ? O5 Cd2 O4 78.66(8) . 2_656 ? O3 Cd2 O4 52.01(8) 2_656 2_656 ? O6 Cd2 O4 128.82(9) . 2_656 ? O8 Cd2 O4 72.97(8) . 2_656 ? O11 Cd2 C24 100.06(10) 2_756 . ? O7 Cd2 C24 91.63(10) . . ? O5 Cd2 C24 27.50(9) . . ? O3 Cd2 C24 109.30(9) 2_656 . ? O6 Cd2 C24 26.66(9) . . ? O8 Cd2 C24 144.24(9) . . ? O4 Cd2 C24 104.64(9) 2_656 . ? O11 Cd2 C26 112.16(10) 2_756 . ? O7 Cd2 C26 26.64(10) . . ? O5 Cd2 C26 124.21(10) . . ? O3 Cd2 C26 122.42(10) 2_656 . ? O6 Cd2 C26 104.85(10) . . ? O8 Cd2 C26 27.45(10) . . ? O4 Cd2 C26 84.52(9) 2_656 . ? C24 Cd2 C26 117.87(11) . . ? O11 Cd2 Na1 87.29(7) 2_756 . ? O7 Cd2 Na1 149.45(8) . . ? O5 Cd2 Na1 46.91(7) . . ? O3 Cd2 Na1 46.52(6) 2_656 . ? O6 Cd2 Na1 84.55(6) . . ? O8 Cd2 Na1 142.29(6) . . ? O4 Cd2 Na1 74.96(6) 2_656 . ? C24 Cd2 Na1 63.89(7) . . ? C26 Cd2 Na1 158.80(8) . . ? O11 Cd2 Na1 148.60(7) 2_756 2_656 ? O7 Cd2 Na1 91.45(8) . 2_656 ? O5 Cd2 Na1 38.86(6) . 2_656 ? O3 Cd2 Na1 74.37(7) 2_656 2_656 ? O6 Cd2 Na1 86.65(7) . 2_656 ? O8 Cd2 Na1 104.09(6) . 2_656 ? O4 Cd2 Na1 42.31(6) 2_656 2_656 ? C24 Cd2 Na1 62.67(8) . 2_656 ? C26 Cd2 Na1 99.23(8) . 2_656 ? Na1 Cd2 Na1 61.83(4) . 2_656 ? O9 Cd3 O2 161.06(11) . 2_656 ? O9 Cd3 N8 88.45(12) . 2 ? O2 Cd3 N8 104.38(12) 2_656 2 ? O9 Cd3 N5 102.61(12) . 2_655 ? O2 Cd3 N5 88.58(11) 2_656 2_655 ? N8 Cd3 N5 101.63(12) 2 2_655 ? O9 Cd3 O8 85.69(10) . . ? O2 Cd3 O8 78.50(9) 2_656 . ? N8 Cd3 O8 165.47(11) 2 . ? N5 Cd3 O8 92.62(10) 2_655 . ? O9 Cd3 O4 83.66(10) . 2_656 ? O2 Cd3 O4 83.33(9) 2_656 2_656 ? N8 Cd3 O4 86.36(11) 2 2_656 ? N5 Cd3 O4 169.85(11) 2_655 2_656 ? O8 Cd3 O4 79.79(9) . 2_656 ? O3WA Na1 O3W 17.7(6) 2_656 2_656 ? O3WA Na1 O12 105.5(7) 2_656 2_756 ? O3W Na1 O12 113.4(6) 2_656 2_756 ? O3WA Na1 O3WB 21.3(6) 2_656 2_656 ? O3W Na1 O3WB 36.6(6) 2_656 2_656 ? O12 Na1 O3WB 85.5(4) 2_756 2_656 ? O3WA Na1 O5 96.5(7) 2_656 2_656 ? O3W Na1 O5 83.4(6) 2_656 2_656 ? O12 Na1 O5 151.61(11) 2_756 2_656 ? O3WB Na1 O5 117.7(4) 2_656 2_656 ? O3WA Na1 O3 112.6(5) 2_656 2_656 ? O3W Na1 O3 97.7(6) 2_656 2_656 ? O12 Na1 O3 79.50(10) 2_756 2_656 ? O3WB Na1 O3 116.7(4) 2_656 2_656 ? O5 Na1 O3 75.54(9) 2_656 2_656 ? O3WA Na1 O5 164.9(5) 2_656 . ? O3W Na1 O5 165.6(6) 2_656 . ? O12 Na1 O5 80.73(10) 2_756 . ? O3WB Na1 O5 154.5(4) 2_656 . ? O5 Na1 O5 82.56(10) 2_656 . ? O3 Na1 O5 81.85(9) 2_656 . ? O3WA Na1 O4 92.9(5) 2_656 . ? O3W Na1 O4 101.9(6) 2_656 . ? O12 Na1 O4 117.30(11) 2_756 . ? O3WB Na1 O4 95.8(4) 2_656 . ? O5 Na1 O4 78.50(9) 2_656 . ? O3 Na1 O4 145.21(11) 2_656 . ? O5 Na1 O4 72.10(9) . . ? O3WA Na1 Cd2 151.0(5) 2_656 . ? O3W Na1 Cd2 141.0(6) 2_656 . ? O12 Na1 Cd2 58.41(8) 2_756 . ? O3WB Na1 Cd2 139.6(4) 2_656 . ? O5 Na1 Cd2 93.90(7) 2_656 . ? O3 Na1 Cd2 44.71(6) 2_656 . ? O5 Na1 Cd2 43.73(6) . . ? O4 Na1 Cd2 115.73(7) . . ? O3WA Na1 Na1 136.5(7) 2_656 2_656 ? O3W Na1 Na1 125.2(6) 2_656 2_656 ? O12 Na1 Na1 118.00(10) 2_756 2_656 ? O3WB Na1 Na1 156.1(4) 2_656 2_656 ? O5 Na1 Na1 41.91(7) 2_656 2_656 ? O3 Na1 Na1 74.96(8) 2_656 2_656 ? O5 Na1 Na1 40.64(6) . 2_656 ? O4 Na1 Na1 70.25(8) . 2_656 ? Cd2 Na1 Na1 63.76(4) . 2_656 ? O3WA Na1 Cd2 85.4(6) 2_656 2_656 ? O3W Na1 Cd2 82.1(6) 2_656 2_656 ? O12 Na1 Cd2 159.43(10) 2_756 2_656 ? O3WB Na1 Cd2 102.0(4) 2_656 2_656 ? O5 Na1 Cd2 37.53(6) 2_656 2_656 ? O3 Na1 Cd2 112.91(8) 2_656 2_656 ? O5 Na1 Cd2 84.80(7) . 2_656 ? O4 Na1 Cd2 43.47(6) . 2_656 ? Cd2 Na1 Cd2 118.17(4) . 2_656 ? Na1 Na1 Cd2 54.41(4) 2_656 2_656 ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 118.6(3) . . ? C4 C3 C6 119.5(4) . . ? C2 C3 C6 122.0(3) . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 123.3(4) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N3 C6 N2 114.8(3) . . ? N3 C6 C3 120.1(3) . . ? N2 C6 C3 124.9(4) . . ? N2 C7 N4 109.7(3) . . ? N2 C7 C8 124.2(4) . . ? N4 C7 C8 126.0(3) . . ? C12 C8 C9 117.6(3) . . ? C12 C8 C7 119.4(3) . . ? C9 C8 C7 123.0(4) . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N5 C10 C9 123.4(4) . . ? N5 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N5 C11 C12 122.9(4) . . ? N5 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C8 C12 C11 119.5(4) . . ? C8 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N4 C13 N6 109.7(3) . . ? N4 C13 H13A 109.7 . . ? N6 C13 H13A 109.7 . . ? N4 C13 H13B 109.7 . . ? N6 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N7 C14 N8 113.1(4) . . ? N7 C14 H14 123.4 . . ? N8 C14 H14 123.4 . . ? N8 C15 N6 109.9(4) . . ? N8 C15 H15 125.1 . . ? N6 C15 H15 125.1 . . ? C17 C16 C21 120.2(3) . . ? C17 C16 H16 119.9 . . ? C21 C16 H16 119.9 . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 119.5(3) . . ? C18 C19 C24 118.6(3) . . ? C20 C19 C24 121.8(3) . . ? C21 C20 C19 119.3(3) . . ? C21 C20 C23 119.1(3) . . ? C19 C20 C23 121.6(3) . . ? C16 C21 C20 120.1(3) . . ? C16 C21 C22 118.4(3) . . ? C20 C21 C22 121.5(3) . . ? O1 C22 O2 123.8(3) . . ? O1 C22 C21 117.6(3) . . ? O2 C22 C21 118.6(3) . . ? O3 C23 O4 122.6(3) . . ? O3 C23 C20 119.2(3) . . ? O4 C23 C20 118.0(3) . . ? O6 C24 O5 121.5(3) . . ? O6 C24 C19 119.8(3) . . ? O5 C24 C19 118.7(3) . . ? O6 C24 Cd2 62.21(18) . . ? O5 C24 Cd2 59.39(17) . . ? C19 C24 Cd2 177.3(2) . . ? O12 C25 O11 125.5(4) . . ? O12 C25 C32 118.6(3) . . ? O11 C25 C32 115.8(3) . . ? O7 C26 O8 121.4(3) . . ? O7 C26 C33 120.7(3) . . ? O8 C26 C33 117.7(3) . . ? O7 C26 Cd2 57.95(19) . . ? O8 C26 Cd2 63.50(18) . . ? C33 C26 Cd2 177.7(3) . . ? O10 C27 O9 123.8(4) . . ? O10 C27 C28 117.8(4) . . ? O9 C27 C28 118.4(4) . . ? C29 C28 C33 119.6(4) . . ? C29 C28 C27 118.5(4) . . ? C33 C28 C27 121.9(3) . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 119.7(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 121.0(4) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C33 119.3(3) . . ? C31 C32 C25 119.1(3) . . ? C33 C32 C25 121.6(3) . . ? C32 C33 C28 119.2(3) . . ? C32 C33 C26 121.0(3) . . ? C28 C33 C26 119.7(3) . . ? C5 N1 C1 117.6(3) . . ? C5 N1 Cd1 117.1(3) . . ? C1 N1 Cd1 125.2(3) . . ? C7 N2 C6 103.4(3) . . ? C6 N3 N4 102.6(3) . . ? C7 N4 N3 109.4(3) . . ? C7 N4 C13 133.8(3) . . ? N3 N4 C13 116.7(3) . . ? C10 N5 C11 117.4(3) . . ? C10 N5 Cd3 116.8(2) . 2_655 ? C11 N5 Cd3 125.7(3) . 2_655 ? C15 N6 N7 110.4(3) . . ? C15 N6 C13 129.4(4) . . ? N7 N6 C13 120.2(3) . . ? C14 N7 N6 102.4(4) . . ? C15 N8 C14 104.2(4) . . ? C15 N8 Cd3 133.8(3) . 2 ? C14 N8 Cd3 119.6(3) . 2 ? C22 O1 Cd1 127.9(2) . . ? C22 O2 Cd3 134.3(2) . 2_656 ? C23 O3 Cd2 97.5(2) . 2_656 ? C23 O3 Na1 109.4(2) . 2_656 ? Cd2 O3 Na1 88.77(9) 2_656 2_656 ? C23 O4 Cd3 111.4(2) . 2_656 ? C23 O4 Na1 113.3(2) . . ? Cd3 O4 Na1 133.16(12) 2_656 . ? C23 O4 Cd2 87.6(2) . 2_656 ? Cd3 O4 Cd2 100.98(9) 2_656 2_656 ? Na1 O4 Cd2 94.23(9) . 2_656 ? C24 O5 Cd2 93.1(2) . . ? C24 O5 Na1 139.7(2) . 2_656 ? Cd2 O5 Na1 103.61(9) . 2_656 ? C24 O5 Na1 119.5(2) . . ? Cd2 O5 Na1 89.36(9) . . ? Na1 O5 Na1 97.44(10) 2_656 . ? C24 O6 Cd2 91.1(2) . . ? C26 O7 Cd2 95.4(2) . . ? C26 O8 Cd3 111.1(2) . . ? C26 O8 Cd2 89.0(2) . . ? Cd3 O8 Cd2 106.26(9) . . ? C27 O9 Cd3 132.9(3) . . ? C25 O11 Cd2 111.5(2) . 2_756 ? C25 O12 Na1 147.8(3) . 2_756 ? O3W O3WA O3WB 140(5) . . ? O3W O3WA Na1 86(3) . 2_656 ? O3WB O3WA Na1 89.5(18) . 2_656 ? O3WA O3W Na1 76(3) . 2_656 ? O3WB O3W Na1 75.1(10) . 2_656 ? O3WA O3WB O3WC 156(2) . . ? O3WC O3WB O3W 158.4(16) . . ? O3WA O3WB Na1 69.3(16) . 2_656 ? O3WC O3WB Na1 132.7(13) . 2_656 ? O3W O3WB Na1 68.3(10) . 2_656 ? O4WB O4WA O4W 148.9(19) . . ? 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 O11 Cd2 Na1 O3WA 44.9(14) 2_756 . . 2_656 ? O7 Cd2 Na1 O3WA -172.7(14) . . . 2_656 ? O5 Cd2 Na1 O3WA 174.1(14) . . . 2_656 ? O3 Cd2 Na1 O3WA -46.0(14) 2_656 . . 2_656 ? O6 Cd2 Na1 O3WA 129.9(14) . . . 2_656 ? O8 Cd2 Na1 O3WA -65.0(14) . . . 2_656 ? O4 Cd2 Na1 O3WA -97.4(14) 2_656 . . 2_656 ? C24 Cd2 Na1 O3WA 147.5(14) . . . 2_656 ? C26 Cd2 Na1 O3WA -112.3(14) . . . 2_656 ? Na1 Cd2 Na1 O3WA -141.0(14) 2_656 . . 2_656 ? O11 Cd2 Na1 O3W 71.5(9) 2_756 . . 2_656 ? O7 Cd2 Na1 O3W -146.1(9) . . . 2_656 ? O5 Cd2 Na1 O3W -159.3(9) . . . 2_656 ? O3 Cd2 Na1 O3W -19.5(9) 2_656 . . 2_656 ? O6 Cd2 Na1 O3W 156.4(9) . . . 2_656 ? O8 Cd2 Na1 O3W -38.4(9) . . . 2_656 ? O4 Cd2 Na1 O3W -70.9(9) 2_656 . . 2_656 ? C24 Cd2 Na1 O3W 174.1(9) . . . 2_656 ? C26 Cd2 Na1 O3W -85.8(10) . . . 2_656 ? Na1 Cd2 Na1 O3W -114.4(9) 2_656 . . 2_656 ? O11 Cd2 Na1 O12 -17.52(12) 2_756 . . 2_756 ? O7 Cd2 Na1 O12 124.87(17) . . . 2_756 ? O5 Cd2 Na1 O12 111.67(13) . . . 2_756 ? O3 Cd2 Na1 O12 -108.48(13) 2_656 . . 2_756 ? O6 Cd2 Na1 O12 67.44(12) . . . 2_756 ? O8 Cd2 Na1 O12 -127.41(14) . . . 2_756 ? O4 Cd2 Na1 O12 -159.90(11) 2_656 . . 2_756 ? C24 Cd2 Na1 O12 85.07(13) . . . 2_756 ? C26 Cd2 Na1 O12 -174.8(2) . . . 2_756 ? Na1 Cd2 Na1 O12 156.56(11) 2_656 . . 2_756 ? O11 Cd2 Na1 O3WB 12.7(6) 2_756 . . 2_656 ? O7 Cd2 Na1 O3WB 155.1(6) . . . 2_656 ? O5 Cd2 Na1 O3WB 141.9(6) . . . 2_656 ? O3 Cd2 Na1 O3WB -78.3(6) 2_656 . . 2_656 ? O6 Cd2 Na1 O3WB 97.6(6) . . . 2_656 ? O8 Cd2 Na1 O3WB -97.2(6) . . . 2_656 ? O4 Cd2 Na1 O3WB -129.7(6) 2_656 . . 2_656 ? C24 Cd2 Na1 O3WB 115.3(6) . . . 2_656 ? C26 Cd2 Na1 O3WB -144.6(7) . . . 2_656 ? Na1 Cd2 Na1 O3WB -173.2(6) 2_656 . . 2_656 ? O11 Cd2 Na1 O5 155.83(10) 2_756 . . 2_656 ? O7 Cd2 Na1 O5 -61.78(17) . . . 2_656 ? O5 Cd2 Na1 O5 -74.98(11) . . . 2_656 ? O3 Cd2 Na1 O5 64.87(11) 2_656 . . 2_656 ? O6 Cd2 Na1 O5 -119.21(10) . . . 2_656 ? O8 Cd2 Na1 O5 45.94(13) . . . 2_656 ? O4 Cd2 Na1 O5 13.45(9) 2_656 . . 2_656 ? C24 Cd2 Na1 O5 -101.58(11) . . . 2_656 ? C26 Cd2 Na1 O5 -1.4(3) . . . 2_656 ? Na1 Cd2 Na1 O5 -30.10(6) 2_656 . . 2_656 ? O11 Cd2 Na1 O3 90.96(12) 2_756 . . 2_656 ? O7 Cd2 Na1 O3 -126.65(17) . . . 2_656 ? O5 Cd2 Na1 O3 -139.86(13) . . . 2_656 ? O6 Cd2 Na1 O3 175.92(11) . . . 2_656 ? O8 Cd2 Na1 O3 -18.93(14) . . . 2_656 ? O4 Cd2 Na1 O3 -51.42(11) 2_656 . . 2_656 ? C24 Cd2 Na1 O3 -166.45(12) . . . 2_656 ? C26 Cd2 Na1 O3 -66.3(3) . . . 2_656 ? Na1 Cd2 Na1 O3 -94.97(10) 2_656 . . 2_656 ? O11 Cd2 Na1 O5 -129.19(11) 2_756 . . . ? O7 Cd2 Na1 O5 13.20(18) . . . . ? O3 Cd2 Na1 O5 139.86(13) 2_656 . . . ? O6 Cd2 Na1 O5 -44.23(11) . . . . ? O8 Cd2 Na1 O5 120.92(13) . . . . ? O4 Cd2 Na1 O5 88.44(10) 2_656 . . . ? C24 Cd2 Na1 O5 -26.60(11) . . . . ? C26 Cd2 Na1 O5 73.6(3) . . . . ? Na1 Cd2 Na1 O5 44.89(8) 2_656 . . . ? O11 Cd2 Na1 O4 -125.05(11) 2_756 . . . ? O7 Cd2 Na1 O4 17.33(18) . . . . ? O5 Cd2 Na1 O4 4.13(10) . . . . ? O3 Cd2 Na1 O4 143.99(13) 2_656 . . . ? O6 Cd2 Na1 O4 -40.09(11) . . . . ? O8 Cd2 Na1 O4 125.05(13) . . . . ? O4 Cd2 Na1 O4 92.57(9) 2_656 . . . ? C24 Cd2 Na1 O4 -22.47(11) . . . . ? C26 Cd2 Na1 O4 77.7(3) . . . . ? Na1 Cd2 Na1 O4 49.02(8) 2_656 . . . ? O11 Cd2 Na1 Na1 -174.07(8) 2_756 . . 2_656 ? O7 Cd2 Na1 Na1 -31.68(16) . . . 2_656 ? O5 Cd2 Na1 Na1 -44.89(8) . . . 2_656 ? O3 Cd2 Na1 Na1 94.97(10) 2_656 . . 2_656 ? O6 Cd2 Na1 Na1 -89.11(8) . . . 2_656 ? O8 Cd2 Na1 Na1 76.04(12) . . . 2_656 ? O4 Cd2 Na1 Na1 43.55(7) 2_656 . . 2_656 ? C24 Cd2 Na1 Na1 -71.48(9) . . . 2_656 ? C26 Cd2 Na1 Na1 28.7(3) . . . 2_656 ? O11 Cd2 Na1 Cd2 -174.07(8) 2_756 . . 2_656 ? O7 Cd2 Na1 Cd2 -31.68(16) . . . 2_656 ? O5 Cd2 Na1 Cd2 -44.89(8) . . . 2_656 ? O3 Cd2 Na1 Cd2 94.97(10) 2_656 . . 2_656 ? O6 Cd2 Na1 Cd2 -89.11(8) . . . 2_656 ? O8 Cd2 Na1 Cd2 76.04(12) . . . 2_656 ? O4 Cd2 Na1 Cd2 43.55(7) 2_656 . . 2_656 ? C24 Cd2 Na1 Cd2 -71.48(9) . . . 2_656 ? C26 Cd2 Na1 Cd2 28.7(3) . . . 2_656 ? Na1 Cd2 Na1 Cd2 0.0 2_656 . . 2_656 ? N1 C1 C2 C3 1.6(6) . . . . ? C1 C2 C3 C4 0.0(6) . . . . ? C1 C2 C3 C6 -177.7(4) . . . . ? C2 C3 C4 C5 -1.0(7) . . . . ? C6 C3 C4 C5 176.8(4) . . . . ? C3 C4 C5 N1 0.5(8) . . . . ? C4 C3 C6 N3 13.8(6) . . . . ? C2 C3 C6 N3 -168.4(4) . . . . ? C4 C3 C6 N2 -162.3(4) . . . . ? C2 C3 C6 N2 15.5(6) . . . . ? N2 C7 C8 C12 25.1(7) . . . . ? N4 C7 C8 C12 -151.8(5) . . . . ? N2 C7 C8 C9 -155.2(4) . . . . ? N4 C7 C8 C9 27.8(7) . . . . ? C12 C8 C9 C10 2.3(7) . . . . ? C7 C8 C9 C10 -177.3(4) . . . . ? C8 C9 C10 N5 -2.4(7) . . . . ? C9 C8 C12 C11 -0.5(8) . . . . ? C7 C8 C12 C11 179.1(5) . . . . ? N5 C11 C12 C8 -1.4(9) . . . . ? C21 C16 C17 C18 -3.1(6) . . . . ? C16 C17 C18 C19 0.8(6) . . . . ? C17 C18 C19 C20 3.4(5) . . . . ? C17 C18 C19 C24 -173.1(3) . . . . ? C18 C19 C20 C21 -5.3(5) . . . . ? C24 C19 C20 C21 171.1(3) . . . . ? C18 C19 C20 C23 175.2(3) . . . . ? C24 C19 C20 C23 -8.4(5) . . . . ? C17 C16 C21 C20 1.1(5) . . . . ? C17 C16 C21 C22 -179.7(3) . . . . ? C19 C20 C21 C16 3.1(5) . . . . ? C23 C20 C21 C16 -177.3(3) . . . . ? C19 C20 C21 C22 -176.1(3) . . . . ? C23 C20 C21 C22 3.5(5) . . . . ? C16 C21 C22 O1 -44.3(4) . . . . ? C20 C21 C22 O1 134.9(3) . . . . ? C16 C21 C22 O2 135.6(3) . . . . ? C20 C21 C22 O2 -45.2(5) . . . . ? C21 C20 C23 O3 -77.1(4) . . . . ? C19 C20 C23 O3 102.4(4) . . . . ? C21 C20 C23 O4 99.2(4) . . . . ? C19 C20 C23 O4 -81.3(4) . . . . ? C18 C19 C24 O6 -5.5(5) . . . . ? C20 C19 C24 O6 178.1(3) . . . . ? C18 C19 C24 O5 173.8(3) . . . . ? C20 C19 C24 O5 -2.7(5) . . . . ? O11 Cd2 C24 O6 -55.9(2) 2_756 . . . ? O7 Cd2 C24 O6 61.2(2) . . . . ? O5 Cd2 C24 O6 177.1(3) . . . . ? O3 Cd2 C24 O6 -148.2(2) 2_656 . . . ? O8 Cd2 C24 O6 76.4(3) . . . . ? O4 Cd2 C24 O6 157.5(2) 2_656 . . . ? C26 Cd2 C24 O6 66.0(2) . . . . ? Na1 Cd2 C24 O6 -137.8(2) . . . . ? Na1 Cd2 C24 O6 152.0(2) 2_656 . . . ? O11 Cd2 C24 O5 127.0(2) 2_756 . . . ? O7 Cd2 C24 O5 -115.9(2) . . . . ? O3 Cd2 C24 O5 34.7(2) 2_656 . . . ? O6 Cd2 C24 O5 -177.1(3) . . . . ? O8 Cd2 C24 O5 -100.7(2) . . . . ? O4 Cd2 C24 O5 -19.7(2) 2_656 . . . ? C26 Cd2 C24 O5 -111.2(2) . . . . ? Na1 Cd2 C24 O5 45.08(17) . . . . ? Na1 Cd2 C24 O5 -25.14(17) 2_656 . . . ? O11 Cd2 C26 O7 104.7(2) 2_756 . . . ? O5 Cd2 C26 O7 -42.0(3) . . . . ? O3 Cd2 C26 O7 -151.8(2) 2_656 . . . ? O6 Cd2 C26 O7 14.4(2) . . . . ? O8 Cd2 C26 O7 -177.3(4) . . . . ? O4 Cd2 C26 O7 -114.3(2) 2_656 . . . ? C24 Cd2 C26 O7 -10.6(3) . . . . ? Na1 Cd2 C26 O7 -99.9(3) . . . . ? Na1 Cd2 C26 O7 -74.5(2) 2_656 . . . ? O11 Cd2 C26 O8 -77.9(2) 2_756 . . . ? O7 Cd2 C26 O8 177.3(4) . . . . ? O5 Cd2 C26 O8 135.33(19) . . . . ? O3 Cd2 C26 O8 25.5(2) 2_656 . . . ? O6 Cd2 C26 O8 -168.22(19) . . . . ? O4 Cd2 C26 O8 63.0(2) 2_656 . . . ? C24 Cd2 C26 O8 166.70(19) . . . . ? Na1 Cd2 C26 O8 77.5(3) . . . . ? Na1 Cd2 C26 O8 102.82(19) 2_656 . . . ? O10 C27 C28 C29 45.2(7) . . . . ? O9 C27 C28 C29 -135.1(5) . . . . ? O10 C27 C28 C33 -133.6(5) . . . . ? O9 C27 C28 C33 46.1(6) . . . . ? C33 C28 C29 C30 -2.0(7) . . . . ? C27 C28 C29 C30 179.2(4) . . . . ? C28 C29 C30 C31 4.5(8) . . . . ? C29 C30 C31 C32 -2.6(7) . . . . ? C30 C31 C32 C33 -1.7(6) . . . . ? C30 C31 C32 C25 178.0(4) . . . . ? O12 C25 C32 C31 4.5(5) . . . . ? O11 C25 C32 C31 -174.8(4) . . . . ? O12 C25 C32 C33 -175.7(4) . . . . ? O11 C25 C32 C33 4.9(5) . . . . ? C31 C32 C33 C28 4.2(6) . . . . ? C25 C32 C33 C28 -175.5(4) . . . . ? C31 C32 C33 C26 -172.4(4) . . . . ? C25 C32 C33 C26 7.9(5) . . . . ? C29 C28 C33 C32 -2.3(6) . . . . ? C27 C28 C33 C32 176.4(4) . . . . ? C29 C28 C33 C26 174.2(4) . . . . ? C27 C28 C33 C26 -7.0(6) . . . . ? O7 C26 C33 C32 -103.7(4) . . . . ? O8 C26 C33 C32 81.1(4) . . . . ? O8 C26 C33 C28 -95.4(4) . . . . ? C4 C5 N1 C1 1.0(7) . . . . ? C4 C5 N1 Cd1 -175.0(4) . . . . ? C2 C1 N1 C5 -2.1(6) . . . . ? C2 C1 N1 Cd1 173.6(3) . . . . ? O1 Cd1 N1 C5 -32.1(4) 2_546 . . . ? O1 Cd1 N1 C5 147.9(4) . . . . ? O1W Cd1 N1 C5 -119.9(4) 2_546 . . . ? O1W Cd1 N1 C5 60.1(4) . . . . ? O1 Cd1 N1 C1 152.2(3) 2_546 . . . ? O1 Cd1 N1 C1 -27.8(3) . . . . ? O1W Cd1 N1 C1 64.4(3) 2_546 . . . ? O1W Cd1 N1 C1 -115.6(3) . . . . ? N4 C7 N2 C6 -1.9(4) . . . . ? C8 C7 N2 C6 -179.2(4) . . . . ? N3 C6 N2 C7 2.0(5) . . . . ? C3 C6 N2 C7 178.3(4) . . . . ? N2 C6 N3 N4 -1.3(5) . . . . ? C3 C6 N3 N4 -177.8(3) . . . . ? N2 C7 N4 N3 1.2(5) . . . . ? C8 C7 N4 N3 178.5(4) . . . . ? N2 C7 N4 C13 -175.2(4) . . . . ? C8 C7 N4 C13 2.1(7) . . . . ? C6 N3 N4 C7 0.0(4) . . . . ? C6 N3 N4 C13 177.1(3) . . . . ? N6 C13 N4 C7 -102.0(5) . . . . ? N6 C13 N4 N3 81.8(4) . . . . ? C9 C10 N5 C11 0.5(7) . . . . ? C9 C10 N5 Cd3 -176.3(3) . . . 2_655 ? C12 C11 N5 C10 1.5(8) . . . . ? C12 C11 N5 Cd3 177.9(4) . . . 2_655 ? N8 C15 N6 N7 -0.2(5) . . . . ? N8 C15 N6 C13 -178.2(4) . . . . ? N4 C13 N6 C15 -118.0(4) . . . . ? N4 C13 N6 N7 64.3(5) . . . . ? N8 C14 N7 N6 0.0(5) . . . . ? C15 N6 N7 C14 0.1(4) . . . . ? C13 N6 N7 C14 178.3(4) . . . . ? N6 C15 N8 C14 0.2(5) . . . . ? N6 C15 N8 Cd3 161.7(3) . . . 2 ? N7 C14 N8 C15 -0.2(5) . . . . ? N7 C14 N8 Cd3 -164.9(3) . . . 2 ? O2 C22 O1 Cd1 18.3(5) . . . . ? C21 C22 O1 Cd1 -161.8(2) . . . . ? N1 Cd1 O1 C22 87.8(3) . . . . ? N1 Cd1 O1 C22 -92.2(3) 2_546 . . . ? O1W Cd1 O1 C22 -3.1(3) 2_546 . . . ? O1W Cd1 O1 C22 176.9(3) . . . . ? O1 C22 O2 Cd3 160.3(3) . . . 2_656 ? C21 C22 O2 Cd3 -19.7(5) . . . 2_656 ? O4 C23 O3 Cd2 -5.3(3) . . . 2_656 ? C20 C23 O3 Cd2 170.8(2) . . . 2_656 ? O4 C23 O3 Na1 86.0(3) . . . 2_656 ? C20 C23 O3 Na1 -97.9(3) . . . 2_656 ? O3 C23 O4 Cd3 105.7(3) . . . 2_656 ? C20 C23 O4 Cd3 -70.4(3) . . . 2_656 ? O3 C23 O4 Na1 -88.7(3) . . . . ? C20 C23 O4 Na1 95.1(3) . . . . ? O3 C23 O4 Cd2 4.9(3) . . . 2_656 ? C20 C23 O4 Cd2 -171.3(3) . . . 2_656 ? O3WA Na1 O4 C23 169.4(7) 2_656 . . . ? O3W Na1 O4 C23 154.0(6) 2_656 . . . ? O12 Na1 O4 C23 -81.5(3) 2_756 . . . ? O3WB Na1 O4 C23 -169.4(5) 2_656 . . . ? O5 Na1 O4 C23 73.4(2) 2_656 . . . ? O3 Na1 O4 C23 31.0(3) 2_656 . . . ? O5 Na1 O4 C23 -12.4(2) . . . . ? Cd2 Na1 O4 C23 -15.4(3) . . . . ? Na1 Na1 O4 C23 30.6(2) 2_656 . . . ? Cd2 Na1 O4 C23 89.3(2) 2_656 . . . ? O3WA Na1 O4 Cd3 -29.2(7) 2_656 . . 2_656 ? O3W Na1 O4 Cd3 -44.6(6) 2_656 . . 2_656 ? O12 Na1 O4 Cd3 79.92(18) 2_756 . . 2_656 ? O3WB Na1 O4 Cd3 -8.0(5) 2_656 . . 2_656 ? O5 Na1 O4 Cd3 -125.21(15) 2_656 . . 2_656 ? O3 Na1 O4 Cd3 -167.54(14) 2_656 . . 2_656 ? O5 Na1 O4 Cd3 148.99(16) . . . 2_656 ? Cd2 Na1 O4 Cd3 146.00(11) . . . 2_656 ? Na1 Na1 O4 Cd3 -167.99(15) 2_656 . . 2_656 ? Cd2 Na1 O4 Cd3 -109.33(16) 2_656 . . 2_656 ? O3WA Na1 O4 Cd2 80.2(7) 2_656 . . 2_656 ? O3W Na1 O4 Cd2 64.8(6) 2_656 . . 2_656 ? O12 Na1 O4 Cd2 -170.74(10) 2_756 . . 2_656 ? O3WB Na1 O4 Cd2 101.3(4) 2_656 . . 2_656 ? O5 Na1 O4 Cd2 -15.87(8) 2_656 . . 2_656 ? O3 Na1 O4 Cd2 -58.21(19) 2_656 . . 2_656 ? O5 Na1 O4 Cd2 -101.67(9) . . . 2_656 ? Cd2 Na1 O4 Cd2 -104.67(7) . . . 2_656 ? Na1 Na1 O4 Cd2 -58.66(6) 2_656 . . 2_656 ? O6 C24 O5 Cd2 -3.0(4) . . . . ? C19 C24 O5 Cd2 177.8(3) . . . . ? O6 C24 O5 Na1 112.4(4) . . . 2_656 ? C19 C24 O5 Na1 -66.8(4) . . . 2_656 ? Cd2 C24 O5 Na1 115.4(3) . . . 2_656 ? O6 C24 O5 Na1 -94.0(4) . . . . ? C19 C24 O5 Na1 86.8(3) . . . . ? Cd2 C24 O5 Na1 -91.02(17) . . . . ? O11 Cd2 O5 C24 -60.5(2) 2_756 . . . ? O7 Cd2 O5 C24 67.4(2) . . . . ? O3 Cd2 O5 C24 -147.4(2) 2_656 . . . ? O6 Cd2 O5 C24 1.58(19) . . . . ? O8 Cd2 O5 C24 115.9(2) . . . . ? O4 Cd2 O5 C24 160.6(2) 2_656 . . . ? C26 Cd2 O5 C24 85.3(2) . . . . ? Na1 Cd2 O5 C24 -119.5(2) . . . . ? Na1 Cd2 O5 C24 143.0(2) 2_656 . . . ? O11 Cd2 O5 Na1 156.48(10) 2_756 . . 2_656 ? O7 Cd2 O5 Na1 -75.65(11) . . . 2_656 ? O3 Cd2 O5 Na1 69.55(10) 2_656 . . 2_656 ? O6 Cd2 O5 Na1 -141.45(15) . . . 2_656 ? O8 Cd2 O5 Na1 -27.17(17) . . . 2_656 ? O4 Cd2 O5 Na1 17.58(9) 2_656 . . 2_656 ? C24 Cd2 O5 Na1 -143.0(2) . . . 2_656 ? C26 Cd2 O5 Na1 -57.70(14) . . . 2_656 ? Na1 Cd2 O5 Na1 97.50(11) . . . 2_656 ? O11 Cd2 O5 Na1 58.97(11) 2_756 . . . ? O7 Cd2 O5 Na1 -173.15(9) . . . . ? O3 Cd2 O5 Na1 -27.96(9) 2_656 . . . ? O6 Cd2 O5 Na1 121.05(13) . . . . ? O8 Cd2 O5 Na1 -124.67(11) . . . . ? O4 Cd2 O5 Na1 -79.92(8) 2_656 . . . ? C24 Cd2 O5 Na1 119.5(2) . . . . ? C26 Cd2 O5 Na1 -155.21(10) . . . . ? Na1 Cd2 O5 Na1 -97.50(11) 2_656 . . . ? O3WA Na1 O5 C24 -76(3) 2_656 . . . ? O3W Na1 O5 C24 -150(3) 2_656 . . . ? O12 Na1 O5 C24 39.9(2) 2_756 . . . ? O3WB Na1 O5 C24 -18.4(10) 2_656 . . . ? O5 Na1 O5 C24 -163.2(3) 2_656 . . . ? O3 Na1 O5 C24 120.5(2) 2_656 . . . ? O4 Na1 O5 C24 -82.9(2) . . . . ? Cd2 Na1 O5 C24 93.2(2) . . . . ? Na1 Na1 O5 C24 -163.2(3) 2_656 . . . ? Cd2 Na1 O5 C24 -125.5(2) 2_656 . . . ? O3WA Na1 O5 Cd2 -169(3) 2_656 . . . ? O3W Na1 O5 Cd2 117(3) 2_656 . . . ? O12 Na1 O5 Cd2 -53.33(10) 2_756 . . . ? O3WB Na1 O5 Cd2 -111.6(9) 2_656 . . . ? O5 Na1 O5 Cd2 103.64(9) 2_656 . . . ? O3 Na1 O5 Cd2 27.27(8) 2_656 . . . ? O4 Na1 O5 Cd2 -176.09(10) . . . . ? Na1 Na1 O5 Cd2 103.64(9) 2_656 . . . ? Cd2 Na1 O5 Cd2 141.34(6) 2_656 . . . ? O3WA Na1 O5 Na1 87(3) 2_656 . . 2_656 ? O3W Na1 O5 Na1 13(3) 2_656 . . 2_656 ? O12 Na1 O5 Na1 -156.97(12) 2_756 . . 2_656 ? O3WB Na1 O5 Na1 144.8(9) 2_656 . . 2_656 ? O5 Na1 O5 Na1 0.0 2_656 . . 2_656 ? O3 Na1 O5 Na1 -76.37(9) 2_656 . . 2_656 ? O4 Na1 O5 Na1 80.27(9) . . . 2_656 ? Cd2 Na1 O5 Na1 -103.64(9) . . . 2_656 ? Cd2 Na1 O5 Na1 37.70(6) 2_656 . . 2_656 ? O5 C24 O6 Cd2 2.9(4) . . . . ? C19 C24 O6 Cd2 -177.9(3) . . . . ? O11 Cd2 O6 C24 125.1(2) 2_756 . . . ? O7 Cd2 O6 C24 -116.8(2) . . . . ? O5 Cd2 O6 C24 -1.6(2) . . . . ? O3 Cd2 O6 C24 41.2(3) 2_656 . . . ? O8 Cd2 O6 C24 -130.6(2) . . . . ? O4 Cd2 O6 C24 -28.4(3) 2_656 . . . ? C26 Cd2 O6 C24 -123.4(2) . . . . ? Na1 Cd2 O6 C24 37.3(2) . . . . ? Na1 Cd2 O6 C24 -24.7(2) 2_656 . . . ? O8 C26 O7 Cd2 -2.8(4) . . . . ? C33 C26 O7 Cd2 -177.8(3) . . . . ? O11 Cd2 O7 C26 -87.3(2) 2_756 . . . ? O5 Cd2 O7 C26 145.4(2) . . . . ? O3 Cd2 O7 C26 43.2(3) 2_656 . . . ? O6 Cd2 O7 C26 -165.8(2) . . . . ? O8 Cd2 O7 C26 1.5(2) . . . . ? O4 Cd2 O7 C26 65.7(2) 2_656 . . . ? C24 Cd2 O7 C26 170.6(2) . . . . ? Na1 Cd2 O7 C26 135.5(2) . . . . ? Na1 Cd2 O7 C26 107.9(2) 2_656 . . . ? O7 C26 O8 Cd3 -104.4(3) . . . . ? C33 C26 O8 Cd3 70.7(3) . . . . ? Cd2 C26 O8 Cd3 -107.08(15) . . . . ? O7 C26 O8 Cd2 2.6(4) . . . . ? C33 C26 O8 Cd2 177.8(3) . . . . ? O9 Cd3 O8 C26 11.2(2) . . . . ? O2 Cd3 O8 C26 -179.2(2) 2_656 . . . ? N8 Cd3 O8 C26 77.7(5) 2 . . . ? N5 Cd3 O8 C26 -91.2(2) 2_655 . . . ? O4 Cd3 O8 C26 95.6(2) 2_656 . . . ? O9 Cd3 O8 Cd2 -84.16(11) . . . . ? O2 Cd3 O8 Cd2 85.36(10) 2_656 . . . ? N8 Cd3 O8 Cd2 -17.7(5) 2 . . . ? N5 Cd3 O8 Cd2 173.38(12) 2_655 . . . ? O4 Cd3 O8 Cd2 0.16(9) 2_656 . . . ? O11 Cd2 O8 C26 110.9(2) 2_756 . . . ? O7 Cd2 O8 C26 -1.5(2) . . . . ? O5 Cd2 O8 C26 -65.7(2) . . . . ? O3 Cd2 O8 C26 -158.5(2) 2_656 . . . ? O6 Cd2 O8 C26 15.3(2) . . . . ? O4 Cd2 O8 C26 -111.9(2) 2_656 . . . ? C24 Cd2 O8 C26 -20.4(3) . . . . ? Na1 Cd2 O8 C26 -144.76(18) . . . . ? Na1 Cd2 O8 C26 -82.9(2) 2_656 . . . ? O11 Cd2 O8 Cd3 -137.34(10) 2_756 . . . ? O7 Cd2 O8 Cd3 110.28(14) . . . . ? O5 Cd2 O8 Cd3 46.06(17) . . . . ? O3 Cd2 O8 Cd3 -46.73(11) 2_656 . . . ? O6 Cd2 O8 Cd3 127.05(11) . . . . ? O4 Cd2 O8 Cd3 -0.15(8) 2_656 . . . ? C24 Cd2 O8 Cd3 91.38(17) . . . . ? C26 Cd2 O8 Cd3 111.8(2) . . . . ? Na1 Cd2 O8 Cd3 -33.01(16) . . . . ? Na1 Cd2 O8 Cd3 28.88(10) 2_656 . . . ? O10 C27 O9 Cd3 -159.7(4) . . . . ? C28 C27 O9 Cd3 20.7(6) . . . . ? O2 Cd3 O9 C27 -99.8(5) 2_656 . . . ? N8 Cd3 O9 C27 126.8(4) 2 . . . ? N5 Cd3 O9 C27 25.3(4) 2_655 . . . ? O8 Cd3 O9 C27 -66.5(4) . . . . ? O4 Cd3 O9 C27 -146.7(4) 2_656 . . . ? O12 C25 O11 Cd2 9.2(5) . . . 2_756 ? C32 C25 O11 Cd2 -171.5(2) . . . 2_756 ? O11 C25 O12 Na1 31.9(8) . . . 2_756 ? C32 C25 O12 Na1 -147.3(4) . . . 2_756 ? Na1 O3WA O3W O3WB 85(5) 2_656 . . . ? O3WB O3WA O3W Na1 -85(5) . . . 2_656 ? O3W O3WA O3WB O3WC -120(7) . . . . ? Na1 O3WA O3WB O3WC 157(6) 2_656 . . . ? Na1 O3WA O3WB O3W -83(6) 2_656 . . . ? O3W O3WA O3WB Na1 83(6) . . . 2_656 ? Na1 O3W O3WB O3WA 90(6) 2_656 . . . ? O3WA O3W O3WB O3WC 103(7) . . . . ? Na1 O3W O3WB O3WC -167(5) 2_656 . . . ? O3WA O3W O3WB Na1 -90(6) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.713 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.088 #========================================================== data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 872133' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H24 Cd3 N8 O15' _chemical_formula_sum 'C33 H24 Cd3 N8 O15' _chemical_formula_weight 1109.80 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 'P n m a' _symmetry_space_group_name_hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 10.0266(2) _cell_length_b 21.0636(6) _cell_length_c 16.6202(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3510.13(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7114 _cell_measurement_theta_min 3.0550 _cell_measurement_theta_max 29.2641 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6599 _exptl_absorpt_correction_T_max 0.6924 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21246 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3307 _reflns_number_gt 2832 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For N2, N2', N2'' and N5, some anisotropic displacement ellipsoids were rather elongated, which led us to use the ISOR restraints. 'Simu' restraints were used for N4, N5, N6, C8 and C9 to make them have close U~eq~. ; _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^)+(0.0379P)^2^+16.7743P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3307 _refine_ls_number_parameters 336 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.102 _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 0.49237(4) 0.39655(2) 0.65169(3) 0.04172(16) Uani 1 1 d . . . Cd2 Cd 0.85402(5) 0.2500 0.64722(3) 0.03001(16) Uani 1 2 d S . . C1 C 0.3230(6) 0.5234(3) 0.7092(4) 0.0466(15) Uani 1 1 d . . . H1 H 0.2724 0.4915 0.7330 0.056 Uiso 1 1 calc R . . C2 C 0.2989(6) 0.5857(3) 0.7310(4) 0.0481(16) Uani 1 1 d . . . H2 H 0.2321 0.5951 0.7679 0.058 Uiso 1 1 calc R . . C3 C 0.3743(6) 0.6337(3) 0.6978(4) 0.0476(16) Uani 1 1 d . . . C4 C 0.4669(8) 0.6163(4) 0.6393(5) 0.074(3) Uani 1 1 d . . . H4 H 0.5169 0.6472 0.6130 0.089 Uiso 1 1 calc R . . C5 C 0.4840(7) 0.5534(3) 0.6206(5) 0.063(2) Uani 1 1 d . . . H5 H 0.5467 0.5427 0.5816 0.076 Uiso 1 1 calc R . . C6 C 0.3594(7) 0.6997(3) 0.7221(4) 0.0486(16) Uani 1 1 d . . . C7 C 0.3141(15) 0.7012(6) 0.8752(7) 0.052(4) Uani 0.50 1 d P . . C10 C 0.7546(5) 0.3921(3) 0.5912(3) 0.0362(13) Uani 1 1 d . . . C11 C 1.0122(5) 0.3758(3) 0.6732(3) 0.0304(12) Uani 1 1 d . . . C12 C 1.2573(6) 0.3878(3) 0.5749(4) 0.0434(14) Uani 1 1 d . . . C13 C 0.8835(6) 0.4029(3) 0.5488(3) 0.0420(14) Uani 1 1 d . . . C14 C 1.0066(5) 0.3918(3) 0.5851(3) 0.0329(12) Uani 1 1 d . . . C15 C 1.1232(6) 0.4000(4) 0.5398(4) 0.0507(17) Uani 1 1 d . . . C16 C 1.1148(14) 0.4023(8) 0.4543(8) 0.042(3) Uani 0.50 1 d P . . C16' C 1.1133(14) 0.4372(6) 0.4667(8) 0.038(3) Uani 0.50 1 d P . . C17 C 0.9955(15) 0.4111(10) 0.4184(9) 0.053(4) Uani 0.50 1 d P . . C17' C 0.9907(14) 0.4498(8) 0.4327(8) 0.039(3) Uani 0.50 1 d P . . C18 C 0.8764(18) 0.4092(8) 0.4621(10) 0.034(4) Uani 0.50 1 d P . . C18' C 0.875(2) 0.4374(7) 0.4766(12) 0.038(4) Uani 0.50 1 d P . . N1 N 0.4159(5) 0.5069(3) 0.6553(3) 0.0473(13) Uani 1 1 d . . . N2 N 0.3250(12) 0.7159(6) 0.7931(7) 0.042(3) Uani 0.60 1 d PU . . N2' N 0.312(2) 0.7500 0.7991(13) 0.055(6) Uani 0.40 2 d SPU . . N2'' N 0.290(3) 0.7014(15) 0.7948(18) 0.042(9) Uani 0.20 1 d PU . . N3 N 0.3875(7) 0.7500 0.6749(4) 0.0400(16) Uani 1 2 d S . . N4 N 0.4323(7) 0.7208(4) 0.9185(4) 0.0470(11) Uani 0.50 1 d PGU . . N5 N 0.5578(7) 0.7184(4) 0.8890(4) 0.0476(12) Uani 0.50 1 d PGU . . C8 C 0.6426(6) 0.7330(4) 0.9494(4) 0.0473(12) Uani 0.50 1 d PGU . . N6 N 0.5697(6) 0.7500(6) 1.0163(4) 0.0470(11) Uani 1 2 d SGU . . C9 C 0.4397(6) 0.7368(5) 0.9971(4) 0.0469(12) Uani 0.50 1 d PGU . . O1 O 0.6672(4) 0.4336(2) 0.5847(3) 0.0599(13) Uani 1 1 d . . . O2 O 0.7324(4) 0.3419(2) 0.6302(3) 0.0508(11) Uani 1 1 d . . . O3 O 1.0081(5) 0.3199(2) 0.6961(3) 0.0580(14) Uani 1 1 d . . . O4 O 1.0145(4) 0.4222(2) 0.7196(3) 0.0518(11) Uani 1 1 d . . . O5 O 1.2668(4) 0.3755(2) 0.6492(2) 0.0473(10) Uani 1 1 d . . . O6 O 1.3580(4) 0.3910(3) 0.5305(3) 0.0638(14) Uani 1 1 d . . . O1W O 0.7521(5) 0.2500 0.7706(3) 0.0320(12) Uani 1 2 d S . . O2W O 0.5728(16) 0.7500 0.5206(6) 0.142(5) Uani 1 2 d S . . O3W O 0.4868(8) 0.2799(4) 0.6367(5) 0.054(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0248(2) 0.0532(3) 0.0472(3) 0.0063(2) -0.00086(18) -0.00449(18) Cd2 0.0310(3) 0.0311(3) 0.0279(3) 0.000 0.0012(2) 0.000 C1 0.045(4) 0.044(4) 0.050(4) 0.011(3) 0.003(3) -0.007(3) C2 0.038(3) 0.066(4) 0.040(3) 0.006(3) 0.003(3) -0.002(3) C3 0.047(4) 0.041(4) 0.055(4) 0.017(3) -0.003(3) 0.007(3) C4 0.063(5) 0.050(4) 0.108(7) 0.033(4) 0.041(5) 0.008(4) C5 0.050(4) 0.046(4) 0.094(6) 0.029(4) 0.026(4) 0.007(3) C6 0.051(4) 0.054(4) 0.041(3) 0.005(3) -0.009(3) 0.007(3) C7 0.076(9) 0.049(7) 0.030(6) 0.016(5) -0.023(6) -0.028(7) C10 0.026(3) 0.045(3) 0.038(3) 0.008(3) -0.002(2) 0.007(3) C11 0.023(3) 0.039(3) 0.030(3) 0.004(2) 0.005(2) -0.001(2) C12 0.029(3) 0.056(4) 0.046(4) 0.007(3) 0.002(3) -0.005(3) C13 0.032(3) 0.056(4) 0.038(3) 0.016(3) 0.002(3) 0.004(3) C14 0.027(3) 0.037(3) 0.035(3) 0.009(2) 0.000(2) 0.001(2) C15 0.025(3) 0.086(5) 0.041(3) 0.016(3) 0.000(3) -0.002(3) C16 0.038(7) 0.050(9) 0.038(7) 0.006(7) 0.004(6) 0.001(7) C16' 0.047(8) 0.017(6) 0.050(8) 0.003(6) 0.009(6) -0.003(6) C17 0.043(8) 0.075(12) 0.041(8) 0.006(8) -0.003(6) 0.004(9) C17' 0.038(7) 0.046(8) 0.033(7) 0.015(6) 0.002(5) 0.000(7) C18 0.032(7) 0.043(10) 0.028(7) 0.006(7) -0.004(5) 0.006(9) C18' 0.040(8) 0.030(9) 0.043(9) 0.003(7) -0.007(6) -0.002(8) N1 0.035(3) 0.049(3) 0.058(3) 0.019(3) 0.006(2) 0.006(2) N2 0.043(3) 0.043(3) 0.042(3) 0.0006(10) -0.0004(10) 0.0000(10) N2' 0.055(6) 0.055(6) 0.055(6) 0.000 -0.0001(10) 0.000 N2'' 0.042(9) 0.042(9) 0.042(9) 0.0001(10) -0.0001(10) -0.0002(10) N3 0.043(4) 0.036(4) 0.041(4) 0.000 -0.006(3) 0.000 N4 0.0501(16) 0.0466(16) 0.0444(15) 0.0000(10) 0.0004(12) -0.0004(10) N5 0.0497(14) 0.0474(14) 0.0456(14) -0.0001(8) 0.0004(9) -0.0003(8) C8 0.0503(16) 0.0471(16) 0.0446(15) -0.0001(8) 0.0007(12) -0.0004(8) N6 0.0503(16) 0.0468(17) 0.0437(16) 0.000 0.0008(13) 0.000 C9 0.0503(16) 0.0466(17) 0.0437(16) 0.0000(9) 0.0005(13) -0.0002(9) O1 0.033(2) 0.058(3) 0.089(4) 0.031(3) 0.013(2) 0.012(2) O2 0.046(3) 0.047(3) 0.059(3) 0.022(2) 0.022(2) 0.009(2) O3 0.062(3) 0.051(3) 0.061(3) 0.035(2) -0.034(2) -0.030(2) O4 0.055(3) 0.058(3) 0.042(2) -0.010(2) 0.000(2) 0.011(2) O5 0.032(2) 0.067(3) 0.043(2) 0.012(2) -0.0017(19) -0.007(2) O6 0.027(2) 0.108(4) 0.056(3) 0.012(3) 0.009(2) -0.003(2) O1W 0.034(3) 0.026(3) 0.035(3) 0.000 0.010(2) 0.000 O2W 0.235(15) 0.109(8) 0.082(7) 0.000 -0.037(9) 0.000 O3W 0.045(5) 0.057(5) 0.059(5) 0.006(4) 0.001(4) -0.009(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.217(4) 6_557 ? Cd1 O1 2.218(4) . ? Cd1 O5 2.306(4) 1_455 ? Cd1 O6 2.426(5) 1_455 ? Cd1 N1 2.449(5) . ? Cd1 O3W 2.471(9) . ? Cd1 C12 2.687(6) 1_455 ? Cd2 O3 2.283(4) . ? Cd2 O3 2.283(4) 8_565 ? Cd2 O1W 2.290(5) . ? Cd2 O2 2.305(4) 8_565 ? Cd2 O2 2.305(4) . ? C1 N1 1.337(8) . ? C1 C2 1.382(9) . ? C1 H1 0.9300 . ? C2 C3 1.378(9) . ? C2 H2 0.9300 . ? C3 C4 1.394(10) . ? C3 C6 1.456(9) . ? C4 C5 1.373(11) . ? C4 H4 0.9300 . ? C5 N1 1.325(8) . ? C5 H5 0.9300 . ? C6 N2 1.275(12) . ? C6 N3 1.348(8) . ? C6 N2'' 1.40(3) . ? C6 N2' 1.727(19) . ? C7 N2'' 1.36(3) . ? C7 N2 1.404(16) . ? C7 N4 1.448(14) . ? C7 N2' 1.63(2) . ? C10 O1 1.243(7) . ? C10 O2 1.260(7) . ? C10 C13 1.490(8) . ? C11 O3 1.239(7) . ? C11 O4 1.245(7) . ? C11 C14 1.504(7) . ? C12 O6 1.252(7) . ? C12 O5 1.265(7) . ? C12 C15 1.488(8) . ? C12 Cd1 2.687(6) 1_655 ? C13 C14 1.394(8) . ? C13 C18' 1.40(2) . ? C13 C18 1.448(18) . ? C14 C15 1.401(8) . ? C15 C16 1.425(15) . ? C15 C16' 1.448(15) . ? C16 C16' 0.763(14) . ? C16 C17 1.35(2) . ? C16 C17' 1.64(2) . ? C16' C17' 1.38(2) . ? C16' C17 1.53(2) . ? C17 C17' 0.849(17) . ? C17 C18 1.40(2) . ? C17 C18' 1.64(2) . ? C17' C18' 1.39(2) . ? C17' C18 1.51(2) . ? C18 C18' 0.639(15) . ? N2 N2' 0.737(12) . ? N2 N2 1.44(3) 8_575 ? N2 N2'' 1.78(3) 8_575 ? N2' N2 0.737(12) 8_575 ? N2' N2'' 1.05(3) . ? N2' N2'' 1.05(3) 8_575 ? N2' C7 1.63(2) 8_575 ? N2' C6 1.727(19) 8_575 ? N2'' N2 1.78(3) 8_575 ? N3 C6 1.348(8) 8_575 ? N4 N4 1.232(16) 8_575 ? N4 N5 1.351(5) . ? N4 C9 1.351(5) . ? N4 C9 1.584(11) 8_575 ? N4 N5 1.861(11) 8_575 ? N5 N5 1.330(16) 8_575 ? N5 C8 1.351(5) . ? N5 C8 1.666(12) 8_575 ? N5 N4 1.861(11) 8_575 ? C8 C8 0.71(2) 8_575 ? C8 N6 1.379(5) . ? C8 N5 1.666(10) 8_575 ? N6 C9 1.370(5) 8_575 ? N6 C9 1.370(5) . ? N6 C8 1.379(6) 8_575 ? N6 Cd2 2.306(6) 2_665 ? C9 C9 0.56(2) 8_575 ? C9 N4 1.584(10) 8_575 ? O4 Cd1 2.217(4) 6_657 ? O5 Cd1 2.306(4) 1_655 ? O6 Cd1 2.426(5) 1_655 ? O3W O3W 1.259(18) 8_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O1 108.64(19) 6_557 . ? O4 Cd1 O5 99.34(16) 6_557 1_455 ? O1 Cd1 O5 146.49(16) . 1_455 ? O4 Cd1 O6 150.25(16) 6_557 1_455 ? O1 Cd1 O6 92.24(17) . 1_455 ? O5 Cd1 O6 55.31(14) 1_455 1_455 ? O4 Cd1 N1 77.06(17) 6_557 . ? O1 Cd1 N1 85.74(17) . . ? O5 Cd1 N1 82.87(17) 1_455 . ? O6 Cd1 N1 83.84(18) 1_455 . ? O4 Cd1 O3W 110.0(2) 6_557 . ? O1 Cd1 O3W 108.5(2) . . ? O5 Cd1 O3W 77.6(2) 1_455 . ? O6 Cd1 O3W 81.7(2) 1_455 . ? N1 Cd1 O3W 160.0(2) . . ? O4 Cd1 C12 124.24(18) 6_557 1_455 ? O1 Cd1 C12 118.60(18) . 1_455 ? O5 Cd1 C12 28.05(16) 1_455 1_455 ? O6 Cd1 C12 27.76(16) 1_455 1_455 ? N1 Cd1 C12 78.60(19) . 1_455 ? O3W Cd1 C12 82.2(2) . 1_455 ? O3 Cd2 O3 80.3(2) . 8_565 ? O3 Cd2 O1W 89.06(16) . . ? O3 Cd2 O1W 89.06(16) 8_565 . ? O3 Cd2 O2 160.55(16) . 8_565 ? O3 Cd2 O2 82.00(17) 8_565 8_565 ? O1W Cd2 O2 82.74(12) . 8_565 ? O3 Cd2 O2 82.00(17) . . ? O3 Cd2 O2 160.55(16) 8_565 . ? O1W Cd2 O2 82.74(12) . . ? O2 Cd2 O2 114.2(2) 8_565 . ? O3 Cd2 N6 96.4(18) . 2_664 ? O3 Cd2 N6 96.4(15) 8_565 2_664 ? O1W Cd2 N6 172.9(16) . 2_664 ? O2 Cd2 N6 93.4(19) 8_565 2_664 ? O2 Cd2 N6 93.4(16) . 2_664 ? N1 C1 C2 123.0(6) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 116.9(6) . . ? C2 C3 C6 122.3(6) . . ? C4 C3 C6 120.8(6) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.4(7) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 N3 112.7(8) . . ? N3 C6 N2'' 126.1(15) . . ? N2 C6 C3 122.6(8) . . ? N3 C6 C3 124.6(6) . . ? N2'' C6 C3 108.4(14) . . ? C3 C6 N2' 145.0(7) . . ? N2'' C7 N4 129.5(18) . . ? N2 C7 N4 110.9(11) . . ? N4 C7 N2' 102.4(11) . . ? O1 C10 O2 120.7(5) . . ? O1 C10 C13 117.5(5) . . ? O2 C10 C13 121.7(5) . . ? O3 C11 O4 123.9(5) . . ? O3 C11 C14 120.7(5) . . ? O4 C11 C14 115.3(5) . . ? O6 C12 O5 121.7(6) . . ? O6 C12 C15 119.3(5) . . ? O5 C12 C15 119.1(5) . . ? O6 C12 Cd1 64.4(3) . 1_655 ? O5 C12 Cd1 59.0(3) . 1_655 ? C15 C12 Cd1 165.2(5) . 1_655 ? C14 C13 C18' 120.5(9) . . ? C14 C13 C18 119.4(9) . . ? C14 C13 C10 122.5(5) . . ? C18' C13 C10 115.7(9) . . ? C18 C13 C10 116.2(9) . . ? C13 C14 C15 119.0(5) . . ? C13 C14 C11 119.5(5) . . ? C15 C14 C11 121.3(5) . . ? C14 C15 C16 119.4(7) . . ? C14 C15 C16' 117.4(7) . . ? C14 C15 C12 121.5(5) . . ? C16 C15 C12 116.7(7) . . ? C16' C15 C12 119.0(7) . . ? C16' C16 C17 88(2) . . ? C16' C16 C15 76.3(17) . . ? C17 C16 C15 119.8(12) . . ? C16' C16 C17' 57.0(17) . . ? C15 C16 C17' 106.5(11) . . ? C16 C16' C17' 95(2) . . ? C16 C16' C15 72.9(16) . . ? C17' C16' C15 120.6(11) . . ? C16 C16' C17 61.9(18) . . ? C15 C16' C17 107.4(11) . . ? C17' C17 C16 93(2) . . ? C17' C17 C18 80.4(18) . . ? C16 C17 C18 121.6(14) . . ? C17' C17 C16' 63.5(16) . . ? C18 C17 C16' 113.4(14) . . ? C17' C17 C18' 58.0(16) . . ? C16 C17 C18' 115.9(14) . . ? C16' C17 C18' 97.9(13) . . ? C17 C17' C16' 83.1(17) . . ? C17 C17' C18' 90.8(18) . . ? C16' C17' C18' 119.3(13) . . ? C17 C17' C18 65.9(16) . . ? C16' C17' C18 115.8(12) . . ? C17 C17' C16 55.4(15) . . ? C18' C17' C16 113.7(12) . . ? C18 C17' C16 99.3(12) . . ? C18' C18 C17 100(4) . . ? C18' C18 C13 73(3) . . ? C17 C18 C13 118.5(14) . . ? C18' C18 C17' 67(3) . . ? C13 C18 C17' 109.6(12) . . ? C18 C18' C17' 88(3) . . ? C18 C18' C13 81(3) . . ? C17' C18' C13 119.8(15) . . ? C18 C18' C17 57(3) . . ? C13 C18' C17 106.7(13) . . ? C5 N1 C1 117.3(6) . . ? C5 N1 Cd1 121.9(4) . . ? C1 N1 Cd1 118.8(4) . . ? N2' N2 C6 116(3) . . ? N2' N2 C7 94(2) . . ? C6 N2 C7 149.5(12) . . ? C6 N2 N2 105.5(7) . 8_575 ? C7 N2 N2 102.7(8) . 8_575 ? C6 N2 N2'' 109.3(14) . 8_575 ? C7 N2 N2'' 100.7(15) . 8_575 ? N2 N2' N2 154(5) . 8_575 ? N2'' N2' N2'' 154(5) . 8_575 ? N2 N2' C7 136(3) . 8_575 ? N2 N2' C7 59.2(18) 8_575 8_575 ? N2'' N2' C7 132(2) . 8_575 ? N2'' N2' C7 56.0(18) 8_575 8_575 ? N2 N2' C7 59.2(18) . . ? N2 N2' C7 136(3) 8_575 . ? N2'' N2' C7 56.0(18) . . ? N2'' N2' C7 132(2) 8_575 . ? C7 N2' C7 78.3(14) 8_575 . ? N2'' N2' C6 127(2) . 8_575 ? N2'' N2' C6 53.9(19) 8_575 8_575 ? C7 N2' C6 100.6(6) 8_575 8_575 ? C7 N2' C6 163.5(17) . 8_575 ? N2'' N2' C6 53.9(19) . . ? N2'' N2' C6 127(2) 8_575 . ? C7 N2' C6 163.5(17) 8_575 . ? C7 N2' C6 100.6(6) . . ? C6 N2' C6 75.6(10) 8_575 . ? N2' N2'' C7 84(2) . . ? N2' N2'' C6 89(3) . . ? C7 N2'' C6 140(3) . . ? C7 N2'' N2 89.1(19) . 8_575 ? C6 N2'' N2 84.9(17) . 8_575 ? C6 N3 C6 103.5(7) . 8_575 ? N4 N4 N5 92.1(3) 8_575 . ? N4 N4 C9 75.5(4) 8_575 . ? N5 N4 C9 108.0 . . ? N4 N4 C7 106.6(6) 8_575 . ? N5 N4 C7 124.9(7) . . ? C9 N4 C7 126.7(7) . . ? N4 N4 C9 55.7(5) 8_575 8_575 ? N5 N4 C9 106.04(10) . 8_575 ? C7 N4 C9 127.5(8) . 8_575 ? N4 N4 N5 46.5(4) 8_575 8_575 ? N5 N4 N5 45.6(4) . 8_575 ? C9 N4 N5 92.61(15) . 8_575 ? C7 N4 N5 128.2(8) . 8_575 ? C9 N4 N5 78.3(5) 8_575 8_575 ? N5 N5 N4 87.9 8_575 . ? N5 N5 C8 76.8 8_575 . ? N4 N5 C8 108.0 . . ? N5 N5 C8 52.1(6) 8_575 8_575 ? N4 N5 C8 103.59(13) . 8_575 ? N5 N5 N4 46.5(4) 8_575 8_575 ? C8 N5 N4 94.2(4) . 8_575 ? C8 N5 N4 76.4(4) 8_575 8_575 ? C8 C8 N5 103.2 8_575 . ? C8 C8 N6 75.0 8_575 . ? N5 C8 N6 108.9 . . ? C8 C8 N5 52.1(5) 8_575 8_575 ? N5 C8 N5 51.0(5) . 8_575 ? N6 C8 N5 93.19(17) . 8_575 ? C9 N6 C8 105.3(4) 8_575 8_575 ? C9 N6 C8 111.64(10) . 8_575 ? C9 N6 C8 111.64(18) 8_575 . ? C9 N6 C8 105.3 . . ? C9 N6 Cd2 122.4(4) 8_575 2_665 ? C9 N6 Cd2 122.4(4) . 2_665 ? C8 N6 Cd2 125.8(5) 8_575 2_665 ? C8 N6 Cd2 125.8(4) . 2_665 ? C9 C9 N4 104.5 8_575 . ? C9 C9 N6 78.3 8_575 . ? N4 C9 N6 109.2 . . ? C9 C9 N4 55.7(6) 8_575 8_575 ? N4 C9 N4 48.8(6) . 8_575 ? N6 C9 N4 97.0(4) . 8_575 ? C10 O1 Cd1 105.4(4) . . ? C10 O2 Cd2 132.4(4) . . ? C11 O3 Cd2 121.8(4) . . ? C11 O4 Cd1 113.8(4) . 6_657 ? C12 O5 Cd1 93.0(3) . 1_655 ? C12 O6 Cd1 87.8(4) . 1_655 ? O3W O3W Cd1 174.1(2) 8_565 . ? 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 C1 C2 C3 -1.3(10) . . . . ? C1 C2 C3 C4 3.8(10) . . . . ? C1 C2 C3 C6 -176.0(6) . . . . ? C2 C3 C4 C5 -3.4(12) . . . . ? C6 C3 C4 C5 176.5(7) . . . . ? C3 C4 C5 N1 0.3(14) . . . . ? C2 C3 C6 N2 30.9(11) . . . . ? C4 C3 C6 N2 -149.0(9) . . . . ? C2 C3 C6 N3 -153.2(7) . . . . ? C4 C3 C6 N3 26.9(11) . . . . ? C2 C3 C6 N2'' 16.1(16) . . . . ? C4 C3 C6 N2'' -163.8(16) . . . . ? C2 C3 C6 N2' 26.4(19) . . . . ? C4 C3 C6 N2' -153.5(16) . . . . ? O1 C10 C13 C14 135.3(6) . . . . ? O2 C10 C13 C14 -47.0(9) . . . . ? O1 C10 C13 C18' -31.8(11) . . . . ? O2 C10 C13 C18' 145.9(9) . . . . ? O1 C10 C13 C18 -60.6(11) . . . . ? O2 C10 C13 C18 117.1(9) . . . . ? C18' C13 C14 C15 -16.9(12) . . . . ? C18 C13 C14 C15 13.0(12) . . . . ? C10 C13 C14 C15 176.7(6) . . . . ? C18' C13 C14 C11 159.0(9) . . . . ? C18 C13 C14 C11 -171.1(9) . . . . ? C10 C13 C14 C11 -7.5(9) . . . . ? O3 C11 C14 C13 90.8(7) . . . . ? O4 C11 C14 C13 -85.8(7) . . . . ? O3 C11 C14 C15 -93.4(7) . . . . ? O4 C11 C14 C15 90.0(7) . . . . ? C13 C14 C15 C16 -16.9(12) . . . . ? C11 C14 C15 C16 167.3(9) . . . . ? C13 C14 C15 C16' 18.2(11) . . . . ? C11 C14 C15 C16' -157.6(8) . . . . ? C13 C14 C15 C12 -178.9(6) . . . . ? C11 C14 C15 C12 5.3(10) . . . . ? O6 C12 C15 C14 174.5(7) . . . . ? O5 C12 C15 C14 -6.6(10) . . . . ? Cd1 C12 C15 C14 -84.8(18) 1_655 . . . ? O6 C12 C15 C16 12.1(12) . . . . ? O5 C12 C15 C16 -169.1(9) . . . . ? Cd1 C12 C15 C16 112.8(18) 1_655 . . . ? O6 C12 C15 C16' -22.7(12) . . . . ? O5 C12 C15 C16' 156.1(9) . . . . ? Cd1 C12 C15 C16' 78.0(19) 1_655 . . . ? C14 C15 C16 C16' 94.9(18) . . . . ? C12 C15 C16 C16' -102.3(17) . . . . ? C14 C15 C16 C17 15(2) . . . . ? C16' C15 C16 C17 -80(2) . . . . ? C12 C15 C16 C17 177.8(14) . . . . ? C14 C15 C16 C17' 45.9(14) . . . . ? C16' C15 C16 C17' -49.0(16) . . . . ? C12 C15 C16 C17' -151.3(9) . . . . ? C17 C16 C16' C17' 0.9(14) . . . . ? C15 C16 C16' C17' -120.4(10) . . . . ? C17 C16 C16' C15 121.3(10) . . . . ? C17' C16 C16' C15 120.4(10) . . . . ? C15 C16 C16' C17 -121.3(10) . . . . ? C17' C16 C16' C17 -0.9(14) . . . . ? C14 C15 C16' C16 -102.2(17) . . . . ? C12 C15 C16' C16 94.4(18) . . . . ? C14 C15 C16' C17' -16.2(18) . . . . ? C16 C15 C16' C17' 86(2) . . . . ? C12 C15 C16' C17' -179.6(12) . . . . ? C14 C15 C16' C17 -50.1(14) . . . . ? C16 C15 C16' C17 52.2(16) . . . . ? C12 C15 C16' C17 146.5(10) . . . . ? C16' C16 C17 C17' -1(2) . . . . ? C15 C16 C17 C17' 72(2) . . . . ? C16' C16 C17 C18 -82(3) . . . . ? C15 C16 C17 C18 -9(3) . . . . ? C17' C16 C17 C18 -81(2) . . . . ? C15 C16 C17 C16' 73.1(19) . . . . ? C17' C16 C17 C16' 1(2) . . . . ? C16' C16 C17 C18' -57(2) . . . . ? C15 C16 C17 C18' 16(3) . . . . ? C17' C16 C17 C18' -55.9(17) . . . . ? C16 C16' C17 C17' 178(3) . . . . ? C15 C16' C17 C17' 119.5(18) . . . . ? C17' C16' C17 C16 -178(3) . . . . ? C15 C16' C17 C16 -58.8(15) . . . . ? C16 C16' C17 C18 113(2) . . . . ? C17' C16' C17 C18 -65.2(18) . . . . ? C15 C16' C17 C18 54.3(19) . . . . ? C16 C16' C17 C18' 130(2) . . . . ? C17' C16' C17 C18' -48.2(15) . . . . ? C15 C16' C17 C18' 71.3(14) . . . . ? C16 C17 C17' C16' 0.8(13) . . . . ? C18 C17 C17' C16' 122.3(11) . . . . ? C18' C17 C17' C16' 119.5(13) . . . . ? C16 C17 C17' C18' -118.6(13) . . . . ? C18 C17 C17' C18' 2.9(15) . . . . ? C16' C17 C17' C18' -119.5(13) . . . . ? C16 C17 C17' C18 -121.5(13) . . . . ? C16' C17 C17' C18 -122.3(11) . . . . ? C18' C17 C17' C18 -2.9(15) . . . . ? C18 C17 C17' C16 121.5(13) . . . . ? C16' C17 C17' C16 -0.8(13) . . . . ? C18' C17 C17' C16 118.6(13) . . . . ? C16 C16' C17' C17 -1(2) . . . . ? C15 C16' C17' C17 -75(2) . . . . ? C16 C16' C17' C18' 86(2) . . . . ? C15 C16' C17' C18' 12(2) . . . . ? C17 C16' C17' C18' 87(2) . . . . ? C16 C16' C17' C18 58(2) . . . . ? C15 C16' C17' C18 -16(2) . . . . ? C17 C16' C17' C18 59.0(16) . . . . ? C15 C16' C17' C16 -73.2(17) . . . . ? C17 C16' C17' C16 1(2) . . . . ? C16' C16 C17' C17 178(3) . . . . ? C15 C16 C17' C17 -121(2) . . . . ? C17 C16 C17' C16' -178(3) . . . . ? C15 C16 C17' C16' 60.9(17) . . . . ? C16' C16 C17' C18' -108(2) . . . . ? C17 C16 C17' C18' 73.4(19) . . . . ? C15 C16 C17' C18' -47.4(18) . . . . ? C16' C16 C17' C18 -130(2) . . . . ? C17 C16 C17' C18 52.1(17) . . . . ? C15 C16 C17' C18 -68.8(14) . . . . ? C17' C17 C18 C18' -6(3) . . . . ? C16 C17 C18 C18' 82(4) . . . . ? C16' C17 C18 C18' 49(4) . . . . ? C17' C17 C18 C13 -83(2) . . . . ? C16 C17 C18 C13 5(3) . . . . ? C16' C17 C18 C13 -27(2) . . . . ? C18' C17 C18 C13 -77(3) . . . . ? C16 C17 C18 C17' 88(2) . . . . ? C16' C17 C18 C17' 55.5(16) . . . . ? C18' C17 C18 C17' 6(3) . . . . ? C14 C13 C18 C18' -100(3) . . . . ? C10 C13 C18 C18' 95(3) . . . . ? C14 C13 C18 C17 -7(2) . . . . ? C18' C13 C18 C17 93(4) . . . . ? C10 C13 C18 C17 -171.7(13) . . . . ? C14 C13 C18 C17' -42.8(15) . . . . ? C18' C13 C18 C17' 57(3) . . . . ? C10 C13 C18 C17' 152.5(10) . . . . ? C17 C17' C18 C18' 173(4) . . . . ? C16' C17' C18 C18' 105(3) . . . . ? C16 C17' C18 C18' 128(3) . . . . ? C16' C17' C18 C17 -68.7(18) . . . . ? C18' C17' C18 C17 -173(4) . . . . ? C16 C17' C18 C17 -45.3(15) . . . . ? C17 C17' C18 C13 112.2(19) . . . . ? C16' C17' C18 C13 43.5(19) . . . . ? C18' C17' C18 C13 -61(3) . . . . ? C16 C17' C18 C13 66.8(14) . . . . ? C17 C18 C18' C17' 4(2) . . . . ? C13 C18 C18' C17' 120.6(11) . . . . ? C17 C18 C18' C13 -116.8(14) . . . . ? C17' C18 C18' C13 -120.6(11) . . . . ? C13 C18 C18' C17 116.8(14) . . . . ? C17' C18 C18' C17 -4(2) . . . . ? C17 C17' C18' C18 -6(3) . . . . ? C16' C17' C18' C18 -89(3) . . . . ? C16 C17' C18' C18 -58(3) . . . . ? C17 C17' C18' C13 72(2) . . . . ? C16' C17' C18' C13 -10(2) . . . . ? C18 C17' C18' C13 78(3) . . . . ? C16 C17' C18' C13 20(2) . . . . ? C16' C17' C18' C17 -82.5(19) . . . . ? C18 C17' C18' C17 6(3) . . . . ? C16 C17' C18' C17 -52.1(15) . . . . ? C14 C13 C18' C18 95(3) . . . . ? C10 C13 C18' C18 -98(3) . . . . ? C14 C13 C18' C17' 12.7(18) . . . . ? C18 C13 C18' C17' -82(3) . . . . ? C10 C13 C18' C17' -179.9(12) . . . . ? C14 C13 C18' C17 43.7(14) . . . . ? C18 C13 C18' C17 -51(3) . . . . ? C10 C13 C18' C17 -149.0(10) . . . . ? C17' C17 C18' C18 173(4) . . . . ? C16 C17 C18' C18 -110(4) . . . . ? C16' C17 C18' C18 -136(3) . . . . ? C16 C17 C18' C17' 77(2) . . . . ? C18 C17 C18' C17' -173(4) . . . . ? C16' C17 C18' C17' 51.9(16) . . . . ? C17' C17 C18' C13 -120(2) . . . . ? C16 C17 C18' C13 -43(2) . . . . ? C18 C17 C18' C13 67(3) . . . . ? C16' C17 C18' C13 -68.6(15) . . . . ? C4 C5 N1 C1 2.3(11) . . . . ? C4 C5 N1 Cd1 -161.2(7) . . . . ? C2 C1 N1 C5 -1.8(10) . . . . ? C2 C1 N1 Cd1 162.2(5) . . . . ? O4 Cd1 N1 C5 111.8(6) 6_557 . . . ? O1 Cd1 N1 C5 1.6(6) . . . . ? O5 Cd1 N1 C5 -146.9(6) 1_455 . . . ? O6 Cd1 N1 C5 -91.2(6) 1_455 . . . ? O3W Cd1 N1 C5 -135.0(8) . . . . ? C12 Cd1 N1 C5 -118.8(6) 1_455 . . . ? O4 Cd1 N1 C1 -51.5(5) 6_557 . . . ? O1 Cd1 N1 C1 -161.8(5) . . . . ? O5 Cd1 N1 C1 49.8(5) 1_455 . . . ? O6 Cd1 N1 C1 105.5(5) 1_455 . . . ? O3W Cd1 N1 C1 61.7(9) . . . . ? C12 Cd1 N1 C1 77.9(5) 1_455 . . . ? N3 C6 N2 N2' 10(3) . . . . ? N2'' C6 N2 N2' -127(6) . . . . ? C3 C6 N2 N2' -173(3) . . . . ? N3 C6 N2 C7 -155(2) . . . . ? N2'' C6 N2 C7 68(5) . . . . ? C3 C6 N2 C7 22(3) . . . . ? N2' C6 N2 C7 -165(5) . . . . ? N3 C6 N2 N2 2.3(7) . . . 8_575 ? N2'' C6 N2 N2 -135(5) . . . 8_575 ? C3 C6 N2 N2 178.6(6) . . . 8_575 ? N2' C6 N2 N2 -8(3) . . . 8_575 ? N3 C6 N2 N2'' 13.6(16) . . . 8_575 ? N2'' C6 N2 N2'' -123(6) . . . 8_575 ? C3 C6 N2 N2'' -170.0(12) . . . 8_575 ? N2' C6 N2 N2'' 3(3) . . . 8_575 ? N2'' C7 N2 N2' 120(6) . . . . ? N4 C7 N2 N2' -76(3) . . . . ? N2'' C7 N2 C6 -74(5) . . . . ? N4 C7 N2 C6 91(2) . . . . ? N2' C7 N2 C6 167(4) . . . . ? N2'' C7 N2 N2 129(5) . . . 8_575 ? N4 C7 N2 N2 -66.4(10) . . . 8_575 ? N2' C7 N2 N2 9(2) . . . 8_575 ? N2'' C7 N2 N2'' 118(6) . . . 8_575 ? N4 C7 N2 N2'' -78.0(16) . . . 8_575 ? N2' C7 N2 N2'' -2(2) . . . 8_575 ? C6 N2 N2' N2 -38(11) . . . 8_575 ? C7 N2 N2' N2 134(10) . . . 8_575 ? N2'' N2 N2' N2 -64(19) 8_575 . . 8_575 ? C6 N2 N2' N2'' 113(7) . . . . ? C7 N2 N2' N2'' -75(6) . . . . ? N2 N2 N2' N2'' 151(9) 8_575 . . . ? N2'' N2 N2' N2'' 87(22) 8_575 . . . ? C6 N2 N2' N2'' 25(22) . . . 8_575 ? C7 N2 N2' N2'' -162(20) . . . 8_575 ? N2 N2 N2' N2'' 64(19) 8_575 . . 8_575 ? C6 N2 N2' C7 -156(3) . . . 8_575 ? C7 N2 N2' C7 17(4) . . . 8_575 ? N2 N2 N2' C7 -117(12) 8_575 . . 8_575 ? C6 N2 N2' C7 -173(2) . . . . ? N2 N2 N2' C7 -134(10) 8_575 . . . ? N2'' N2 N2' C7 162(20) 8_575 . . . ? C6 N2 N2' C6 -11(4) . . . 8_575 ? C7 N2 N2' C6 161.7(18) . . . 8_575 ? N2 N2 N2' C6 28(8) 8_575 . . 8_575 ? N2'' N2 N2' C6 -36(19) 8_575 . . 8_575 ? C7 N2 N2' C6 173(2) . . . . ? N2 N2 N2' C6 38(11) 8_575 . . . ? N2'' N2 N2' C6 -25(22) 8_575 . . . ? N2'' C7 N2' N2 -27(3) . . . . ? N4 C7 N2' N2 112(3) . . . . ? N2'' C7 N2' N2 180(6) . . . 8_575 ? N2 C7 N2' N2 -154(7) . . . 8_575 ? N4 C7 N2' N2 -42(5) . . . 8_575 ? N2 C7 N2' N2'' 27(3) . . . . ? N4 C7 N2' N2'' 139(3) . . . . ? N2'' C7 N2' N2'' 148(6) . . . 8_575 ? N2 C7 N2' N2'' 175(6) . . . 8_575 ? N4 C7 N2' N2'' -73(4) . . . 8_575 ? N2'' C7 N2' C7 165(3) . . . 8_575 ? N2 C7 N2' C7 -168(3) . . . 8_575 ? N4 C7 N2' C7 -56.2(14) . . . 8_575 ? N2'' C7 N2' C6 -107(5) . . . 8_575 ? N2 C7 N2' C6 -80(4) . . . 8_575 ? N4 C7 N2' C6 32(4) . . . 8_575 ? N2'' C7 N2' C6 -32(2) . . . . ? N2 C7 N2' C6 -5.1(16) . . . . ? N4 C7 N2' C6 106.9(12) . . . . ? N3 C6 N2' N2 -170(3) . . . . ? N2'' C6 N2' N2 26(3) . . . . ? C3 C6 N2' N2 10(4) . . . . ? N2 C6 N2' N2 163(6) . . . 8_575 ? N3 C6 N2' N2 -8(3) . . . 8_575 ? N2'' C6 N2' N2 -171(5) . . . 8_575 ? C3 C6 N2' N2 173(2) . . . 8_575 ? N2 C6 N2' N2'' -26(3) . . . . ? N3 C6 N2' N2'' 164(2) . . . . ? C3 C6 N2' N2'' -16(3) . . . . ? N2 C6 N2' N2'' -174(6) . . . 8_575 ? N3 C6 N2' N2'' 16(3) . . . 8_575 ? N2'' C6 N2' N2'' -147(6) . . . 8_575 ? C3 C6 N2' N2'' -164(3) . . . 8_575 ? N2 C6 N2' C7 91(5) . . . 8_575 ? N3 C6 N2' C7 -79(4) . . . 8_575 ? N2'' C6 N2' C7 117(5) . . . 8_575 ? C3 C6 N2' C7 101(4) . . . 8_575 ? N2 C6 N2' C7 7(2) . . . . ? N3 C6 N2' C7 -163.8(11) . . . . ? N2'' C6 N2' C7 33(2) . . . . ? C3 C6 N2' C7 17(2) . . . . ? N2 C6 N2' C6 170(3) . . . 8_575 ? N3 C6 N2' C6 -0.3(8) . . . 8_575 ? N2'' C6 N2' C6 -164(3) . . . 8_575 ? C3 C6 N2' C6 -180.0(9) . . . 8_575 ? N2 N2' N2'' C7 91(6) . . . . ? N2'' N2' N2'' C7 -118(9) 8_575 . . . ? C7 N2' N2'' C7 -20(4) 8_575 . . . ? C6 N2' N2'' C7 160(2) 8_575 . . . ? C6 N2' N2'' C7 140(2) . . . . ? N2 N2' N2'' C6 -49(6) . . . . ? N2 N2' N2'' C6 41(21) 8_575 . . . ? N2'' N2' N2'' C6 102(9) 8_575 . . . ? C7 N2' N2'' C6 -160(3) 8_575 . . . ? C7 N2' N2'' C6 -140(2) . . . . ? C6 N2' N2'' C6 20(3) 8_575 . . . ? N2 N2' N2'' N2 -90(22) . . . 8_575 ? N2'' N2' N2'' N2 62(18) 8_575 . . 8_575 ? C6 N2' N2'' N2 -21(18) 8_575 . . 8_575 ? C6 N2' N2'' N2 -41(21) . . . 8_575 ? N2 C7 N2'' N2' -38(4) . . . . ? N4 C7 N2'' N2' -57(3) . . . . ? N2 C7 N2'' C6 43(4) . . . . ? N4 C7 N2'' C6 24(5) . . . . ? N2' C7 N2'' C6 81(4) . . . . ? N2 C7 N2'' N2 -38(4) . . . 8_575 ? N4 C7 N2'' N2 -57(2) . . . 8_575 ? N2' C7 N2'' N2 -0.1(17) . . . 8_575 ? N2 C6 N2'' N2' 31(4) . . . . ? N3 C6 N2'' N2' -21(3) . . . . ? C3 C6 N2'' N2' 170.3(19) . . . . ? N2 C6 N2'' C7 -49(4) . . . . ? N3 C6 N2'' C7 -100(4) . . . . ? C3 C6 N2'' C7 91(4) . . . . ? N2' C6 N2'' C7 -79(4) . . . . ? N2 C6 N2'' N2 34(4) . . . 8_575 ? N3 C6 N2'' N2 -17(2) . . . 8_575 ? C3 C6 N2'' N2 173.6(8) . . . 8_575 ? N2' C6 N2'' N2 3.2(17) . . . 8_575 ? N2 C6 N3 C6 -3.6(11) . . . 8_575 ? N2'' C6 N3 C6 13(2) . . . 8_575 ? C3 C6 N3 C6 -179.8(4) . . . 8_575 ? N2' C6 N3 C6 0.4(11) . . . 8_575 ? N2'' C7 N4 N4 76(2) . . . 8_575 ? N2 C7 N4 N4 68.9(11) . . . 8_575 ? N2' C7 N4 N4 42.3(11) . . . 8_575 ? N2'' C7 N4 N5 -29(2) . . . . ? N2 C7 N4 N5 -35.8(14) . . . . ? N2' C7 N4 N5 -62.4(13) . . . . ? N2'' C7 N4 C9 160(2) . . . . ? N2 C7 N4 C9 152.9(10) . . . . ? N2' C7 N4 C9 126.3(10) . . . . ? N2'' C7 N4 C9 135(2) . . . 8_575 ? N2 C7 N4 C9 128.0(11) . . . 8_575 ? N2' C7 N4 C9 101.4(12) . . . 8_575 ? N2'' C7 N4 N5 28(3) . . . 8_575 ? N2 C7 N4 N5 21.7(16) . . . 8_575 ? N2' C7 N4 N5 -4.9(15) . . . 8_575 ? N4 N4 N5 N5 0.0(4) 8_575 . . 8_575 ? C9 N4 N5 N5 -75.4 . . . 8_575 ? C7 N4 N5 N5 111.9(10) . . . 8_575 ? C9 N4 N5 N5 -54.8(7) 8_575 . . 8_575 ? N4 N4 N5 C8 75.4(4) 8_575 . . . ? C9 N4 N5 C8 0.0 . . . . ? C7 N4 N5 C8 -172.6(10) . . . . ? C9 N4 N5 C8 20.7(7) 8_575 . . . ? N5 N4 N5 C8 75.4 8_575 . . . ? N4 N4 N5 C8 50.2(5) 8_575 . . 8_575 ? C9 N4 N5 C8 -25.3(6) . . . 8_575 ? C7 N4 N5 C8 162.1(9) . . . 8_575 ? C9 N4 N5 C8 -4.6(7) 8_575 . . 8_575 ? N5 N4 N5 C8 50.2(6) 8_575 . . 8_575 ? C9 N4 N5 N4 -75.4(4) . . . 8_575 ? C7 N4 N5 N4 111.9(8) . . . 8_575 ? C9 N4 N5 N4 -54.8(5) 8_575 . . 8_575 ? N5 N4 N5 N4 0.0(4) 8_575 . . 8_575 ? N5 N5 C8 C8 0.0 8_575 . . 8_575 ? N4 N5 C8 C8 -83.4 . . . 8_575 ? N4 N5 C8 C8 -43.4(4) 8_575 . . 8_575 ? N5 N5 C8 N6 78.4 8_575 . . . ? N4 N5 C8 N6 -5.0 . . . . ? C8 N5 C8 N6 78.4 8_575 . . . ? N4 N5 C8 N6 34.9(4) 8_575 . . . ? N4 N5 C8 N5 -83.4 . . . 8_575 ? C8 N5 C8 N5 0.0 8_575 . . 8_575 ? N4 N5 C8 N5 -43.4(4) 8_575 . . 8_575 ? C8 C8 N6 C9 83.1(9) 8_575 . . 8_575 ? N5 C8 N6 C9 -15.9(9) . . . 8_575 ? N5 C8 N6 C9 33.8(10) 8_575 . . 8_575 ? C8 C8 N6 C9 106.9 8_575 . . . ? N5 C8 N6 C9 7.9 . . . . ? N5 C8 N6 C9 57.6(4) 8_575 . . . ? N5 C8 N6 C8 -99.0 . . . 8_575 ? N5 C8 N6 C8 -49.4(4) 8_575 . . 8_575 ? C8 C8 N6 Cd2 -101.2(9) 8_575 . . 2_665 ? N5 C8 N6 Cd2 159.8(9) . . . 2_665 ? N5 C8 N6 Cd2 -150.5(9) 8_575 . . 2_665 ? N4 N4 C9 C9 0.0(3) 8_575 . . 8_575 ? N5 N4 C9 C9 87.5 . . . 8_575 ? C7 N4 C9 C9 -100.1(11) . . . 8_575 ? N5 N4 C9 C9 43.7(4) 8_575 . . 8_575 ? N4 N4 C9 N6 -82.4(3) 8_575 . . . ? N5 N4 C9 N6 5.0 . . . . ? C7 N4 C9 N6 177.5(10) . . . . ? C9 N4 C9 N6 -82.4 8_575 . . . ? N5 N4 C9 N6 -38.7(3) 8_575 . . . ? N5 N4 C9 N4 87.5(3) . . . 8_575 ? C7 N4 C9 N4 -100.1(9) . . . 8_575 ? C9 N4 C9 N4 0.0(3) 8_575 . . 8_575 ? N5 N4 C9 N4 43.7(4) 8_575 . . 8_575 ? C8 N6 C9 C9 -78.3(9) 8_575 . . 8_575 ? C8 N6 C9 C9 -109.3 . . . 8_575 ? Cd2 N6 C9 C9 97.6(9) 2_665 . . 8_575 ? C9 N6 C9 N4 101.4 8_575 . . . ? C8 N6 C9 N4 23.1(9) 8_575 . . . ? C8 N6 C9 N4 -7.9 . . . . ? Cd2 N6 C9 N4 -161.0(9) 2_665 . . . ? C9 N6 C9 N4 52.7(5) 8_575 . . 8_575 ? C8 N6 C9 N4 -25.6(11) 8_575 . . 8_575 ? C8 N6 C9 N4 -56.6(5) . . . 8_575 ? Cd2 N6 C9 N4 150.3(7) 2_665 . . 8_575 ? O2 C10 O1 Cd1 -0.2(7) . . . . ? C13 C10 O1 Cd1 177.6(4) . . . . ? O4 Cd1 O1 C10 85.7(4) 6_557 . . . ? O5 Cd1 O1 C10 -129.2(4) 1_455 . . . ? O6 Cd1 O1 C10 -115.8(4) 1_455 . . . ? N1 Cd1 O1 C10 160.5(4) . . . . ? O3W Cd1 O1 C10 -33.8(5) . . . . ? C12 Cd1 O1 C10 -124.9(4) 1_455 . . . ? O1 C10 O2 Cd2 173.1(4) . . . . ? C13 C10 O2 Cd2 -4.6(9) . . . . ? O3 Cd2 O2 C10 58.4(6) . . . . ? O3 Cd2 O2 C10 82.7(8) 8_565 . . . ? O1W Cd2 O2 C10 148.5(6) . . . . ? O2 Cd2 O2 C10 -132.9(5) 8_565 . . . ? N6 Cd2 O2 C10 -37.6(18) 2_664 . . . ? O4 C11 O3 Cd2 129.1(5) . . . . ? C14 C11 O3 Cd2 -47.3(7) . . . . ? O3 Cd2 O3 C11 160.3(4) 8_565 . . . ? O1W Cd2 O3 C11 -110.5(5) . . . . ? O2 Cd2 O3 C11 -175.3(4) 8_565 . . . ? O2 Cd2 O3 C11 -27.7(5) . . . . ? N6 Cd2 O3 C11 64.9(17) 2_664 . . . ? O3 C11 O4 Cd1 -5.1(7) . . . 6_657 ? C14 C11 O4 Cd1 171.4(3) . . . 6_657 ? O6 C12 O5 Cd1 15.7(7) . . . 1_655 ? C15 C12 O5 Cd1 -163.1(6) . . . 1_655 ? O5 C12 O6 Cd1 -14.9(7) . . . 1_655 ? C15 C12 O6 Cd1 163.9(6) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.106 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.109 #========================================================== data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 872134' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H16 N8 O4 Zn' _chemical_formula_sum 'C23 H16 N8 O4 Zn' _chemical_formula_weight 533.81 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 monoclinic _symmetry_space_group_name_H-M p21/n _symmetry_space_group_name_hall '-P 2yn' 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 10.1516(4) _cell_length_b 16.5563(7) _cell_length_c 13.2469(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.846(4) _cell_angle_gamma 90.00 _cell_volume 2199.96(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3059 _cell_measurement_theta_min 3.1063 _cell_measurement_theta_max 29.2255 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80164 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8329 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4006 _reflns_number_gt 3120 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0407P)^2^+0.4442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4006 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Zn1 Zn 0.42756(3) 0.11247(2) 0.51135(2) 0.02706(13) Uani 1 1 d . . . C1 C 0.0490(3) -0.20951(19) 0.0329(2) 0.0334(7) Uani 1 1 d . . . H1 H -0.0124 -0.2278 0.0730 0.040 Uiso 1 1 calc R . . C2 C 0.0856(3) -0.12925(18) 0.0397(2) 0.0328(7) Uani 1 1 d . . . H2 H 0.0500 -0.0947 0.0838 0.039 Uiso 1 1 calc R . . C3 C 0.1762(3) -0.10099(17) -0.0201(2) 0.0278(7) Uani 1 1 d . . . C4 C 0.2250(3) -0.15489(19) -0.0851(2) 0.0358(7) Uani 1 1 d . . . H4 H 0.2852 -0.1379 -0.1270 0.043 Uiso 1 1 calc R . . C5 C 0.1832(3) -0.23394(19) -0.0869(2) 0.0358(7) Uani 1 1 d . . . H5 H 0.2165 -0.2695 -0.1311 0.043 Uiso 1 1 calc R . . C6 C 0.2238(3) -0.01698(18) -0.0151(2) 0.0295(7) Uani 1 1 d . . . C7 C 0.3241(3) 0.08719(18) -0.0533(2) 0.0280(7) Uani 1 1 d . . . C8 C 0.4038(3) 0.14352(18) -0.1057(2) 0.0283(7) Uani 1 1 d . . . C9 C 0.3774(3) 0.22516(18) -0.1167(2) 0.0336(7) Uani 1 1 d . . . H9 H 0.3072 0.2485 -0.0896 0.040 Uiso 1 1 calc R . . C10 C 0.4585(3) 0.2715(2) -0.1695(2) 0.0415(8) Uani 1 1 d . . . H10 H 0.4408 0.3265 -0.1760 0.050 Uiso 1 1 calc R . . C11 C 0.5817(3) 0.1635(2) -0.2004(3) 0.0468(9) Uani 1 1 d . . . H11 H 0.6518 0.1415 -0.2289 0.056 Uiso 1 1 calc R . . C12 C 0.5071(3) 0.1121(2) -0.1497(2) 0.0383(8) Uani 1 1 d . . . H12 H 0.5263 0.0571 -0.1453 0.046 Uiso 1 1 calc R . . C13 C 0.2828(3) 0.16921(18) 0.1024(2) 0.0336(7) Uani 1 1 d . . . H13A H 0.3303 0.2128 0.0748 0.040 Uiso 1 1 calc R . . H13B H 0.1964 0.1895 0.1132 0.040 Uiso 1 1 calc R . . C14 C 0.3229(3) 0.14451(17) 0.2906(2) 0.0272(6) Uani 1 1 d . . . H14 H 0.2430 0.1649 0.3059 0.033 Uiso 1 1 calc R . . C15 C 0.5122(3) 0.0913(2) 0.2993(2) 0.0378(8) Uani 1 1 d . . . H15 H 0.5921 0.0665 0.3262 0.045 Uiso 1 1 calc R . . C16 C 0.6973(3) 0.10536(17) 0.5569(2) 0.0256(6) Uani 1 1 d . . . C17 C 1.1842(3) 0.08674(18) 0.5485(2) 0.0289(7) Uani 1 1 d . . . C18 C 0.8322(3) 0.07563(17) 0.6067(2) 0.0245(6) Uani 1 1 d . . . C19 C 0.8485(3) 0.02892(18) 0.6946(2) 0.0281(6) Uani 1 1 d . . . H19 H 0.7747 0.0153 0.7249 0.034 Uiso 1 1 calc R . . C20 C 0.9734(3) 0.00268(19) 0.7371(2) 0.0324(7) Uani 1 1 d . . . H20 H 0.9839 -0.0274 0.7971 0.039 Uiso 1 1 calc R . . C21 C 1.0838(3) 0.02074(19) 0.6911(2) 0.0308(7) Uani 1 1 d . . . H21 H 1.1677 0.0020 0.7196 0.037 Uiso 1 1 calc R . . C22 C 1.0687(3) 0.06681(17) 0.6026(2) 0.0246(6) Uani 1 1 d . . . C23 C 0.9434(3) 0.09404(17) 0.5618(2) 0.0265(6) Uani 1 1 d . . . H23 H 0.9331 0.1254 0.5029 0.032 Uiso 1 1 calc R . . N1 N 0.0974(2) -0.26252(15) -0.02866(17) 0.0297(6) Uani 1 1 d . . . N2 N 0.2985(2) 0.01244(15) -0.08379(17) 0.0312(6) Uani 1 1 d . . . N3 N 0.2006(2) 0.03483(15) 0.05591(18) 0.0323(6) Uani 1 1 d . . . N4 N 0.2651(2) 0.10246(14) 0.03040(17) 0.0295(6) Uani 1 1 d . . . N5 N 0.5599(3) 0.24244(19) -0.2111(2) 0.0451(7) Uani 1 1 d . . . N6 N 0.3572(2) 0.14251(15) 0.19864(17) 0.0290(6) Uani 1 1 d . . . N7 N 0.4801(3) 0.10830(18) 0.20196(19) 0.0435(7) Uani 1 1 d . . . N8 N 0.4190(2) 0.11317(14) 0.35748(17) 0.0252(5) Uani 1 1 d . . . O1 O 0.59621(17) 0.06681(13) 0.57947(14) 0.0321(5) Uani 1 1 d . . . O2 O 0.68892(19) 0.16285(13) 0.49762(17) 0.0389(5) Uani 1 1 d . . . O3 O 1.1654(2) 0.12477(14) 0.46821(16) 0.0400(6) Uani 1 1 d . . . O4 O 1.30075(17) 0.06429(13) 0.59195(15) 0.0345(5) 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 0.02028(19) 0.0321(2) 0.0293(2) 0.00643(15) 0.00535(13) 0.00457(14) C1 0.0280(16) 0.0342(18) 0.0390(17) 0.0009(15) 0.0085(13) -0.0026(14) C2 0.0278(16) 0.0323(18) 0.0382(17) -0.0027(14) 0.0049(13) -0.0013(13) C3 0.0260(15) 0.0267(16) 0.0294(15) 0.0005(13) 0.0001(12) -0.0022(13) C4 0.0419(18) 0.0329(18) 0.0348(17) 0.0006(15) 0.0127(14) -0.0043(15) C5 0.0422(19) 0.0329(18) 0.0336(16) -0.0004(15) 0.0102(14) -0.0019(15) C6 0.0303(16) 0.0261(16) 0.0305(15) 0.0016(14) -0.0003(13) -0.0010(13) C7 0.0267(15) 0.0316(18) 0.0251(14) -0.0003(13) 0.0023(12) 0.0002(13) C8 0.0312(16) 0.0263(16) 0.0268(15) -0.0047(13) 0.0027(13) -0.0021(13) C9 0.0383(18) 0.0303(18) 0.0337(16) -0.0023(14) 0.0103(14) -0.0015(14) C10 0.055(2) 0.0309(19) 0.0391(18) -0.0027(15) 0.0094(16) -0.0090(16) C11 0.0372(19) 0.058(3) 0.048(2) -0.0098(19) 0.0184(16) -0.0022(17) C12 0.0389(18) 0.0324(18) 0.0452(18) -0.0079(16) 0.0114(15) 0.0018(15) C13 0.0480(19) 0.0246(16) 0.0278(15) 0.0008(13) 0.0051(13) 0.0046(14) C14 0.0231(15) 0.0277(16) 0.0317(15) -0.0026(13) 0.0071(12) 0.0024(12) C15 0.0295(17) 0.047(2) 0.0373(17) -0.0002(16) 0.0054(13) 0.0133(15) C16 0.0197(15) 0.0263(16) 0.0311(15) -0.0044(13) 0.0049(12) 0.0013(12) C17 0.0209(15) 0.0330(17) 0.0335(16) -0.0064(14) 0.0060(12) 0.0008(13) C18 0.0176(14) 0.0265(16) 0.0296(14) -0.0006(13) 0.0045(11) 0.0008(12) C19 0.0213(14) 0.0321(17) 0.0318(15) 0.0027(14) 0.0075(12) -0.0016(13) C20 0.0281(16) 0.0379(18) 0.0313(15) 0.0074(14) 0.0049(12) 0.0043(14) C21 0.0184(14) 0.0414(19) 0.0315(15) 0.0023(14) 0.0007(12) 0.0055(13) C22 0.0182(14) 0.0287(16) 0.0268(14) -0.0068(13) 0.0033(11) -0.0003(12) C23 0.0218(15) 0.0307(17) 0.0265(14) 0.0034(13) 0.0026(11) 0.0017(12) N1 0.0297(13) 0.0274(14) 0.0320(13) 0.0004(11) 0.0048(11) -0.0031(11) N2 0.0360(14) 0.0279(15) 0.0302(13) -0.0001(11) 0.0063(11) -0.0026(11) N3 0.0354(14) 0.0273(14) 0.0348(13) 0.0022(12) 0.0074(11) -0.0023(11) N4 0.0360(14) 0.0249(14) 0.0278(12) 0.0025(11) 0.0052(11) 0.0004(11) N5 0.0467(18) 0.049(2) 0.0427(16) -0.0077(14) 0.0170(13) -0.0161(14) N6 0.0285(13) 0.0305(14) 0.0286(13) -0.0008(11) 0.0058(10) 0.0060(11) N7 0.0371(16) 0.059(2) 0.0370(15) 0.0025(14) 0.0137(12) 0.0168(14) N8 0.0233(12) 0.0254(13) 0.0279(12) -0.0028(11) 0.0066(10) 0.0019(10) O1 0.0147(10) 0.0395(13) 0.0427(11) 0.0090(10) 0.0063(8) -0.0001(9) O2 0.0249(11) 0.0351(13) 0.0558(13) 0.0167(11) 0.0029(10) 0.0009(9) O3 0.0271(11) 0.0597(16) 0.0348(12) 0.0111(11) 0.0098(9) -0.0003(10) O4 0.0164(10) 0.0440(13) 0.0444(11) 0.0074(11) 0.0088(9) 0.0031(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.9601(18) . ? Zn1 O4 1.9637(19) 1_455 ? Zn1 N8 2.027(2) . ? Zn1 N1 2.102(2) 2 ? C1 N1 1.341(4) . ? C1 C2 1.379(4) . ? C1 H1 0.9300 . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 C6 1.471(4) . ? C4 C5 1.375(4) . ? C4 H4 0.9300 . ? C5 N1 1.336(4) . ? C5 H5 0.9300 . ? C6 N3 1.321(4) . ? C6 N2 1.361(4) . ? C7 N2 1.315(4) . ? C7 N4 1.363(4) . ? C7 C8 1.476(4) . ? C8 C12 1.377(4) . ? C8 C9 1.381(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C10 N5 1.330(4) . ? C10 H10 0.9300 . ? C11 N5 1.329(5) . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N6 1.448(3) . ? C13 N4 1.453(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N6 1.317(3) . ? C14 N8 1.319(3) . ? C14 H14 0.9300 . ? C15 N7 1.311(4) . ? C15 N8 1.358(4) . ? C15 H15 0.9300 . ? C16 O2 1.228(3) . ? C16 O1 1.282(3) . ? C16 C18 1.509(4) . ? C17 O3 1.226(3) . ? C17 O4 1.288(3) . ? C17 C22 1.502(4) . ? C18 C19 1.386(4) . ? C18 C23 1.389(4) . ? C19 C20 1.376(4) . ? C19 H19 0.9300 . ? C20 C21 1.388(4) . ? C20 H20 0.9300 . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C22 C23 1.379(4) . ? C23 H23 0.9300 . ? N1 Zn1 2.102(2) 2_545 ? N3 N4 1.365(3) . ? N6 N7 1.365(3) . ? O4 Zn1 1.9637(19) 1_655 ? 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 O4 101.09(8) . 1_455 ? O1 Zn1 N8 111.38(9) . . ? O4 Zn1 N8 128.23(9) 1_455 . ? O1 Zn1 N1 116.15(9) . 2 ? O4 Zn1 N1 103.93(9) 1_455 2 ? N8 Zn1 N1 96.71(9) . 2 ? N1 C1 C2 123.4(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 118.1(3) . . ? C2 C3 C6 122.5(3) . . ? C4 C3 C6 119.4(3) . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N3 C6 N2 115.0(3) . . ? N3 C6 C3 123.5(3) . . ? N2 C6 C3 121.5(3) . . ? N2 C7 N4 109.5(3) . . ? N2 C7 C8 123.2(3) . . ? N4 C7 C8 127.4(3) . . ? C12 C8 C9 118.3(3) . . ? C12 C8 C7 117.9(3) . . ? C9 C8 C7 123.8(3) . . ? C8 C9 C10 118.2(3) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N5 C10 C9 124.4(3) . . ? N5 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N5 C11 C12 124.3(3) . . ? N5 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C8 C12 C11 118.8(3) . . ? C8 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N6 C13 N4 109.9(2) . . ? N6 C13 H13A 109.7 . . ? N4 C13 H13A 109.7 . . ? N6 C13 H13B 109.7 . . ? N4 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N6 C14 N8 109.8(3) . . ? N6 C14 H14 125.1 . . ? N8 C14 H14 125.1 . . ? N7 C15 N8 114.3(3) . . ? N7 C15 H15 122.8 . . ? N8 C15 H15 122.8 . . ? O2 C16 O1 123.8(2) . . ? O2 C16 C18 120.1(2) . . ? O1 C16 C18 116.1(2) . . ? O3 C17 O4 123.1(3) . . ? O3 C17 C22 119.9(2) . . ? O4 C17 C22 117.0(2) . . ? C19 C18 C23 118.9(2) . . ? C19 C18 C16 122.2(2) . . ? C23 C18 C16 118.9(2) . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 119.8(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.1(2) . . ? C23 C22 C17 118.8(2) . . ? C21 C22 C17 122.1(2) . . ? C22 C23 C18 121.5(3) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C5 N1 C1 116.8(3) . . ? C5 N1 Zn1 120.8(2) . 2_545 ? C1 N1 Zn1 121.1(2) . 2_545 ? C7 N2 C6 103.6(2) . . ? C6 N3 N4 102.2(2) . . ? C7 N4 N3 109.7(2) . . ? C7 N4 C13 130.5(3) . . ? N3 N4 C13 118.5(2) . . ? C11 N5 C10 116.0(3) . . ? C14 N6 N7 110.5(2) . . ? C14 N6 C13 129.1(3) . . ? N7 N6 C13 120.4(2) . . ? C15 N7 N6 102.0(2) . . ? C14 N8 C15 103.3(2) . . ? C14 N8 Zn1 126.23(19) . . ? C15 N8 Zn1 130.05(19) . . ? C16 O1 Zn1 111.97(17) . . ? C17 O4 Zn1 105.89(18) . 1_655 ? 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 C1 C2 C3 0.4(4) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C1 C2 C3 C6 -178.0(3) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C6 C3 C4 C5 177.9(3) . . . . ? C3 C4 C5 N1 -0.2(5) . . . . ? C2 C3 C6 N3 10.3(4) . . . . ? C4 C3 C6 N3 -168.3(3) . . . . ? C2 C3 C6 N2 -171.0(3) . . . . ? C4 C3 C6 N2 10.4(4) . . . . ? N2 C7 C8 C12 -33.9(4) . . . . ? N4 C7 C8 C12 146.9(3) . . . . ? N2 C7 C8 C9 143.4(3) . . . . ? N4 C7 C8 C9 -35.8(4) . . . . ? C12 C8 C9 C10 -1.5(4) . . . . ? C7 C8 C9 C10 -178.8(3) . . . . ? C8 C9 C10 N5 0.6(5) . . . . ? C9 C8 C12 C11 1.6(4) . . . . ? C7 C8 C12 C11 179.0(3) . . . . ? N5 C11 C12 C8 -0.8(5) . . . . ? O2 C16 C18 C19 160.3(3) . . . . ? O1 C16 C18 C19 -20.4(4) . . . . ? O2 C16 C18 C23 -21.2(4) . . . . ? O1 C16 C18 C23 158.0(3) . . . . ? C23 C18 C19 C20 1.1(4) . . . . ? C16 C18 C19 C20 179.6(3) . . . . ? C18 C19 C20 C21 -1.7(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C20 C21 C22 C17 -178.7(3) . . . . ? O3 C17 C22 C23 -1.9(4) . . . . ? O4 C17 C22 C23 176.1(3) . . . . ? O3 C17 C22 C21 177.0(3) . . . . ? O4 C17 C22 C21 -5.0(4) . . . . ? C21 C22 C23 C18 -0.7(4) . . . . ? C17 C22 C23 C18 178.2(3) . . . . ? C19 C18 C23 C22 0.1(4) . . . . ? C16 C18 C23 C22 -178.4(3) . . . . ? C4 C5 N1 C1 1.2(4) . . . . ? C4 C5 N1 Zn1 -166.0(2) . . . 2_545 ? C2 C1 N1 C5 -1.4(4) . . . . ? C2 C1 N1 Zn1 165.8(2) . . . 2_545 ? N4 C7 N2 C6 -0.7(3) . . . . ? C8 C7 N2 C6 180.0(3) . . . . ? N3 C6 N2 C7 0.3(3) . . . . ? C3 C6 N2 C7 -178.4(2) . . . . ? N2 C6 N3 N4 0.2(3) . . . . ? C3 C6 N3 N4 178.9(2) . . . . ? N2 C7 N4 N3 0.9(3) . . . . ? C8 C7 N4 N3 -179.8(3) . . . . ? N2 C7 N4 C13 167.4(3) . . . . ? C8 C7 N4 C13 -13.4(5) . . . . ? C6 N3 N4 C7 -0.7(3) . . . . ? C6 N3 N4 C13 -169.0(2) . . . . ? N6 C13 N4 C7 -106.5(3) . . . . ? N6 C13 N4 N3 58.9(3) . . . . ? C12 C11 N5 C10 -0.1(5) . . . . ? C9 C10 N5 C11 0.2(5) . . . . ? N8 C14 N6 N7 0.4(4) . . . . ? N8 C14 N6 C13 179.2(3) . . . . ? N4 C13 N6 C14 -122.0(3) . . . . ? N4 C13 N6 N7 56.6(4) . . . . ? N8 C15 N7 N6 -0.6(4) . . . . ? C14 N6 N7 C15 0.1(4) . . . . ? C13 N6 N7 C15 -178.7(3) . . . . ? N6 C14 N8 C15 -0.8(3) . . . . ? N6 C14 N8 Zn1 172.73(18) . . . . ? N7 C15 N8 C14 0.9(4) . . . . ? N7 C15 N8 Zn1 -172.3(2) . . . . ? O1 Zn1 N8 C14 -175.4(2) . . . . ? O4 Zn1 N8 C14 59.7(3) 1_455 . . . ? N1 Zn1 N8 C14 -53.9(2) 2 . . . ? O1 Zn1 N8 C15 -3.7(3) . . . . ? O4 Zn1 N8 C15 -128.5(3) 1_455 . . . ? N1 Zn1 N8 C15 117.8(3) 2 . . . ? O2 C16 O1 Zn1 -1.6(4) . . . . ? C18 C16 O1 Zn1 179.16(18) . . . . ? O4 Zn1 O1 C16 -163.42(18) 1_455 . . . ? N8 Zn1 O1 C16 57.7(2) . . . . ? N1 Zn1 O1 C16 -51.7(2) 2 . . . ? O3 C17 O4 Zn1 5.4(4) . . . 1_655 ? C22 C17 O4 Zn1 -172.5(2) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.323 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.068 #========================================================== data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 872135' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H47 N16 O17.50 Zn3' _chemical_formula_sum 'C54 H47 N16 O17.50 Zn3' _chemical_formula_weight 1396.19 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_hall '-C 2yc' 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 35.7465(14) _cell_length_b 11.2708(3) _cell_length_c 14.9426(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.934(4) _cell_angle_gamma 90.00 _cell_volume 5759.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5220 _cell_measurement_theta_min 2.8442 _cell_measurement_theta_max 29.1278 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2852 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90176 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17397 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5277 _reflns_number_gt 4142 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For O4W, some anisotropic displacement ellipsoids were rather elongated, which led us to use the ISOR restraints. ; _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^)+(0.0525P)^2^+4.0107P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5277 _refine_ls_number_parameters 417 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.049 _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 Zn1 Zn 0.154742(10) -0.34789(3) 0.42500(2) 0.02217(12) Uani 1 1 d . . . Zn2 Zn 0.2500 -0.2500 0.5000 0.02144(14) Uani 1 2 d S . . C1 C 0.09089(9) -0.5351(3) 0.3863(2) 0.0314(8) Uani 1 1 d . . . H1 H 0.1108 -0.5863 0.3826 0.038 Uiso 1 1 calc R . . C2 C 0.05416(10) -0.5808(3) 0.3737(2) 0.0336(8) Uani 1 1 d . . . H2 H 0.0493 -0.6610 0.3610 0.040 Uiso 1 1 calc R . . C3 C 0.02440(10) -0.5057(3) 0.3802(2) 0.0331(8) Uani 1 1 d . . . C4 C 0.03276(10) -0.3873(3) 0.3976(3) 0.0399(9) Uani 1 1 d . . . H4 H 0.0133 -0.3346 0.4017 0.048 Uiso 1 1 calc R . . C5 C 0.07026(10) -0.3483(3) 0.4089(3) 0.0366(8) Uani 1 1 d . . . H5 H 0.0756 -0.2681 0.4207 0.044 Uiso 1 1 calc R . . C6 C -0.01549(9) -0.5526(3) 0.3685(2) 0.0334(8) Uani 1 1 d . . . C7 C -0.07626(10) -0.5581(3) 0.3502(2) 0.0353(8) Uani 1 1 d . . . C8 C -0.11714(10) -0.5225(4) 0.3402(2) 0.0372(9) Uani 1 1 d . . . C9 C -0.12361(11) -0.4201(4) 0.3849(3) 0.0429(9) Uani 1 1 d . . . H9 H -0.1028 -0.3747 0.4200 0.051 Uiso 1 1 calc R . . C10 C -0.16176(12) -0.3871(4) 0.3759(3) 0.0514(11) Uani 1 1 d . . . H10 H -0.1658 -0.3187 0.4065 0.062 Uiso 1 1 calc R . . C11 C -0.18622(11) -0.5441(4) 0.2832(3) 0.0528(11) Uani 1 1 d . . . H11 H -0.2077 -0.5871 0.2481 0.063 Uiso 1 1 calc R . . C12 C -0.14924(10) -0.5854(4) 0.2872(3) 0.0448(10) Uani 1 1 d . . . H12 H -0.1461 -0.6536 0.2551 0.054 Uiso 1 1 calc R . . C13 C -0.08055(12) -0.7839(4) 0.3518(3) 0.0520(11) Uani 1 1 d . . . H13A H -0.0644 -0.8324 0.4018 0.062 Uiso 1 1 calc R . . H13B H -0.1057 -0.7736 0.3631 0.062 Uiso 1 1 calc R . . C14 C -0.06435(18) -0.9272(5) 0.2420(6) 0.109(2) Uani 1 1 d . . . H14 H -0.0421 -0.9607 0.2829 0.131 Uiso 1 1 calc R . . C15 C -0.11017(19) -0.8868(6) 0.1248(5) 0.104(2) Uani 1 1 d . . . H15 H -0.1267 -0.8889 0.0639 0.125 Uiso 1 1 calc R . . C16 C 0.18207(9) -0.1959(3) 0.5768(2) 0.0264(7) Uani 1 1 d . . . C17 C 0.17970(9) -0.0910(3) 0.6360(2) 0.0258(7) Uani 1 1 d . . . C18 C 0.14607(9) -0.0220(3) 0.6164(2) 0.0301(8) Uani 1 1 d . . . H18 H 0.1251 -0.0396 0.5645 0.036 Uiso 1 1 calc R . . C19 C 0.14346(9) 0.0720(3) 0.6728(2) 0.0310(8) Uani 1 1 d . . . H19 H 0.1207 0.1171 0.6589 0.037 Uiso 1 1 calc R . . C20 C 0.17475(9) 0.1003(3) 0.7509(2) 0.0274(7) Uani 1 1 d . . . C21 C 0.20877(9) 0.0334(3) 0.7684(2) 0.0350(8) Uani 1 1 d . . . H21 H 0.2301 0.0523 0.8191 0.042 Uiso 1 1 calc R . . C22 C 0.21126(10) -0.0606(3) 0.7117(2) 0.0341(8) Uani 1 1 d . . . H22 H 0.2343 -0.1042 0.7241 0.041 Uiso 1 1 calc R . . C23 C 0.17134(10) 0.1973(3) 0.8152(2) 0.0278(7) Uani 1 1 d . . . C24 C 0.22099(9) -0.5095(3) 0.4713(2) 0.0237(7) Uani 1 1 d . . . C25 C 0.23578(9) -0.6341(3) 0.4857(2) 0.0262(7) Uani 1 1 d . . . C26 C 0.27521(10) -0.6556(3) 0.5281(3) 0.0353(8) Uani 1 1 d . . . H26 H 0.2923 -0.5921 0.5470 0.042 Uiso 1 1 calc R . . C27 C 0.28919(10) -0.7695(3) 0.5423(2) 0.0332(8) Uani 1 1 d . . . H27 H 0.3157 -0.7824 0.5709 0.040 Uiso 1 1 calc R . . N1 N 0.09948(7) -0.4200(2) 0.40383(18) 0.0268(6) Uani 1 1 d . . . N2 N -0.04717(8) -0.4812(3) 0.3603(2) 0.0366(7) Uani 1 1 d . . . N3 N -0.02298(8) -0.6671(3) 0.3637(2) 0.0416(8) Uani 1 1 d . . . N4 N -0.06232(8) -0.6695(3) 0.3525(2) 0.0404(8) Uani 1 1 d . . . N5 N -0.19294(9) -0.4466(4) 0.3266(2) 0.0561(10) Uani 1 1 d . . . N6 N -0.08586(10) -0.8429(3) 0.2651(3) 0.0571(10) Uani 1 1 d . . . N7 N -0.11602(12) -0.8156(4) 0.1874(3) 0.0725(12) Uani 1 1 d . . . N8 N -0.07885(18) -0.9568(6) 0.1531(5) 0.133(2) Uani 1 1 d . . . O1 O 0.15032(6) -0.2299(2) 0.51905(16) 0.0354(6) Uani 1 1 d . . . O2 O 0.21420(6) -0.2445(2) 0.58678(15) 0.0326(5) Uani 1 1 d . . . O3 O 0.13892(7) 0.2484(2) 0.80417(16) 0.0375(6) Uani 1 1 d . . . O4 O 0.19992(7) 0.2287(2) 0.88154(16) 0.0374(6) Uani 1 1 d . . . O5 O 0.18415(6) -0.49472(18) 0.44173(15) 0.0295(5) Uani 1 1 d . . . O6 O 0.24603(6) -0.42914(18) 0.49034(16) 0.0320(5) Uani 1 1 d . . . O1W O 0.05964(9) 0.2355(3) 0.6959(3) 0.0785(10) Uani 1 1 d . . . H1A H 0.0821 0.2513 0.7329 0.118 Uiso 1 1 d R . . H1B H 0.0472 0.3004 0.6823 0.118 Uiso 1 1 d R . . O2W O -0.0363(2) -1.0632(6) 0.0334(5) 0.187(3) Uani 1 1 d . . . O3W O 0.0000 0.1258(7) 0.7500 0.221(6) Uani 1 2 d S . . O4W O 0.0459(5) 0.1687(16) 0.5192(12) 0.122(6) Uani 0.25 1 d PU . . H4A H 0.0492 0.1930 0.5748 0.183 Uiso 0.25 1 d PR . . H4B H 0.0283 0.2115 0.4831 0.183 Uiso 0.25 1 d PR . . 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 0.0204(2) 0.0167(2) 0.0290(2) -0.00055(15) 0.00664(14) 0.00031(14) Zn2 0.0187(3) 0.0137(3) 0.0323(3) 0.0007(2) 0.0081(2) 0.00057(19) C1 0.0264(18) 0.0303(19) 0.0380(19) 0.0000(16) 0.0104(14) 0.0010(15) C2 0.0296(19) 0.0252(18) 0.044(2) -0.0013(16) 0.0072(15) -0.0041(14) C3 0.0272(18) 0.039(2) 0.0322(18) 0.0025(16) 0.0063(14) -0.0040(15) C4 0.0220(19) 0.037(2) 0.060(2) -0.0032(18) 0.0103(16) 0.0020(15) C5 0.0289(19) 0.0268(19) 0.053(2) -0.0039(17) 0.0110(16) -0.0022(15) C6 0.0222(18) 0.041(2) 0.0359(19) 0.0045(17) 0.0060(14) -0.0030(15) C7 0.0264(19) 0.043(2) 0.0342(19) 0.0057(17) 0.0059(14) -0.0021(16) C8 0.0243(19) 0.054(2) 0.0333(19) 0.0137(18) 0.0082(14) 0.0000(16) C9 0.034(2) 0.058(3) 0.039(2) 0.006(2) 0.0143(16) -0.0034(18) C10 0.044(3) 0.067(3) 0.049(2) 0.005(2) 0.0233(19) 0.004(2) C11 0.027(2) 0.075(3) 0.053(2) 0.005(2) 0.0057(17) -0.004(2) C12 0.029(2) 0.058(3) 0.047(2) -0.002(2) 0.0096(17) -0.0057(18) C13 0.032(2) 0.046(2) 0.075(3) 0.013(2) 0.0110(19) -0.0115(18) C14 0.061(4) 0.076(4) 0.172(7) -0.031(5) 0.006(4) 0.015(3) C15 0.084(5) 0.091(5) 0.126(5) -0.047(4) 0.014(4) 0.006(4) C16 0.0286(19) 0.0248(17) 0.0284(18) -0.0021(14) 0.0123(14) -0.0031(14) C17 0.0235(17) 0.0241(17) 0.0328(18) -0.0058(15) 0.0128(14) -0.0050(13) C18 0.0284(19) 0.0314(19) 0.0273(17) -0.0060(15) 0.0033(14) -0.0042(14) C19 0.0243(17) 0.0277(18) 0.0387(19) -0.0044(15) 0.0056(14) 0.0048(14) C20 0.0264(18) 0.0253(17) 0.0306(18) -0.0019(15) 0.0085(14) -0.0008(14) C21 0.0233(18) 0.044(2) 0.0333(19) -0.0124(17) 0.0006(14) 0.0000(15) C22 0.0235(18) 0.035(2) 0.042(2) -0.0087(17) 0.0053(15) 0.0041(15) C23 0.033(2) 0.0211(16) 0.0295(18) 0.0019(15) 0.0096(15) 0.0012(14) C24 0.0282(18) 0.0151(15) 0.0285(17) 0.0017(13) 0.0093(13) 0.0001(13) C25 0.0273(18) 0.0152(15) 0.0372(19) 0.0006(14) 0.0113(14) 0.0017(13) C26 0.0283(19) 0.0187(17) 0.056(2) -0.0028(16) 0.0080(16) -0.0014(14) C27 0.0233(18) 0.0188(17) 0.054(2) 0.0018(16) 0.0057(15) 0.0012(13) N1 0.0236(14) 0.0257(15) 0.0303(15) 0.0007(12) 0.0067(11) -0.0022(11) N2 0.0218(15) 0.0457(19) 0.0419(17) 0.0018(15) 0.0088(12) -0.0047(13) N3 0.0218(16) 0.0430(19) 0.056(2) 0.0072(16) 0.0059(13) -0.0049(13) N4 0.0229(16) 0.0450(19) 0.0516(19) 0.0059(15) 0.0084(13) -0.0069(14) N5 0.0337(19) 0.082(3) 0.053(2) 0.012(2) 0.0146(16) 0.0067(19) N6 0.039(2) 0.0354(19) 0.095(3) 0.000(2) 0.016(2) -0.0062(16) N7 0.060(3) 0.061(3) 0.085(3) -0.013(2) 0.004(2) 0.004(2) N8 0.094(4) 0.109(5) 0.185(6) -0.077(5) 0.024(4) 0.013(4) O1 0.0297(14) 0.0346(14) 0.0428(14) -0.0165(11) 0.0120(11) -0.0037(10) O2 0.0317(14) 0.0323(13) 0.0376(13) -0.0013(11) 0.0160(10) 0.0079(10) O3 0.0347(14) 0.0370(14) 0.0382(14) -0.0096(11) 0.0062(11) 0.0090(11) O4 0.0330(14) 0.0376(14) 0.0360(13) -0.0114(11) 0.0013(11) -0.0043(11) O5 0.0260(13) 0.0173(11) 0.0441(13) 0.0018(10) 0.0083(10) 0.0033(9) O6 0.0274(12) 0.0136(11) 0.0545(15) -0.0002(10) 0.0111(10) 0.0006(9) O1W 0.049(2) 0.069(2) 0.112(3) 0.007(2) 0.0137(18) 0.0074(16) O2W 0.200(7) 0.165(6) 0.193(6) -0.093(5) 0.051(5) -0.028(5) O3W 0.129(7) 0.082(5) 0.491(19) 0.000 0.151(9) 0.000 O4W 0.124(9) 0.115(9) 0.103(9) -0.029(8) -0.005(7) 0.031(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.937(2) . ? Zn1 O1 1.974(2) . ? Zn1 O3 2.060(2) 6 ? Zn1 N1 2.073(3) . ? Zn1 O4 2.334(2) 6 ? Zn1 C23 2.548(3) 6 ? Zn2 O6 2.026(2) 7_546 ? Zn2 O6 2.026(2) . ? Zn2 O2 2.071(2) . ? Zn2 O2 2.071(2) 7_546 ? Zn2 O4 2.133(2) 4_546 ? Zn2 O4 2.133(2) 6 ? C1 N1 1.341(4) . ? C1 C2 1.371(5) . ? C1 H1 0.9300 . ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C3 C4 1.376(5) . ? C3 C6 1.482(5) . ? C4 C5 1.374(5) . ? C4 H4 0.9300 . ? C5 N1 1.340(4) . ? C5 H5 0.9300 . ? C6 N3 1.315(4) . ? C6 N2 1.366(4) . ? C7 N2 1.328(4) . ? C7 N4 1.348(5) . ? C7 C8 1.481(5) . ? C8 C12 1.385(5) . ? C8 C9 1.386(5) . ? C9 C10 1.382(5) . ? C9 H9 0.9300 . ? C10 N5 1.325(5) . ? C10 H10 0.9300 . ? C11 N5 1.332(6) . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N6 1.419(6) . ? C13 N4 1.443(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N8 1.321(9) . ? C14 N6 1.329(7) . ? C14 H14 0.9300 . ? C15 N7 1.295(7) . ? C15 N8 1.334(8) . ? C15 H15 0.9300 . ? C16 O2 1.242(4) . ? C16 O1 1.269(4) . ? C16 C17 1.495(4) . ? C17 C22 1.387(4) . ? C17 C18 1.389(4) . ? C18 C19 1.373(5) . ? C18 H18 0.9300 . ? C19 C20 1.398(4) . ? C19 H19 0.9300 . ? C20 C21 1.390(5) . ? C20 C23 1.484(5) . ? C21 C22 1.376(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O4 1.250(4) . ? C23 O3 1.261(4) . ? C23 Zn1 2.548(3) 6_556 ? C24 O6 1.247(4) . ? C24 O5 1.272(4) . ? C24 C25 1.494(4) . ? C25 C26 1.388(5) . ? C25 C27 1.391(4) 7_536 ? C26 C27 1.372(4) . ? C26 H26 0.9300 . ? C27 C25 1.391(4) 7_536 ? C27 H27 0.9300 . ? N3 N4 1.367(4) . ? N6 N7 1.369(5) . ? O3 Zn1 2.060(2) 6_556 ? O4 Zn2 2.133(2) 4_556 ? O4 Zn1 2.334(2) 6_556 ? O1W H1A 0.8502 . ? O1W H1B 0.8500 . ? O4W H4A 0.8500 . ? O4W H4B 0.8501 . ? 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 Zn1 O1 129.52(10) . . ? O5 Zn1 O3 125.34(10) . 6 ? O1 Zn1 O3 101.46(10) . 6 ? O5 Zn1 N1 98.16(10) . . ? O1 Zn1 N1 95.88(10) . . ? O3 Zn1 N1 94.22(10) 6 . ? O5 Zn1 O4 97.70(9) . 6 ? O1 Zn1 O4 90.90(9) . 6 ? O3 Zn1 O4 58.55(8) 6 6 ? N1 Zn1 O4 152.76(9) . 6 ? O5 Zn1 C23 115.63(10) . 6 ? O1 Zn1 C23 95.27(10) . 6 ? O3 Zn1 C23 29.40(9) 6 6 ? N1 Zn1 C23 123.58(10) . 6 ? O4 Zn1 C23 29.25(9) 6 6 ? O6 Zn2 O6 180.00(14) 7_546 . ? O6 Zn2 O2 88.22(9) 7_546 . ? O6 Zn2 O2 91.78(9) . . ? O6 Zn2 O2 91.78(9) 7_546 7_546 ? O6 Zn2 O2 88.22(9) . 7_546 ? O2 Zn2 O2 180.00(8) . 7_546 ? O6 Zn2 O4 91.64(9) 7_546 4_546 ? O6 Zn2 O4 88.36(9) . 4_546 ? O2 Zn2 O4 90.35(9) . 4_546 ? O2 Zn2 O4 89.65(9) 7_546 4_546 ? O6 Zn2 O4 88.36(9) 7_546 6 ? O6 Zn2 O4 91.64(9) . 6 ? O2 Zn2 O4 89.66(9) . 6 ? O2 Zn2 O4 90.35(9) 7_546 6 ? O4 Zn2 O4 180.00(10) 4_546 6 ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.5(3) . . ? C4 C3 C6 121.1(3) . . ? C2 C3 C6 120.4(3) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N3 C6 N2 115.0(3) . . ? N3 C6 C3 122.0(3) . . ? N2 C6 C3 123.0(3) . . ? N2 C7 N4 109.5(3) . . ? N2 C7 C8 123.5(3) . . ? N4 C7 C8 127.0(3) . . ? C12 C8 C9 118.4(3) . . ? C12 C8 C7 123.2(4) . . ? C9 C8 C7 118.4(3) . . ? C10 C9 C8 118.4(4) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? N5 C10 C9 124.4(4) . . ? N5 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N5 C11 C12 124.1(4) . . ? N5 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C8 C12 C11 118.2(4) . . ? C8 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N6 C13 N4 111.4(3) . . ? N6 C13 H13A 109.3 . . ? N4 C13 H13A 109.3 . . ? N6 C13 H13B 109.3 . . ? N4 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N8 C14 N6 110.7(6) . . ? N8 C14 H14 124.6 . . ? N6 C14 H14 124.6 . . ? N7 C15 N8 115.7(6) . . ? N7 C15 H15 122.1 . . ? N8 C15 H15 122.1 . . ? O2 C16 O1 124.1(3) . . ? O2 C16 C17 119.2(3) . . ? O1 C16 C17 116.6(3) . . ? C22 C17 C18 118.8(3) . . ? C22 C17 C16 120.3(3) . . ? C18 C17 C16 120.9(3) . . ? C19 C18 C17 120.8(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 118.5(3) . . ? C21 C20 C23 120.7(3) . . ? C19 C20 C23 120.8(3) . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C17 120.6(3) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? O4 C23 O3 118.9(3) . . ? O4 C23 C20 121.3(3) . . ? O3 C23 C20 119.8(3) . . ? O4 C23 Zn1 65.83(18) . 6_556 ? O3 C23 Zn1 53.32(16) . 6_556 ? C20 C23 Zn1 170.5(2) . 6_556 ? O6 C24 O5 125.8(3) . . ? O6 C24 C25 116.7(3) . . ? O5 C24 C25 117.4(3) . . ? C26 C25 C27 118.6(3) . 7_536 ? C26 C25 C24 120.0(3) . . ? C27 C25 C24 121.5(3) 7_536 . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C25 120.8(3) . 7_536 ? C26 C27 H27 119.6 . . ? C25 C27 H27 119.6 7_536 . ? C5 N1 C1 117.2(3) . . ? C5 N1 Zn1 118.6(2) . . ? C1 N1 Zn1 124.2(2) . . ? C7 N2 C6 103.1(3) . . ? C6 N3 N4 102.2(3) . . ? C7 N4 N3 110.1(3) . . ? C7 N4 C13 132.0(3) . . ? N3 N4 C13 117.7(3) . . ? C10 N5 C11 116.5(4) . . ? C14 N6 N7 108.2(5) . . ? C14 N6 C13 129.6(5) . . ? N7 N6 C13 122.1(4) . . ? C15 N7 N6 102.7(5) . . ? C14 N8 C15 102.6(5) . . ? C16 O1 Zn1 116.5(2) . . ? C16 O2 Zn2 131.0(2) . . ? C23 O3 Zn1 97.3(2) . 6_556 ? C23 O4 Zn2 170.0(2) . 4_556 ? C23 O4 Zn1 84.9(2) . 6_556 ? Zn2 O4 Zn1 100.71(9) 4_556 6_556 ? C24 O5 Zn1 128.7(2) . . ? C24 O6 Zn2 140.5(2) . . ? H1A O1W H1B 107.7 . . ? H4A O4W H4B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C1 C2 C3 C6 -179.0(3) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? C6 C3 C4 C5 179.3(3) . . . . ? C3 C4 C5 N1 0.0(6) . . . . ? C4 C3 C6 N3 -171.2(4) . . . . ? C2 C3 C6 N3 8.8(5) . . . . ? C4 C3 C6 N2 10.0(5) . . . . ? C2 C3 C6 N2 -170.0(3) . . . . ? N2 C7 C8 C12 147.5(4) . . . . ? N4 C7 C8 C12 -34.0(5) . . . . ? N2 C7 C8 C9 -31.5(5) . . . . ? N4 C7 C8 C9 147.0(4) . . . . ? C12 C8 C9 C10 1.3(5) . . . . ? C7 C8 C9 C10 -179.7(3) . . . . ? C8 C9 C10 N5 -0.5(6) . . . . ? C9 C8 C12 C11 -1.3(5) . . . . ? C7 C8 C12 C11 179.7(3) . . . . ? N5 C11 C12 C8 0.6(6) . . . . ? O2 C16 C17 C22 -10.9(5) . . . . ? O1 C16 C17 C22 168.7(3) . . . . ? O2 C16 C17 C18 168.9(3) . . . . ? O1 C16 C17 C18 -11.5(4) . . . . ? C22 C17 C18 C19 -2.4(5) . . . . ? C16 C17 C18 C19 177.8(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C21 1.8(5) . . . . ? C18 C19 C20 C23 -176.5(3) . . . . ? C19 C20 C21 C22 -1.7(5) . . . . ? C23 C20 C21 C22 176.6(3) . . . . ? C20 C21 C22 C17 -0.4(5) . . . . ? C18 C17 C22 C21 2.5(5) . . . . ? C16 C17 C22 C21 -177.7(3) . . . . ? C21 C20 C23 O4 6.7(5) . . . . ? C19 C20 C23 O4 -175.1(3) . . . . ? C21 C20 C23 O3 -172.1(3) . . . . ? C19 C20 C23 O3 6.1(5) . . . . ? O6 C24 C25 C26 7.0(5) . . . . ? O5 C24 C25 C26 -172.4(3) . . . . ? O6 C24 C25 C27 -173.3(3) . . . 7_536 ? O5 C24 C25 C27 7.3(5) . . . 7_536 ? C27 C25 C26 C27 -0.2(6) 7_536 . . . ? C24 C25 C26 C27 179.6(3) . . . . ? C25 C26 C27 C25 0.2(6) . . . 7_536 ? C4 C5 N1 C1 0.3(5) . . . . ? C4 C5 N1 Zn1 -178.9(3) . . . . ? C2 C1 N1 C5 0.1(5) . . . . ? C2 C1 N1 Zn1 179.2(2) . . . . ? O5 Zn1 N1 C5 165.7(2) . . . . ? O1 Zn1 N1 C5 34.4(3) . . . . ? O3 Zn1 N1 C5 -67.6(3) 6 . . . ? O4 Zn1 N1 C5 -69.2(3) 6 . . . ? C23 Zn1 N1 C5 -66.0(3) 6 . . . ? O5 Zn1 N1 C1 -13.4(3) . . . . ? O1 Zn1 N1 C1 -144.7(3) . . . . ? O3 Zn1 N1 C1 113.3(3) 6 . . . ? O4 Zn1 N1 C1 111.7(3) 6 . . . ? C23 Zn1 N1 C1 114.9(3) 6 . . . ? N4 C7 N2 C6 0.1(4) . . . . ? C8 C7 N2 C6 178.9(3) . . . . ? N3 C6 N2 C7 0.3(4) . . . . ? C3 C6 N2 C7 179.2(3) . . . . ? N2 C6 N3 N4 -0.6(4) . . . . ? C3 C6 N3 N4 -179.5(3) . . . . ? N2 C7 N4 N3 -0.5(4) . . . . ? C8 C7 N4 N3 -179.2(3) . . . . ? N2 C7 N4 C13 174.7(4) . . . . ? C8 C7 N4 C13 -4.0(6) . . . . ? C6 N3 N4 C7 0.6(4) . . . . ? C6 N3 N4 C13 -175.3(3) . . . . ? N6 C13 N4 C7 108.4(5) . . . . ? N6 C13 N4 N3 -76.7(4) . . . . ? C9 C10 N5 C11 -0.2(6) . . . . ? C12 C11 N5 C10 0.2(6) . . . . ? N8 C14 N6 N7 0.0(7) . . . . ? N8 C14 N6 C13 -178.7(5) . . . . ? N4 C13 N6 C14 99.1(6) . . . . ? N4 C13 N6 N7 -79.3(5) . . . . ? N8 C15 N7 N6 -1.0(8) . . . . ? C14 N6 N7 C15 0.6(6) . . . . ? C13 N6 N7 C15 179.3(5) . . . . ? N6 C14 N8 C15 -0.5(8) . . . . ? N7 C15 N8 C14 1.0(9) . . . . ? O2 C16 O1 Zn1 -11.6(4) . . . . ? C17 C16 O1 Zn1 168.8(2) . . . . ? O5 Zn1 O1 C16 48.4(3) . . . . ? O3 Zn1 O1 C16 -110.4(2) 6 . . . ? N1 Zn1 O1 C16 154.1(2) . . . . ? O4 Zn1 O1 C16 -52.4(2) 6 . . . ? C23 Zn1 O1 C16 -81.3(2) 6 . . . ? O1 C16 O2 Zn2 70.4(4) . . . . ? C17 C16 O2 Zn2 -110.1(3) . . . . ? O6 Zn2 O2 C16 60.8(3) 7_546 . . . ? O6 Zn2 O2 C16 -119.2(3) . . . . ? O4 Zn2 O2 C16 152.4(3) 4_546 . . . ? O4 Zn2 O2 C16 -27.6(3) 6 . . . ? O4 C23 O3 Zn1 -6.7(3) . . . 6_556 ? C20 C23 O3 Zn1 172.1(3) . . . 6_556 ? O3 C23 O4 Zn2 130.7(12) . . . 4_556 ? C20 C23 O4 Zn2 -48.1(15) . . . 4_556 ? Zn1 C23 O4 Zn2 124.8(14) 6_556 . . 4_556 ? O3 C23 O4 Zn1 5.9(3) . . . 6_556 ? C20 C23 O4 Zn1 -172.9(3) . . . 6_556 ? O6 C24 O5 Zn1 -4.8(5) . . . . ? C25 C24 O5 Zn1 174.5(2) . . . . ? O1 Zn1 O5 C24 -63.6(3) . . . . ? O3 Zn1 O5 C24 90.6(3) 6 . . . ? N1 Zn1 O5 C24 -168.3(3) . . . . ? O4 Zn1 O5 C24 34.0(3) 6 . . . ? C23 Zn1 O5 C24 58.2(3) 6 . . . ? O5 C24 O6 Zn2 5.8(6) . . . . ? C25 C24 O6 Zn2 -173.6(2) . . . . ? O2 Zn2 O6 C24 51.9(3) . . . . ? O2 Zn2 O6 C24 -128.1(3) 7_546 . . . ? O4 Zn2 O6 C24 142.1(3) 4_546 . . . ? O4 Zn2 O6 C24 -37.9(3) 6 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.789 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.072 #========================================================== data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 872136' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H24 N8 O15 Zn3' _chemical_formula_sum 'C33 H24 N8 O15 Zn3' _chemical_formula_weight 968.71 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 'P n a m' _symmetry_space_group_name_hall '-P 2c 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 9.9290(2) _cell_length_b 16.2793(4) _cell_length_c 21.2630(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3436.89(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7167 _cell_measurement_theta_min 3.0673 _cell_measurement_theta_max 29.1751 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6243 _exptl_absorpt_correction_T_max 0.6711 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12830 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3130 _reflns_number_gt 2969 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For N6, some anisotropic displacement ellipsoids were rather elongated, which led us to use the ISOR restraints. ; _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^)+(0.0000P)^2^+60.3463P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3130 _refine_ls_number_parameters 316 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.169 _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 Zn1 Zn 0.96490(9) 0.14946(6) 0.09090(5) 0.0307(3) Uani 1 1 d . . . Zn2 Zn 0.36740(12) 0.15122(7) 0.2500 0.0183(3) Uani 1 2 d S . . C1 C 0.8300(8) 0.2133(6) -0.0259(4) 0.0330(19) Uani 1 1 d . . . H1 H 0.7765 0.2384 0.0045 0.040 Uiso 1 1 calc R . . C2 C 0.8090(9) 0.2329(5) -0.0888(4) 0.036(2) Uani 1 1 d . . . H2 H 0.7429 0.2706 -0.0999 0.043 Uiso 1 1 calc R . . C3 C 0.9809(10) 0.1376(7) -0.1155(4) 0.047(3) Uani 1 1 d . . . H3 H 1.0333 0.1101 -0.1451 0.057 Uiso 1 1 calc R . . C4 C 0.9951(10) 0.1213(6) -0.0525(4) 0.044(2) Uani 1 1 d . . . H4 H 1.0570 0.0814 -0.0405 0.053 Uiso 1 1 calc R . . C6 C 0.8739(9) 0.2201(5) -0.2010(4) 0.035(2) Uani 1 1 d . . . C7 C 0.829(2) 0.3755(11) -0.1993(9) 0.044(5) Uani 0.50 1 d P . . H7A H 0.8245 0.3773 -0.1538 0.052 Uiso 0.50 1 calc PR . . H7B H 0.7467 0.4004 -0.2153 0.052 Uiso 0.50 1 calc PR . . C9 C 1.1468(18) 0.4587(9) -0.2348(6) 0.032(5) Uani 0.50 1 d P . . C8 C 0.9414(16) 0.5035(9) -0.2500 0.065(5) Uani 1 2 d S . . C10 C 0.7442(9) 0.0754(6) 0.1022(4) 0.039(2) Uani 1 1 d . . . C11 C 0.5016(7) 0.1787(5) 0.1294(3) 0.0190(15) Uani 1 1 d . . . C12 C 0.2392(8) 0.0976(5) 0.1212(4) 0.0269(17) Uani 1 1 d . . . C13 C 0.3661(8) 0.0540(5) 0.1035(4) 0.035(2) Uani 1 1 d . . . C14 C 0.4916(8) 0.0888(5) 0.1100(4) 0.0259(17) Uani 1 1 d . . . C15 C 0.6062(9) 0.0420(6) 0.0965(6) 0.048(3) Uani 1 1 d . . . C16' C 0.588(2) -0.0345(12) 0.0591(9) 0.029(4) Uani 0.50 1 d P . . C16 C 0.596(2) -0.0442(13) 0.0925(11) 0.040(5) Uani 0.50 1 d P . . C17 C 0.473(2) -0.0787(11) 0.0822(14) 0.046(5) Uani 0.50 1 d P . . C17' C 0.456(2) -0.0651(15) 0.0466(10) 0.041(6) Uani 0.50 1 d P . . C18 C 0.3509(10) -0.0251(7) 0.0786(7) 0.070(4) Uani 1 1 d . . . N1 N 0.9248(7) 0.1595(4) -0.0074(3) 0.0315(16) Uani 1 1 d . . . N2 N 0.9018(10) 0.1709(6) -0.2500 0.028(2) Uani 1 2 d S . . N3 N 0.8322(10) 0.2934(5) -0.2184(4) 0.058(2) Uani 1 1 d . . . N4 N 0.9448(16) 0.4249(8) -0.2205(6) 0.033(3) Uani 0.50 1 d P . . N5 N 1.0694(17) 0.3962(10) -0.2190(8) 0.047(4) Uani 0.50 1 d P . . N6 N 1.0684(11) 0.5273(7) -0.2567(14) 0.027(4) Uani 0.50 1 d PU . . C5 C 0.8868(9) 0.1960(5) -0.1346(4) 0.0322(19) Uani 1 1 d . . . O1 O 0.8416(6) 0.0307(5) 0.0916(4) 0.056(2) Uani 1 1 d . . . O2 O 0.7602(6) 0.1513(4) 0.1158(4) 0.0521(19) Uani 1 1 d . . . O3 O 0.4961(6) 0.2289(4) 0.0859(3) 0.0347(14) Uani 1 1 d . . . O4 O 0.5064(6) 0.1954(4) 0.1859(2) 0.0344(14) Uani 1 1 d . . . O5 O 0.2319(5) 0.1320(4) 0.1746(3) 0.0324(14) Uani 1 1 d . . . O6 O 0.1439(6) 0.0958(4) 0.0831(3) 0.0383(15) Uani 1 1 d . . . O3W O 0.9739(6) 0.1297(4) 0.1948(5) 0.029(2) Uani 0.50 1 d P . . H3A H 0.9237 0.1486 0.2238 0.043 Uiso 0.50 1 d PR . . H3B H 1.0519 0.1224 0.2103 0.043 Uiso 0.50 1 d PR . . O1W O 0.2680(6) 0.2707(4) 0.2500(5) 0.0243(16) Uani 1 2 d SR . . O2W O 0.6029(6) 0.4877(4) -0.2500(5) 0.105(5) Uani 1 2 d SR . . 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 0.0226(5) 0.0363(6) 0.0331(5) -0.0090(4) -0.0079(4) 0.0009(4) Zn2 0.0176(6) 0.0179(6) 0.0195(6) 0.000 0.000 0.0004(5) C1 0.026(4) 0.038(5) 0.034(4) -0.007(4) 0.003(4) 0.001(4) C2 0.037(5) 0.036(5) 0.034(4) -0.003(4) -0.004(4) 0.008(4) C3 0.036(5) 0.069(7) 0.037(5) -0.028(5) -0.005(4) 0.012(5) C4 0.044(6) 0.051(6) 0.036(5) -0.011(4) -0.008(4) 0.019(5) C6 0.038(5) 0.031(4) 0.035(4) -0.005(4) -0.003(4) -0.010(4) C7 0.064(13) 0.028(9) 0.039(10) -0.008(8) 0.035(10) -0.006(9) C9 0.049(10) 0.021(7) 0.025(14) 0.008(6) -0.001(6) -0.007(7) C8 0.047(9) 0.019(7) 0.129(16) 0.000 0.000 -0.009(7) C10 0.035(5) 0.040(5) 0.042(5) -0.004(4) 0.010(4) 0.009(4) C11 0.013(3) 0.028(4) 0.017(3) -0.003(3) 0.003(3) 0.003(3) C12 0.022(4) 0.027(4) 0.032(4) -0.007(3) -0.001(3) -0.003(3) C13 0.026(4) 0.028(4) 0.050(5) -0.012(4) 0.001(4) 0.003(4) C14 0.024(4) 0.022(4) 0.031(4) -0.004(3) 0.001(3) 0.004(3) C15 0.025(5) 0.028(5) 0.091(8) -0.018(5) 0.018(5) 0.005(4) C16' 0.042(11) 0.031(9) 0.015(9) -0.002(8) 0.011(9) 0.014(8) C16 0.043(12) 0.047(12) 0.028(11) 0.012(10) 0.008(11) 0.013(9) C17 0.037(11) 0.016(9) 0.084(18) -0.017(11) -0.005(13) -0.006(8) C17' 0.042(12) 0.060(14) 0.023(10) -0.001(10) -0.003(9) 0.009(10) C18 0.031(5) 0.045(6) 0.135(12) -0.051(7) 0.023(7) -0.012(5) N1 0.027(4) 0.039(4) 0.028(4) -0.016(3) -0.003(3) 0.005(3) N2 0.033(5) 0.029(5) 0.022(5) 0.000 0.000 -0.002(4) N3 0.070(6) 0.030(4) 0.074(6) -0.010(4) -0.008(5) -0.010(4) N4 0.056(10) 0.020(7) 0.024(6) 0.001(5) -0.002(7) 0.002(7) N5 0.052(10) 0.036(9) 0.052(9) 0.007(7) 0.012(8) 0.011(8) N6 0.027(4) 0.026(4) 0.027(7) -0.002(5) -0.001(5) -0.001(3) C5 0.033(5) 0.036(4) 0.027(4) -0.009(4) -0.007(4) -0.009(4) O1 0.026(3) 0.060(5) 0.083(5) -0.016(4) 0.007(4) 0.013(3) O2 0.031(3) 0.046(4) 0.079(5) -0.004(4) 0.025(3) -0.001(3) O3 0.046(4) 0.032(3) 0.025(3) 0.007(2) -0.005(3) 0.009(3) O4 0.043(4) 0.042(3) 0.019(3) -0.004(2) 0.005(2) -0.023(3) O5 0.024(3) 0.041(3) 0.032(3) -0.011(3) -0.010(2) 0.009(3) O6 0.027(3) 0.055(4) 0.033(3) -0.020(3) -0.012(3) 0.004(3) O3W 0.029(6) 0.027(6) 0.030(6) -0.006(5) 0.001(5) 0.002(5) O1W 0.017(4) 0.028(4) 0.029(4) 0.000 0.000 0.005(3) O2W 0.089(11) 0.102(12) 0.125(13) 0.000 0.000 0.019(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.988(6) 1_655 ? Zn1 O3 2.008(6) 8_665 ? Zn1 O2 2.101(6) . ? Zn1 N1 2.134(7) . ? Zn1 O3W 2.234(11) . ? Zn1 O1 2.288(8) . ? Zn1 C10 2.512(10) . ? Zn2 O4 2.068(5) . ? Zn2 O4 2.068(5) 6_556 ? Zn2 O5 2.116(5) . ? Zn2 O5 2.116(5) 6_556 ? Zn2 N6 2.121(11) 7_756 ? Zn2 N6 2.121(11) 4_645 ? Zn2 O1W 2.181(6) . ? C1 N1 1.346(11) . ? C1 C2 1.389(12) . ? C1 H1 0.9300 . ? C2 C5 1.381(12) . ? C2 H2 0.9300 . ? C3 C4 1.373(13) . ? C3 C5 1.393(13) . ? C3 H3 0.9300 . ? C4 N1 1.339(11) . ? C4 H4 0.9300 . ? C6 N3 1.315(13) . ? C6 N2 1.343(11) . ? C6 C5 1.472(12) . ? C7 N3 1.398(19) . ? C7 N4 1.48(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C9 0.65(3) 6 ? C9 N5 1.32(2) . ? C9 N6 1.37(2) 6 ? C9 N6 1.44(2) . ? C9 N5 1.61(2) 6 ? C8 N6 1.327(19) . ? C8 N6 1.327(19) 6 ? C8 N4 1.425(18) 6 ? C8 N4 1.425(18) . ? C10 O1 1.231(10) . ? C10 O2 1.280(12) . ? C10 C15 1.479(13) . ? C11 O4 1.234(9) . ? C11 O3 1.236(9) . ? C11 C14 1.523(10) . ? C12 O6 1.247(9) . ? C12 O5 1.267(10) . ? C12 C13 1.495(11) . ? C13 C14 1.376(11) . ? C13 C18 1.400(13) . ? C14 C15 1.400(11) . ? C15 C16 1.41(2) . ? C15 C16' 1.49(2) . ? C16' C16 0.73(2) . ? C16' C17' 1.42(3) . ? C16' C17 1.44(3) . ? C16 C17 1.36(3) . ? C16 C17' 1.73(3) . ? C17 C17' 0.80(3) . ? C17 C18 1.49(2) . ? C17' C18 1.41(2) . ? N2 C6 1.343(11) 6 ? N3 N3 1.343(19) 6 ? N4 N4 1.25(3) 6 ? N4 N5 1.32(2) . ? N4 N5 1.85(2) 6 ? N5 N5 1.32(3) 6 ? N5 C9 1.61(2) 6 ? N5 N4 1.85(2) 6 ? N6 N6 0.29(6) 6 ? N6 C9 1.37(2) 6 ? N6 Zn2 2.121(11) 7_765 ? O3 Zn1 2.008(6) 8_565 ? O6 Zn1 1.988(6) 1_455 ? O3W H3A 0.8499 . ? O3W H3B 0.8500 . ? 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 O6 Zn1 O3 106.9(3) 1_655 8_665 ? O6 Zn1 O2 153.2(3) 1_655 . ? O3 Zn1 O2 98.5(3) 8_665 . ? O6 Zn1 N1 96.8(2) 1_655 . ? O3 Zn1 N1 84.3(3) 8_665 . ? O2 Zn1 N1 93.8(3) . . ? O6 Zn1 O3W 89.1(2) 1_655 . ? O3 Zn1 O3W 100.9(2) 8_665 . ? O2 Zn1 O3W 77.9(3) . . ? N1 Zn1 O3W 170.7(2) . . ? O6 Zn1 O1 96.2(2) 1_655 . ? O3 Zn1 O1 156.4(2) 8_665 . ? O2 Zn1 O1 59.5(3) . . ? N1 Zn1 O1 88.3(3) . . ? O3W Zn1 O1 83.9(3) . . ? O6 Zn1 C10 125.2(3) 1_655 . ? O3 Zn1 C10 127.8(3) 8_665 . ? O2 Zn1 C10 30.6(3) . . ? N1 Zn1 C10 88.1(3) . . ? O3W Zn1 C10 82.6(3) . . ? O1 Zn1 C10 29.2(3) . . ? O4 Zn2 O4 82.4(3) . 6_556 ? O4 Zn2 O5 88.7(2) . . ? O4 Zn2 O5 167.1(2) 6_556 . ? O4 Zn2 O5 167.1(2) . 6_556 ? O4 Zn2 O5 88.7(2) 6_556 6_556 ? O5 Zn2 O5 98.5(3) . 6_556 ? O4 Zn2 N6 94.9(6) . 7_756 ? O4 Zn2 N6 100.1(6) 6_556 7_756 ? O5 Zn2 N6 89.9(6) . 7_756 ? O5 Zn2 N6 95.8(6) 6_556 7_756 ? O4 Zn2 N6 100.1(6) . 4_645 ? O4 Zn2 N6 94.9(6) 6_556 4_645 ? O5 Zn2 N6 95.8(6) . 4_645 ? O5 Zn2 N6 89.9(6) 6_556 4_645 ? N6 Zn2 N6 7.7(16) 7_756 4_645 ? O4 Zn2 O1W 89.5(3) . . ? O4 Zn2 O1W 89.5(3) 6_556 . ? O5 Zn2 O1W 81.0(3) . . ? O5 Zn2 O1W 81.0(3) 6_556 . ? N6 Zn2 O1W 169.9(4) 7_756 . ? N6 Zn2 O1W 169.9(4) 4_645 . ? N1 C1 C2 122.4(8) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C5 C2 C1 119.7(8) . . ? C5 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C5 118.9(8) . . ? C4 C3 H3 120.5 . . ? C5 C3 H3 120.5 . . ? N1 C4 C3 123.8(9) . . ? N1 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? N3 C6 N2 112.8(9) . . ? N3 C6 C5 122.6(8) . . ? N2 C6 C5 124.6(8) . . ? N3 C7 N4 114.3(14) . . ? N3 C7 H7A 108.7 . . ? N4 C7 H7A 108.7 . . ? N3 C7 H7B 108.7 . . ? N4 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C9 N5 104.8(10) 6 . ? C9 C9 N6 82.5(13) 6 6 ? N5 C9 N6 109.3(15) . 6 ? C9 C9 N6 71.1(12) 6 . ? N5 C9 N6 111.5(15) . . ? C9 C9 N5 52.4(8) 6 6 ? N5 C9 N5 52.4(15) . 6 ? N6 C9 N5 99.4(14) 6 6 ? N6 C9 N5 92.0(13) . 6 ? N6 C8 N4 101.1(14) . 6 ? N6 C8 N4 106.7(14) 6 6 ? N6 C8 N4 106.7(14) . . ? N6 C8 N4 101.1(14) 6 . ? N4 C8 N4 52.2(12) 6 . ? O1 C10 O2 121.0(9) . . ? O1 C10 C15 119.7(9) . . ? O2 C10 C15 119.2(8) . . ? O1 C10 Zn1 65.2(5) . . ? O2 C10 Zn1 56.6(5) . . ? C15 C10 Zn1 167.5(8) . . ? O4 C11 O3 125.9(7) . . ? O4 C11 C14 118.5(7) . . ? O3 C11 C14 115.5(6) . . ? O6 C12 O5 123.4(7) . . ? O6 C12 C13 117.6(7) . . ? O5 C12 C13 118.9(7) . . ? C14 C13 C18 120.9(8) . . ? C14 C13 C12 122.9(7) . . ? C18 C13 C12 116.2(8) . . ? C13 C14 C15 119.5(7) . . ? C13 C14 C11 118.8(7) . . ? C15 C14 C11 121.7(7) . . ? C14 C15 C16 119.7(12) . . ? C14 C15 C10 122.4(8) . . ? C16 C15 C10 116.0(11) . . ? C14 C15 C16' 117.8(11) . . ? C10 C15 C16' 117.6(10) . . ? C16 C16' C17' 102(3) . . ? C16 C16' C17 69(3) . . ? C16 C16' C15 69(2) . . ? C17' C16' C15 120.3(15) . . ? C17 C16' C15 109.4(15) . . ? C16' C16 C17 81(3) . . ? C16' C16 C15 81(3) . . ? C17 C16 C15 119.0(17) . . ? C16' C16 C17' 54(3) . . ? C15 C16 C17' 106.7(16) . . ? C17' C17 C16 103(3) . . ? C17' C17 C16' 73(3) . . ? C17' C17 C18 68(3) . . ? C16 C17 C18 119.6(16) . . ? C16' C17 C18 109.6(17) . . ? C17 C17' C18 80(3) . . ? C17 C17' C16' 75(3) . . ? C18 C17' C16' 115.5(18) . . ? C17 C17' C16 50(2) . . ? C18 C17' C16 103.4(15) . . ? C13 C18 C17' 121.9(13) . . ? C13 C18 C17 115.6(11) . . ? C4 N1 C1 117.2(8) . . ? C4 N1 Zn1 124.7(6) . . ? C1 N1 Zn1 117.8(5) . . ? C6 N2 C6 101.7(10) 6 . ? C6 N3 N3 106.3(6) . 6 ? C6 N3 C7 142.6(13) . . ? N3 N3 C7 106.9(9) 6 . ? N4 N4 N5 91.4(9) 6 . ? N4 N4 C8 63.9(6) 6 . ? N5 N4 C8 110.5(14) . . ? N4 N4 C7 107.8(9) 6 . ? N5 N4 C7 122.0(14) . . ? C8 N4 C7 127.2(15) . . ? N4 N4 N5 45.8(6) 6 6 ? N5 N4 N5 45.6(12) . 6 ? C8 N4 N5 86.4(10) . 6 ? C7 N4 N5 126.7(12) . 6 ? N5 N5 C9 75.2(10) 6 . ? N5 N5 N4 88.6(9) 6 . ? C9 N5 N4 105.4(15) . . ? N5 N5 C9 52.4(8) 6 6 ? N4 N5 C9 102.0(13) . 6 ? N5 N5 N4 45.8(6) 6 6 ? C9 N5 N4 91.0(12) . 6 ? C9 N5 N4 74.6(10) 6 6 ? N6 N6 C8 83.8(13) 6 . ? N6 N6 C9 97.5(13) 6 6 ? C8 N6 C9 108.4(12) . 6 ? N6 N6 C9 71.1(12) 6 . ? C8 N6 C9 104.6(13) . . ? N6 N6 Zn2 86.1(8) 6 7_765 ? C8 N6 Zn2 123.8(10) . 7_765 ? C9 N6 Zn2 127.8(10) 6 7_765 ? C9 N6 Zn2 123.7(11) . 7_765 ? C2 C5 C3 117.8(8) . . ? C2 C5 C6 120.8(8) . . ? C3 C5 C6 121.3(8) . . ? C10 O1 Zn1 85.5(6) . . ? C10 O2 Zn1 92.8(5) . . ? C11 O3 Zn1 128.3(5) . 8_565 ? C11 O4 Zn2 122.7(5) . . ? C12 O5 Zn2 135.0(5) . . ? C12 O6 Zn1 127.8(5) . 1_455 ? Zn1 O3W H3A 129.9 . . ? Zn1 O3W H3B 116.0 . . ? H3A O3W H3B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C5 0.4(14) . . . . ? C5 C3 C4 N1 -1.2(17) . . . . ? O6 Zn1 C10 O1 -7.1(7) 1_655 . . . ? O3 Zn1 C10 O1 171.2(5) 8_665 . . . ? O2 Zn1 C10 O1 -169.5(10) . . . . ? N1 Zn1 C10 O1 89.9(6) . . . . ? O3W Zn1 C10 O1 -90.7(6) . . . . ? O6 Zn1 C10 O2 162.4(5) 1_655 . . . ? O3 Zn1 C10 O2 -19.3(7) 8_665 . . . ? N1 Zn1 C10 O2 -100.6(6) . . . . ? O3W Zn1 C10 O2 78.8(6) . . . . ? O1 Zn1 C10 O2 169.5(10) . . . . ? O6 Zn1 C10 C15 -123(3) 1_655 . . . ? O3 Zn1 C10 C15 55(3) 8_665 . . . ? O2 Zn1 C10 C15 74(3) . . . . ? N1 Zn1 C10 C15 -26(3) . . . . ? O3W Zn1 C10 C15 153(3) . . . . ? O1 Zn1 C10 C15 -116(3) . . . . ? O6 C12 C13 C14 133.5(9) . . . . ? O5 C12 C13 C14 -48.9(13) . . . . ? O6 C12 C13 C18 -45.8(14) . . . . ? O5 C12 C13 C18 131.9(11) . . . . ? C18 C13 C14 C15 -5.2(16) . . . . ? C12 C13 C14 C15 175.6(9) . . . . ? C18 C13 C14 C11 172.3(10) . . . . ? C12 C13 C14 C11 -6.9(13) . . . . ? O4 C11 C14 C13 89.6(10) . . . . ? O3 C11 C14 C13 -86.3(10) . . . . ? O4 C11 C14 C15 -93.0(11) . . . . ? O3 C11 C14 C15 91.2(10) . . . . ? C13 C14 C15 C16 -16.7(19) . . . . ? C11 C14 C15 C16 165.9(14) . . . . ? C13 C14 C15 C10 179.7(10) . . . . ? C11 C14 C15 C10 2.3(15) . . . . ? C13 C14 C15 C16' 16.6(17) . . . . ? C11 C14 C15 C16' -160.8(11) . . . . ? O1 C10 C15 C14 177.7(10) . . . . ? O2 C10 C15 C14 -4.9(16) . . . . ? Zn1 C10 C15 C14 -72(3) . . . . ? O1 C10 C15 C16 13.5(18) . . . . ? O2 C10 C15 C16 -169.1(14) . . . . ? Zn1 C10 C15 C16 124(3) . . . . ? O1 C10 C15 C16' -19.1(17) . . . . ? O2 C10 C15 C16' 158.3(13) . . . . ? Zn1 C10 C15 C16' 91(3) . . . . ? C14 C15 C16' C16 -102(3) . . . . ? C10 C15 C16' C16 94(3) . . . . ? C14 C15 C16' C17' -10(2) . . . . ? C16 C15 C16' C17' 92(3) . . . . ? C10 C15 C16' C17' -173.7(16) . . . . ? C14 C15 C16' C17 -44(2) . . . . ? C16 C15 C16' C17 58(3) . . . . ? C10 C15 C16' C17 152.2(16) . . . . ? C17' C16' C16 C17 3(2) . . . . ? C15 C16' C16 C17 121.4(14) . . . . ? C17' C16' C16 C15 -118.1(16) . . . . ? C17 C16' C16 C15 -121.4(14) . . . . ? C17 C16' C16 C17' -3(2) . . . . ? C15 C16' C16 C17' 118.1(16) . . . . ? C14 C15 C16 C16' 95(3) . . . . ? C10 C15 C16 C16' -101(3) . . . . ? C14 C15 C16 C17 20(3) . . . . ? C10 C15 C16 C17 -175(2) . . . . ? C16' C15 C16 C17 -74(3) . . . . ? C14 C15 C16 C17' 47(2) . . . . ? C10 C15 C16 C17' -148.6(13) . . . . ? C16' C15 C16 C17' -48(2) . . . . ? C16' C16 C17 C17' -6(4) . . . . ? C15 C16 C17 C17' 69(4) . . . . ? C15 C16 C17 C16' 75(3) . . . . ? C17' C16 C17 C16' 6(4) . . . . ? C16' C16 C17 C18 -78(3) . . . . ? C15 C16 C17 C18 -3(4) . . . . ? C17' C16 C17 C18 -72(3) . . . . ? C16 C16' C17 C17' 174(4) . . . . ? C15 C16' C17 C17' 116(3) . . . . ? C17' C16' C17 C16 -174(4) . . . . ? C15 C16' C17 C16 -58(2) . . . . ? C16 C16' C17 C18 116(3) . . . . ? C17' C16' C17 C18 -58(3) . . . . ? C15 C16' C17 C18 58(2) . . . . ? C16 C17 C17' C18 -117.1(17) . . . . ? C16' C17 C17' C18 -120.2(13) . . . . ? C16 C17 C17' C16' 3.1(19) . . . . ? C18 C17 C17' C16' 120.2(13) . . . . ? C16' C17 C17' C16 -3.1(19) . . . . ? C18 C17 C17' C16 117.1(17) . . . . ? C16 C16' C17' C17 -6(3) . . . . ? C15 C16' C17' C17 -79(3) . . . . ? C16 C16' C17' C18 65(3) . . . . ? C17 C16' C17' C18 70(2) . . . . ? C15 C16' C17' C18 -8(3) . . . . ? C17 C16' C17' C16 6(3) . . . . ? C15 C16' C17' C16 -73(3) . . . . ? C16' C16 C17' C17 173(4) . . . . ? C15 C16 C17' C17 -122(3) . . . . ? C16' C16 C17' C18 -123(3) . . . . ? C17 C16 C17' C18 64(3) . . . . ? C15 C16 C17' C18 -57(2) . . . . ? C17 C16 C17' C16' -173(4) . . . . ? C15 C16 C17' C16' 66(3) . . . . ? C14 C13 C18 C17' -14(2) . . . . ? C12 C13 C18 C17' 164.8(15) . . . . ? C14 C13 C18 C17 22(2) . . . . ? C12 C13 C18 C17 -159.2(15) . . . . ? C17 C17' C18 C13 88(3) . . . . ? C16' C17' C18 C13 20(3) . . . . ? C16 C17' C18 C13 43(2) . . . . ? C16' C17' C18 C17 -67(2) . . . . ? C16 C17' C18 C17 -45(2) . . . . ? C17' C17 C18 C13 -110(3) . . . . ? C16 C17 C18 C13 -17(3) . . . . ? C16' C17 C18 C13 -49(3) . . . . ? C16 C17 C18 C17' 92(4) . . . . ? C16' C17 C18 C17' 61(3) . . . . ? C3 C4 N1 C1 3.9(15) . . . . ? C3 C4 N1 Zn1 -170.1(8) . . . . ? C2 C1 N1 C4 -3.5(13) . . . . ? C2 C1 N1 Zn1 170.9(7) . . . . ? O6 Zn1 N1 C4 12.5(8) 1_655 . . . ? O3 Zn1 N1 C4 118.9(8) 8_665 . . . ? O2 Zn1 N1 C4 -142.8(8) . . . . ? O1 Zn1 N1 C4 -83.5(8) . . . . ? C10 Zn1 N1 C4 -112.8(8) . . . . ? O6 Zn1 N1 C1 -161.5(6) 1_655 . . . ? O3 Zn1 N1 C1 -55.0(6) 8_665 . . . ? O2 Zn1 N1 C1 43.2(7) . . . . ? O1 Zn1 N1 C1 102.5(6) . . . . ? C10 Zn1 N1 C1 73.3(7) . . . . ? N3 C6 N2 C6 0.0(14) . . . 6 ? C5 C6 N2 C6 179.7(5) . . . 6 ? N2 C6 N3 N3 0.0(9) . . . 6 ? C5 C6 N3 N3 -179.7(7) . . . 6 ? N2 C6 N3 C7 -151.7(17) . . . . ? C5 C6 N3 C7 29(2) . . . . ? N4 C7 N3 C6 91(2) . . . . ? N4 C7 N3 N3 -60.9(17) . . . 6 ? N6 C8 N4 N4 -91.2(14) . . . 6 ? N6 C8 N4 N4 -102.6(14) 6 . . 6 ? N6 C8 N4 N5 -10.1(18) . . . . ? N6 C8 N4 N5 -21.5(18) 6 . . . ? N4 C8 N4 N5 81.1(13) 6 . . . ? N6 C8 N4 C7 175.7(17) . . . . ? N6 C8 N4 C7 164.3(18) 6 . . . ? N4 C8 N4 C7 -93.1(15) 6 . . . ? N6 C8 N4 N5 -49.5(14) . . . 6 ? N6 C8 N4 N5 -60.9(14) 6 . . 6 ? N4 C8 N4 N5 41.7(9) 6 . . 6 ? N3 C7 N4 N4 61.4(17) . . . 6 ? N3 C7 N4 N5 -42(2) . . . . ? N3 C7 N4 C8 131.6(15) . . . . ? N3 C7 N4 N5 14(3) . . . 6 ? C9 C9 N5 N5 0.000(4) 6 . . 6 ? N6 C9 N5 N5 87.1(15) 6 . . 6 ? N6 C9 N5 N5 75.2(15) . . . 6 ? C9 C9 N5 N4 -84.4(12) 6 . . . ? N6 C9 N5 N4 3(2) 6 . . . ? N6 C9 N5 N4 -9(2) . . . . ? N5 C9 N5 N4 -84.4(12) 6 . . . ? N6 C9 N5 C9 87.1(15) 6 . . 6 ? N6 C9 N5 C9 75.2(15) . . . 6 ? N5 C9 N5 C9 0.000(6) 6 . . 6 ? C9 C9 N5 N4 -43.5(8) 6 . . 6 ? N6 C9 N5 N4 43.6(17) 6 . . 6 ? N6 C9 N5 N4 31.7(17) . . . 6 ? N5 C9 N5 N4 -43.5(8) 6 . . 6 ? N4 N4 N5 N5 0.000(2) 6 . . 6 ? C8 N4 N5 N5 -62.5(9) . . . 6 ? C7 N4 N5 N5 112.0(14) . . . 6 ? N4 N4 N5 C9 74.3(12) 6 . . . ? C8 N4 N5 C9 11.7(18) . . . . ? C7 N4 N5 C9 -173.7(14) . . . . ? N5 N4 N5 C9 74.3(12) 6 . . . ? N4 N4 N5 C9 51.0(10) 6 . . 6 ? C8 N4 N5 C9 -11.5(15) . . . 6 ? C7 N4 N5 C9 163.0(14) . . . 6 ? N5 N4 N5 C9 51.0(10) 6 . . 6 ? C8 N4 N5 N4 -62.5(9) . . . 6 ? C7 N4 N5 N4 112.0(14) . . . 6 ? N5 N4 N5 N4 0.000(3) 6 . . 6 ? N4 C8 N6 N6 -118.2(7) 6 . . 6 ? N4 C8 N6 N6 -64.5(7) . . . 6 ? N6 C8 N6 C9 95.9(18) 6 . . 6 ? N4 C8 N6 C9 -22(2) 6 . . 6 ? N4 C8 N6 C9 31(2) . . . 6 ? N6 C8 N6 C9 68.6(16) 6 . . . ? N4 C8 N6 C9 -49.6(18) 6 . . . ? N4 C8 N6 C9 4(2) . . . . ? N6 C8 N6 Zn2 -81.1(18) 6 . . 7_765 ? N4 C8 N6 Zn2 160.7(17) 6 . . 7_765 ? N4 C8 N6 Zn2 -145.7(16) . . . 7_765 ? C9 C9 N6 N6 180.000(4) 6 . . 6 ? N5 C9 N6 N6 81.1(13) . . . 6 ? N5 C9 N6 N6 131.1(10) 6 . . 6 ? C9 C9 N6 C8 102.0(16) 6 . . . ? N5 C9 N6 C8 3(2) . . . . ? N6 C9 N6 C8 -78.0(16) 6 . . . ? N5 C9 N6 C8 53.1(18) 6 . . . ? N5 C9 N6 C9 -98.9(13) . . . 6 ? N6 C9 N6 C9 180.000(4) 6 . . 6 ? N5 C9 N6 C9 -48.9(10) 6 . . 6 ? C9 C9 N6 Zn2 -108.3(17) 6 . . 7_765 ? N5 C9 N6 Zn2 152.8(15) . . . 7_765 ? N6 C9 N6 Zn2 71.7(17) 6 . . 7_765 ? N5 C9 N6 Zn2 -157.2(17) 6 . . 7_765 ? C1 C2 C5 C3 2.4(13) . . . . ? C1 C2 C5 C6 -175.3(8) . . . . ? C4 C3 C5 C2 -2.0(14) . . . . ? C4 C3 C5 C6 175.7(9) . . . . ? N3 C6 C5 C2 26.3(14) . . . . ? N2 C6 C5 C2 -153.3(10) . . . . ? N3 C6 C5 C3 -151.3(10) . . . . ? N2 C6 C5 C3 29.1(14) . . . . ? O2 C10 O1 Zn1 -10.2(10) . . . . ? C15 C10 O1 Zn1 167.1(9) . . . . ? O6 Zn1 O1 C10 174.2(6) 1_655 . . . ? O3 Zn1 O1 C10 -17.5(11) 8_665 . . . ? O2 Zn1 O1 C10 6.2(6) . . . . ? N1 Zn1 O1 C10 -89.2(6) . . . . ? O3W Zn1 O1 C10 85.8(6) . . . . ? O1 C10 O2 Zn1 11.1(11) . . . . ? C15 C10 O2 Zn1 -166.2(9) . . . . ? O6 Zn1 O2 C10 -33.3(10) 1_655 . . . ? O3 Zn1 O2 C10 164.7(6) 8_665 . . . ? N1 Zn1 O2 C10 79.9(6) . . . . ? O3W Zn1 O2 C10 -95.9(6) . . . . ? O1 Zn1 O2 C10 -5.9(6) . . . . ? O4 C11 O3 Zn1 -10.2(11) . . . 8_565 ? C14 C11 O3 Zn1 165.3(5) . . . 8_565 ? O3 C11 O4 Zn2 123.6(7) . . . . ? C14 C11 O4 Zn2 -51.8(9) . . . . ? O4 Zn2 O4 C11 167.8(5) 6_556 . . . ? O5 Zn2 O4 C11 -21.6(7) . . . . ? O5 Zn2 O4 C11 -145.6(9) 6_556 . . . ? N6 Zn2 O4 C11 68.3(9) 7_756 . . . ? N6 Zn2 O4 C11 74.1(9) 4_645 . . . ? O1W Zn2 O4 C11 -102.6(7) . . . . ? O6 C12 O5 Zn2 -178.1(6) . . . . ? C13 C12 O5 Zn2 4.4(12) . . . . ? O4 Zn2 O5 C12 49.6(8) . . . . ? O4 Zn2 O5 C12 95.7(13) 6_556 . . . ? O5 Zn2 O5 C12 -141.2(7) 6_556 . . . ? N6 Zn2 O5 C12 -45.3(10) 7_756 . . . ? N6 Zn2 O5 C12 -50.4(10) 4_645 . . . ? O1W Zn2 O5 C12 139.3(8) . . . . ? O5 C12 O6 Zn1 4.3(13) . . . 1_455 ? C13 C12 O6 Zn1 -178.2(6) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.851 _refine_diff_density_min -1.783 _refine_diff_density_rms 0.144 #==========================================================end