# Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Cadmium(II) Complexes with 3,5-Di(1H-imidazol-1-yl)benzoic Acid: Topological and Structural Diversity Tuned by Metal to Ligand Ratio and Counteranions ; loop_ _publ_author_name 'Wei-Yin Sun.' 'Kai Cai.' 'Shui-Sheng Chen.' 'Man-Sheng Chen.' 'Jian Fan.' ; Zhi Su ; # Attachment 'sunwy-dal-cif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 727675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Cd N4 O4,(H2O)' _chemical_formula_sum 'C15 H14 Cd N4 O5' _chemical_formula_weight 442.69 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.689(10) _cell_length_b 18.209(15) _cell_length_c 8.209(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.557(2) _cell_angle_gamma 90.00 _cell_volume 1636(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1177 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 21.08 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7713 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'sadabs, bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8284 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.1204 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2941 _reflns_number_gt 1697 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2941 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.26964(4) 0.03042(2) 0.89028(6) 0.03437(16) Uani 1 1 d . . . C1 C 0.2193(6) 0.3091(3) 0.7202(7) 0.0325(15) Uani 1 1 d . . . C2 C 0.1094(5) 0.2884(3) 0.7396(7) 0.0354(16) Uani 1 1 d . . . H2 H 0.0538 0.3241 0.7446 0.043 Uiso 1 1 calc R . . C3 C 0.0841(5) 0.2154(3) 0.7513(7) 0.0309(15) Uani 1 1 d . . . C4 C 0.1677(5) 0.1610(3) 0.7483(7) 0.0325(16) Uani 1 1 d . . . H4 H 0.1504 0.1117 0.7579 0.039 Uiso 1 1 calc R . . C5 C 0.2769(5) 0.1819(3) 0.7308(8) 0.0350(16) Uani 1 1 d . . . C6 C 0.3042(5) 0.2555(3) 0.7169(8) 0.0383(16) Uani 1 1 d . . . H6 H 0.3778 0.2689 0.7056 0.046 Uiso 1 1 calc R . . C7 C 0.2456(6) 0.3884(3) 0.6955(8) 0.0408(18) Uani 1 1 d . . . C8 C -0.1390(6) 0.2313(4) 0.6992(8) 0.0432(17) Uani 1 1 d . . . H8 H -0.1504 0.2774 0.6473 0.052 Uiso 1 1 calc R . . C9 C -0.2262(6) 0.1888(3) 0.7255(8) 0.0457(18) Uani 1 1 d . . . H9 H -0.3080 0.2016 0.6954 0.055 Uiso 1 1 calc R . . C10 C -0.0574(6) 0.1290(3) 0.8212(7) 0.0368(16) Uani 1 1 d . . . H10 H -0.0002 0.0922 0.8680 0.044 Uiso 1 1 calc R . . C11 C 0.3348(6) 0.0618(3) 0.6336(8) 0.0436(18) Uani 1 1 d . . . H11 H 0.2574 0.0461 0.5639 0.052 Uiso 1 1 calc R . . C12 C 0.4390(5) 0.0260(4) 0.6639(8) 0.0457(17) Uani 1 1 d . . . H12 H 0.4463 -0.0196 0.6176 0.055 Uiso 1 1 calc R . . C13 C 0.4837(6) 0.1262(3) 0.8085(9) 0.049(2) Uani 1 1 d . . . H13 H 0.5268 0.1634 0.8821 0.059 Uiso 1 1 calc R . . C14 C -0.1719(6) 0.0635(4) 1.2289(8) 0.0400(17) Uani 1 1 d . . . C15 C -0.1074(7) 0.0827(4) 1.4183(8) 0.071(3) Uani 1 1 d . . . H15A H -0.0606 0.1268 1.4268 0.107 Uiso 1 1 calc R . . H15B H -0.0538 0.0432 1.4753 0.107 Uiso 1 1 calc R . . H15C H -0.1667 0.0902 1.4731 0.107 Uiso 1 1 calc R . . N1 N -0.1747(4) 0.1232(3) 0.8042(6) 0.0366(13) Uani 1 1 d . . . N2 N -0.0304(4) 0.1933(2) 0.7639(6) 0.0294(12) Uani 1 1 d . . . N3 N 0.5339(5) 0.0659(3) 0.7729(7) 0.0447(15) Uani 1 1 d . . . N4 N 0.3630(4) 0.1265(2) 0.7244(6) 0.0343(13) Uani 1 1 d . . . O1 O 0.3405(4) 0.4056(2) 0.6630(6) 0.0530(13) Uani 1 1 d . . . O2 O 0.1687(4) 0.4355(2) 0.7049(5) 0.0443(12) Uani 1 1 d . . . O3 O -0.2567(4) 0.1035(2) 1.1396(6) 0.0505(13) Uani 1 1 d . . . O4 O -0.1376(4) 0.0080(2) 1.1685(5) 0.0506(13) Uani 1 1 d . . . O5 O 0.5688(5) 0.3246(3) 0.7472(8) 0.097(2) 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 0.0290(3) 0.0218(2) 0.0538(3) -0.0008(3) 0.0163(2) 0.0011(2) C1 0.033(4) 0.027(4) 0.037(4) 0.003(3) 0.012(3) 0.004(3) C2 0.031(4) 0.025(4) 0.048(4) 0.004(3) 0.012(3) 0.004(3) C3 0.023(4) 0.030(4) 0.036(4) 0.003(3) 0.006(3) 0.000(3) C4 0.029(4) 0.021(4) 0.047(4) 0.007(3) 0.013(3) 0.001(3) C5 0.024(4) 0.023(3) 0.056(4) 0.004(3) 0.012(3) -0.001(3) C6 0.024(4) 0.030(4) 0.062(4) 0.002(3) 0.017(3) -0.005(3) C7 0.049(5) 0.021(4) 0.045(4) 0.000(3) 0.007(4) -0.006(3) C8 0.039(4) 0.031(4) 0.069(5) 0.015(4) 0.029(4) 0.010(3) C9 0.027(4) 0.040(4) 0.073(5) 0.017(4) 0.021(4) 0.011(3) C10 0.031(4) 0.032(4) 0.046(4) 0.007(3) 0.012(3) 0.003(3) C11 0.029(4) 0.037(4) 0.062(5) -0.005(4) 0.012(3) -0.001(3) C12 0.034(4) 0.034(4) 0.072(5) -0.009(4) 0.022(4) 0.000(3) C13 0.028(4) 0.026(4) 0.087(5) -0.008(4) 0.012(4) -0.002(3) C14 0.047(5) 0.036(4) 0.041(4) 0.008(4) 0.020(4) -0.011(4) C15 0.099(7) 0.052(5) 0.054(5) -0.018(4) 0.015(5) -0.007(5) N1 0.025(3) 0.037(3) 0.049(3) 0.015(3) 0.015(3) 0.002(2) N2 0.025(3) 0.022(3) 0.043(3) 0.003(2) 0.014(3) 0.000(2) N3 0.029(3) 0.031(3) 0.070(4) -0.006(3) 0.012(3) -0.001(3) N4 0.023(3) 0.018(3) 0.060(3) 0.000(3) 0.013(3) 0.001(2) O1 0.044(3) 0.026(3) 0.093(4) 0.018(3) 0.029(3) -0.004(2) O2 0.046(3) 0.021(2) 0.069(3) 0.005(2) 0.023(2) 0.003(2) O3 0.046(3) 0.044(3) 0.061(3) -0.002(2) 0.019(3) 0.008(2) O4 0.063(3) 0.025(3) 0.066(3) -0.005(2) 0.026(3) 0.007(2) O5 0.063(4) 0.065(4) 0.172(5) 0.032(4) 0.051(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.251(5) 1_455 ? Cd1 N1 2.266(5) . ? Cd1 O4 2.300(4) . ? Cd1 O2 2.375(4) 2_546 ? Cd1 O3 2.401(4) . ? Cd1 O1 2.406(4) 2_546 ? C1 C6 1.398(8) . ? C1 C2 1.400(8) . ? C1 C7 1.505(8) . ? C2 C3 1.373(8) . ? C2 H2 0.9300 . ? C3 C4 1.397(8) . ? C3 N2 1.436(7) . ? C4 C5 1.387(8) . ? C4 H4 0.9300 . ? C5 C6 1.391(8) . ? C5 N4 1.440(7) . ? C6 H6 0.9300 . ? C7 O2 1.263(7) . ? C7 O1 1.268(7) . ? C7 Cd1 2.720(6) 2_556 ? C8 C9 1.355(8) . ? C8 N2 1.378(7) . ? C8 H8 0.9300 . ? C9 N1 1.390(7) . ? C9 H9 0.9300 . ? C10 N1 1.333(7) . ? C10 N2 1.340(7) . ? C10 H10 0.9300 . ? C11 C12 1.326(8) . ? C11 N4 1.370(7) . ? C11 H11 0.9300 . ? C12 N3 1.365(7) . ? C12 H12 0.9300 . ? C13 N3 1.325(7) . ? C13 N4 1.335(7) . ? C13 H13 0.9300 . ? C14 O3 1.241(7) . ? C14 O4 1.254(7) . ? C14 C15 1.511(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? N3 Cd1 2.251(5) 1_655 ? O1 Cd1 2.406(4) 2_556 ? O2 Cd1 2.375(4) 2_556 ? 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 N3 Cd1 N1 100.96(19) 1_455 . ? N3 Cd1 O4 134.77(18) 1_455 . ? N1 Cd1 O4 102.16(17) . . ? N3 Cd1 O2 128.20(17) 1_455 2_546 ? N1 Cd1 O2 94.95(17) . 2_546 ? O4 Cd1 O2 87.67(16) . 2_546 ? N3 Cd1 O3 87.42(17) 1_455 . ? N1 Cd1 O3 87.78(17) . . ? O4 Cd1 O3 55.44(15) . . ? O2 Cd1 O3 142.57(14) 2_546 . ? N3 Cd1 O1 87.65(17) 1_455 2_546 ? N1 Cd1 O1 145.37(17) . 2_546 ? O4 Cd1 O1 94.63(15) . 2_546 ? O2 Cd1 O1 55.36(15) 2_546 2_546 ? O3 Cd1 O1 126.37(16) . 2_546 ? C6 C1 C2 120.0(6) . . ? C6 C1 C7 119.2(6) . . ? C2 C1 C7 120.7(6) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.1(6) . . ? C2 C3 N2 120.4(6) . . ? C4 C3 N2 118.5(5) . . ? C5 C4 C3 118.8(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.3(6) . . ? C4 C5 N4 119.4(5) . . ? C6 C5 N4 119.3(5) . . ? C5 C6 C1 119.1(6) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? O2 C7 O1 122.6(6) . . ? O2 C7 C1 117.4(6) . . ? O1 C7 C1 120.0(6) . . ? O2 C7 Cd1 60.8(3) . 2_556 ? O1 C7 Cd1 62.2(3) . 2_556 ? C1 C7 Cd1 172.6(4) . 2_556 ? C9 C8 N2 107.1(6) . . ? C9 C8 H8 126.4 . . ? N2 C8 H8 126.4 . . ? C8 C9 N1 109.7(6) . . ? C8 C9 H9 125.1 . . ? N1 C9 H9 125.1 . . ? N1 C10 N2 113.1(5) . . ? N1 C10 H10 123.4 . . ? N2 C10 H10 123.4 . . ? C12 C11 N4 107.0(6) . . ? C12 C11 H11 126.5 . . ? N4 C11 H11 126.5 . . ? C11 C12 N3 110.0(6) . . ? C11 C12 H12 125.0 . . ? N3 C12 H12 125.0 . . ? N3 C13 N4 111.0(5) . . ? N3 C13 H13 124.5 . . ? N4 C13 H13 124.5 . . ? O3 C14 O4 122.7(6) . . ? O3 C14 C15 118.7(7) . . ? O4 C14 C15 118.7(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 N1 C9 104.0(5) . . ? C10 N1 Cd1 128.6(4) . . ? C9 N1 Cd1 127.3(4) . . ? C10 N2 C8 105.9(5) . . ? C10 N2 C3 127.6(5) . . ? C8 N2 C3 126.0(5) . . ? C13 N3 C12 105.4(5) . . ? C13 N3 Cd1 127.4(4) . 1_655 ? C12 N3 Cd1 126.9(4) . 1_655 ? C13 N4 C11 106.7(5) . . ? C13 N4 C5 127.5(5) . . ? C11 N4 C5 125.8(5) . . ? C7 O1 Cd1 90.0(4) . 2_556 ? C7 O2 Cd1 91.6(4) . 2_556 ? C14 O3 Cd1 88.7(4) . . ? C14 O4 Cd1 93.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.884 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.132 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 727676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H10 Cd N4 O3, (H2O)' _chemical_formula_sum 'C13 H12 Cd N4 O4' _chemical_formula_weight 400.64 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 'C 2/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 13.0295(17) _cell_length_b 13.8924(18) _cell_length_c 7.6163(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(2) _cell_angle_gamma 90.00 _cell_volume 1378.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2578 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 28.29 _exptl_crystal_description prism _exptl_crystal_colour corlorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5002 _exptl_absorpt_correction_T_max 0.8557 _exptl_absorpt_process_details sadabs,bruker(2000) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3444 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1231 _reflns_number_gt 1179 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+1.1788P] 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 1231 _refine_ls_number_parameters 105 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.5000 0.0000 0.02714(16) Uani 1 2 d SU . . C1 C 1.0000 0.7996(4) 0.2500 0.0284(10) Uani 1 2 d S . . C2 C 1.0813(3) 0.8493(3) 0.1771(6) 0.0314(9) Uani 1 1 d . . . H2A H 1.1348 0.8161 0.1236 0.038 Uiso 1 1 calc R . . C3 C 1.0827(3) 0.9482(3) 0.1843(5) 0.0278(8) Uani 1 1 d . . . C4 C 1.0000 0.9983(3) 0.2500 0.0310(12) Uani 1 2 d S . . H4A H 1.0000 1.0653 0.2500 0.037 Uiso 1 2 calc SR . . C5 C 1.0000 0.6900(4) 0.2500 0.0301(11) Uani 1 2 d S . . C6 C 1.1793(3) 1.0971(3) 0.0989(7) 0.0453(12) Uani 1 1 d . . . H6A H 1.1281 1.1430 0.1150 0.054 Uiso 1 1 calc R . . C7 C 1.2773(4) 1.1133(3) 0.0456(7) 0.0483(12) Uani 1 1 d . . . H7A H 1.3048 1.1733 0.0188 0.058 Uiso 1 1 calc R . . C8 C 1.2635(3) 0.9635(3) 0.0875(6) 0.0367(10) Uani 1 1 d . . . H8A H 1.2794 0.8984 0.0967 0.044 Uiso 1 1 calc R . . N1 N 1.3290(3) 1.0289(3) 0.0374(5) 0.0389(9) Uani 1 1 d . . . N2 N 1.1710(3) 1.00000(19) 0.1242(7) 0.0319(9) Uani 1 1 d . . . O1 O 1.0413(3) 0.6505(2) 0.1218(4) 0.0408(7) Uani 1 1 d . . . O2 O 1.0000 0.4218(2) 0.2500 0.0307(8) Uani 1 2 d SU . . O3 O 1.0000 0.2393(4) 0.2500 0.127(4) Uani 1 2 d S . . 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 0.0239(2) 0.0241(2) 0.0334(2) -0.00045(13) 0.0093(7) -0.00243(14) C1 0.022(2) 0.027(2) 0.036(3) 0.000 -0.006(4) 0.000 C2 0.0234(19) 0.034(2) 0.0372(19) 0.0011(17) 0.0066(18) 0.0033(17) C3 0.0230(19) 0.0239(19) 0.0365(19) 0.0000(16) 0.0070(16) -0.0038(15) C4 0.026(3) 0.025(2) 0.043(3) 0.000 -0.001(12) 0.000 C5 0.020(2) 0.028(2) 0.043(3) 0.000 -0.002(4) 0.000 C6 0.026(2) 0.029(2) 0.081(3) 0.014(2) 0.013(2) 0.0047(18) C7 0.037(2) 0.029(2) 0.079(3) 0.008(2) 0.007(2) -0.0042(19) C8 0.027(2) 0.027(2) 0.056(3) -0.004(2) 0.014(2) -0.0021(18) N1 0.0301(19) 0.0379(19) 0.049(3) -0.0017(17) 0.0102(18) -0.0030(16) N2 0.024(2) 0.028(2) 0.045(2) 0.0007(13) 0.007(2) -0.0001(13) O1 0.0443(16) 0.0279(15) 0.0502(18) -0.0070(14) 0.0157(14) -0.0076(13) O2 0.055(2) 0.0155(15) 0.0213(15) 0.000 0.011(2) 0.000 O3 0.151(7) 0.036(3) 0.195(9) 0.000 0.087(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.1919(15) 5_765 ? Cd1 O2 2.1919(15) . ? Cd1 N1 2.281(4) 7_765 ? Cd1 N1 2.281(4) 3_445 ? Cd1 O1 2.350(3) . ? Cd1 O1 2.350(3) 5_765 ? C1 C2 1.381(4) . ? C1 C2 1.381(4) 2_755 ? C1 C5 1.523(7) . ? C2 C3 1.376(6) . ? C2 H2A 0.9300 . ? C3 C4 1.377(4) . ? C3 N2 1.432(5) . ? C4 C3 1.377(4) 2_755 ? C4 H4A 0.9300 . ? C5 O1 1.243(4) . ? C5 O1 1.243(4) 2_755 ? C6 C7 1.359(6) . ? C6 N2 1.367(5) . ? C6 H6A 0.9300 . ? C7 N1 1.353(6) . ? C7 H7A 0.9300 . ? C8 N1 1.304(6) . ? C8 N2 1.336(6) . ? C8 H8A 0.9300 . ? N1 Cd1 2.281(4) 3 ? O2 Cd1 2.1919(15) 2_755 ? 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 O2 Cd1 O2 180.00(14) 5_765 . ? O2 Cd1 N1 88.79(11) 5_765 7_765 ? O2 Cd1 N1 91.21(11) . 7_765 ? O2 Cd1 N1 91.21(11) 5_765 3_445 ? O2 Cd1 N1 88.79(11) . 3_445 ? N1 Cd1 N1 180.0 7_765 3_445 ? O2 Cd1 O1 84.39(10) 5_765 . ? O2 Cd1 O1 95.61(10) . . ? N1 Cd1 O1 88.98(13) 7_765 . ? N1 Cd1 O1 91.02(13) 3_445 . ? O2 Cd1 O1 95.61(10) 5_765 5_765 ? O2 Cd1 O1 84.39(10) . 5_765 ? N1 Cd1 O1 91.02(13) 7_765 5_765 ? N1 Cd1 O1 88.98(13) 3_445 5_765 ? O1 Cd1 O1 180.0 . 5_765 ? C2 C1 C2 120.1(5) . 2_755 ? C2 C1 C5 120.0(2) . . ? C2 C1 C5 120.0(2) 2_755 . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 N2 119.4(3) . . ? C2 C3 N2 120.0(3) . . ? C3 C4 C3 119.3(5) 2_755 . ? C3 C4 H4A 120.4 2_755 . ? C3 C4 H4A 120.4 . . ? O1 C5 O1 127.6(5) . 2_755 ? O1 C5 C1 116.2(2) . . ? O1 C5 C1 116.2(2) 2_755 . ? C7 C6 N2 106.2(4) . . ? C7 C6 H6A 126.9 . . ? N2 C6 H6A 126.9 . . ? N1 C7 C6 109.8(4) . . ? N1 C7 H7A 125.1 . . ? C6 C7 H7A 125.1 . . ? N1 C8 N2 112.8(4) . . ? N1 C8 H8A 123.6 . . ? N2 C8 H8A 123.6 . . ? C8 N1 C7 105.3(4) . . ? C8 N1 Cd1 123.6(3) . 3 ? C7 N1 Cd1 130.1(3) . 3 ? C8 N2 C6 105.9(4) . . ? C8 N2 C3 126.9(3) . . ? C6 N2 C3 127.1(4) . . ? C5 O1 Cd1 127.2(3) . . ? Cd1 O2 Cd1 120.61(14) 2_755 . ? 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 C2 C1 C2 C3 2.7(3) 2_755 . . . ? C5 C1 C2 C3 -177.3(3) . . . . ? C1 C2 C3 C4 -5.5(6) . . . . ? C1 C2 C3 N2 174.1(4) . . . . ? C2 C3 C4 C3 2.8(3) . . . 2_755 ? N2 C3 C4 C3 -176.8(5) . . . 2_755 ? C2 C1 C5 O1 -33.5(3) . . . . ? C2 C1 C5 O1 146.5(3) 2_755 . . . ? C2 C1 C5 O1 146.5(3) . . . 2_755 ? C2 C1 C5 O1 -33.5(3) 2_755 . . 2_755 ? N2 C6 C7 N1 0.1(6) . . . . ? N2 C8 N1 C7 1.5(6) . . . . ? N2 C8 N1 Cd1 171.1(3) . . . 3 ? C6 C7 N1 C8 -0.9(6) . . . . ? C6 C7 N1 Cd1 -169.6(4) . . . 3 ? N1 C8 N2 C6 -1.4(6) . . . . ? N1 C8 N2 C3 -179.2(5) . . . . ? C7 C6 N2 C8 0.8(6) . . . . ? C7 C6 N2 C3 178.6(5) . . . . ? C4 C3 N2 C8 166.8(4) . . . . ? C2 C3 N2 C8 -12.7(8) . . . . ? C4 C3 N2 C6 -10.5(7) . . . . ? C2 C3 N2 C6 169.9(5) . . . . ? O1 C5 O1 Cd1 29.40(17) 2_755 . . . ? C1 C5 O1 Cd1 -150.60(17) . . . . ? O2 Cd1 O1 C5 131.2(3) 5_765 . . . ? O2 Cd1 O1 C5 -48.8(3) . . . . ? N1 Cd1 O1 C5 -139.9(3) 7_765 . . . ? N1 Cd1 O1 C5 40.1(3) 3_445 . . . ? O1 Cd1 O1 C5 -137(16) 5_765 . . . ? O2 Cd1 O2 Cd1 67(100) 5_765 . . 2_755 ? N1 Cd1 O2 Cd1 102.41(10) 7_765 . . 2_755 ? N1 Cd1 O2 Cd1 -77.59(10) 3_445 . . 2_755 ? O1 Cd1 O2 Cd1 13.31(8) . . . 2_755 ? O1 Cd1 O2 Cd1 -166.69(8) 5_765 . . 2_755 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.568 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.093 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 727677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Cd2 N8 O10 S, 5(H2O)' _chemical_formula_sum 'C26 H32 Cd2 N8 O15 S' _chemical_formula_weight 953.34 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7731(15) _cell_length_b 12.8762(18) _cell_length_c 13.8455(19) _cell_angle_alpha 99.3870(10) _cell_angle_beta 111.108(2) _cell_angle_gamma 106.958(3) _cell_volume 1634.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1299 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.42 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8452 _exptl_absorpt_correction_T_max 0.8928 _exptl_absorpt_process_details sadabs,bruker(2000) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8291 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.1277 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5714 _reflns_number_gt 3705 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5714 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.50154(6) 0.19162(5) 0.09762(5) 0.02702(18) Uani 1 1 d . . . Cd2 Cd 1.04870(6) 0.37535(5) 0.45531(5) 0.02980(18) Uani 1 1 d . . . C1 C 0.7971(7) 0.2956(6) -0.0435(6) 0.0244(18) Uani 1 1 d . . . C2 C 0.7578(7) 0.3459(6) -0.1244(5) 0.0213(17) Uani 1 1 d . . . H2 H 0.6647 0.3443 -0.1554 0.026 Uiso 1 1 calc R . . C3 C 0.8584(7) 0.3988(6) -0.1588(6) 0.0227(18) Uani 1 1 d . . . C4 C 0.9963(7) 0.3987(6) -0.1148(5) 0.0232(18) Uani 1 1 d . . . H4 H 1.0636 0.4342 -0.1383 0.028 Uiso 1 1 calc R . . C5 C 1.0323(7) 0.3465(6) -0.0373(5) 0.0216(18) Uani 1 1 d . . . C6 C 0.9334(7) 0.2942(6) -0.0002(6) 0.0256(18) Uani 1 1 d . . . H6 H 0.9591 0.2589 0.0531 0.031 Uiso 1 1 calc R . . C7 C 0.6878(9) 0.2477(7) 0.0018(6) 0.034(2) Uani 1 1 d . . . C8 C 0.6997(8) 0.4767(8) -0.2828(7) 0.044(2) Uani 1 1 d . . . H8 H 0.6248 0.4617 -0.2621 0.053 Uiso 1 1 calc R . . C9 C 0.7119(8) 0.5269(8) -0.3589(7) 0.047(3) Uani 1 1 d . . . H9 H 0.6443 0.5523 -0.4004 0.056 Uiso 1 1 calc R . . C10 C 0.8988(8) 0.4899(7) -0.2955(6) 0.035(2) Uani 1 1 d . . . H10 H 0.9870 0.4839 -0.2826 0.043 Uiso 1 1 calc R . . C11 C 1.2966(8) 0.4297(7) 0.0109(6) 0.032(2) Uani 1 1 d . . . H11 H 1.3017 0.4961 -0.0086 0.038 Uiso 1 1 calc R . . C12 C 1.4040(8) 0.3939(7) 0.0497(6) 0.035(2) Uani 1 1 d . . . H12 H 1.4986 0.4337 0.0630 0.041 Uiso 1 1 calc R . . C13 C 1.2172(8) 0.2666(7) 0.0380(6) 0.034(2) Uani 1 1 d . . . H13 H 1.1547 0.2004 0.0396 0.041 Uiso 1 1 calc R . . C14 C 0.4622(8) -0.0318(7) 0.2932(6) 0.030(2) Uani 1 1 d . . . C15 C 0.5799(8) -0.0596(6) 0.3387(6) 0.031(2) Uani 1 1 d . . . H15 H 0.6590 -0.0334 0.3238 0.037 Uiso 1 1 calc R . . C16 C 0.5791(8) -0.1275(7) 0.4075(6) 0.033(2) Uani 1 1 d . . . C17 C 0.4586(8) -0.1731(6) 0.4248(6) 0.030(2) Uani 1 1 d . . . H17 H 0.4567 -0.2214 0.4679 0.036 Uiso 1 1 calc R . . C18 C 0.3407(8) -0.1450(6) 0.3765(6) 0.0269(19) Uani 1 1 d . . . C19 C 0.3419(8) -0.0730(6) 0.3123(6) 0.030(2) Uani 1 1 d . . . H19 H 0.2634 -0.0527 0.2825 0.036 Uiso 1 1 calc R . . C20 C 0.4623(9) 0.0412(7) 0.2180(6) 0.033(2) Uani 1 1 d . . . C21 C 0.8336(9) -0.0750(7) 0.5192(6) 0.040(2) Uani 1 1 d . . . H21 H 0.8613 0.0031 0.5301 0.048 Uiso 1 1 calc R . . C22 C 0.9207(9) -0.1302(7) 0.5597(7) 0.044(2) Uani 1 1 d . . . H22 H 1.0194 -0.0959 0.6032 0.053 Uiso 1 1 calc R . . C23 C 0.7091(8) -0.2547(7) 0.4683(6) 0.033(2) Uani 1 1 d . . . H23 H 0.6293 -0.3228 0.4353 0.039 Uiso 1 1 calc R . . C24 C 0.0790(8) -0.2004(7) 0.3265(6) 0.035(2) Uani 1 1 d . . . H24 H 0.0539 -0.1736 0.2667 0.042 Uiso 1 1 calc R . . C25 C -0.0108(8) -0.2549(7) 0.3670(6) 0.034(2) Uani 1 1 d . . . H25 H -0.1097 -0.2738 0.3373 0.041 Uiso 1 1 calc R . . C26 C 0.2013(8) -0.2404(7) 0.4701(6) 0.035(2) Uani 1 1 d . . . H26 H 0.2775 -0.2461 0.5253 0.042 Uiso 1 1 calc R . . N1 N 0.8386(6) 0.5355(6) -0.3671(5) 0.0349(18) Uani 1 1 d . . . N2 N 0.8210(6) 0.4523(5) -0.2420(5) 0.0267(16) Uani 1 1 d . . . N3 N 1.3566(6) 0.2898(5) 0.0677(5) 0.0289(16) Uani 1 1 d . . . N4 N 1.1764(6) 0.3478(5) 0.0056(5) 0.0242(15) Uani 1 1 d . . . N5 N 0.8389(7) -0.2463(6) 0.5259(5) 0.0337(17) Uani 1 1 d . . . N6 N 0.7041(7) -0.1517(6) 0.4621(5) 0.0339(17) Uani 1 1 d . . . N7 N 0.0676(7) -0.2778(6) 0.4587(5) 0.0349(18) Uani 1 1 d . . . N8 N 0.2149(6) -0.1931(5) 0.3927(5) 0.0275(16) Uani 1 1 d . . . O1 O 0.7171(5) 0.1894(5) 0.0642(4) 0.0404(15) Uani 1 1 d . . . O2 O 0.5793(5) 0.2711(5) -0.0254(4) 0.0397(16) Uani 1 1 d . . . O3 O 0.5586(6) 0.0605(5) 0.1857(4) 0.0459(16) Uani 1 1 d . . . O4 O 0.3683(6) 0.0841(5) 0.1938(5) 0.0498(17) Uani 1 1 d . . . O5 O 0.8830(6) 0.2282(5) 0.2892(4) 0.0551(18) Uani 1 1 d . . . O6 O 0.6580(6) 0.3139(5) 0.2648(5) 0.0526(18) Uani 1 1 d . . . O7 O 0.8758(5) 0.4650(5) 0.3987(4) 0.0356(14) Uani 1 1 d . . . O8 O 0.7584(6) 0.4815(6) 0.2204(5) 0.077(2) Uani 1 1 d . . . O9 O 0.6535(7) 0.4903(6) 0.3446(5) 0.078(2) Uani 1 1 d . . . O10 O 0.3332(5) 0.0354(5) -0.0576(4) 0.0470(16) Uani 1 1 d . . . S1 S 0.7342(2) 0.43920(19) 0.30513(17) 0.0338(5) Uani 1 1 d . . . O11 O 0.3885(7) 0.3205(6) -0.2163(5) 0.083(2) Uani 1 1 d . . . O12 O 0.5474(8) -0.2870(6) 0.6277(6) 0.092(3) Uani 1 1 d . . . O13 O 1.0944(11) 0.1812(11) 0.2145(8) 0.188(5) Uani 1 1 d . . . O14 O 1.1685(13) 0.1054(11) 0.7797(9) 0.237(6) Uani 1 1 d . . . O15 O 1.0637(12) -0.0153(10) 0.0934(15) 0.369(13) 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 0.0267(3) 0.0300(4) 0.0334(4) 0.0183(3) 0.0172(3) 0.0129(3) Cd2 0.0328(4) 0.0326(4) 0.0310(4) 0.0179(3) 0.0186(3) 0.0113(3) C1 0.026(4) 0.018(4) 0.030(5) 0.011(4) 0.014(4) 0.006(4) C2 0.019(4) 0.022(4) 0.027(4) 0.008(4) 0.011(3) 0.012(4) C3 0.026(4) 0.021(4) 0.023(4) 0.005(4) 0.013(4) 0.008(4) C4 0.029(4) 0.021(4) 0.029(4) 0.018(4) 0.019(4) 0.009(4) C5 0.021(4) 0.016(4) 0.022(4) 0.003(4) 0.007(3) 0.003(4) C6 0.030(4) 0.028(5) 0.025(4) 0.015(4) 0.015(4) 0.012(4) C7 0.036(5) 0.028(5) 0.023(5) 0.000(4) 0.017(4) -0.008(4) C8 0.037(5) 0.068(7) 0.052(6) 0.043(6) 0.028(5) 0.029(5) C9 0.038(5) 0.070(7) 0.053(6) 0.039(6) 0.024(5) 0.031(5) C10 0.033(5) 0.054(6) 0.036(5) 0.027(5) 0.022(4) 0.025(5) C11 0.029(5) 0.027(5) 0.048(5) 0.021(4) 0.022(4) 0.011(4) C12 0.024(4) 0.040(6) 0.046(6) 0.019(5) 0.018(4) 0.014(4) C13 0.028(5) 0.036(6) 0.038(5) 0.014(5) 0.017(4) 0.008(4) C14 0.037(5) 0.027(5) 0.042(5) 0.020(4) 0.026(4) 0.015(4) C15 0.032(5) 0.026(5) 0.040(5) 0.015(4) 0.024(4) 0.005(4) C16 0.029(5) 0.040(6) 0.042(5) 0.019(5) 0.023(4) 0.016(4) C17 0.042(5) 0.023(5) 0.039(5) 0.020(4) 0.029(4) 0.010(4) C18 0.042(5) 0.022(5) 0.027(5) 0.012(4) 0.022(4) 0.014(4) C19 0.029(4) 0.030(5) 0.034(5) 0.011(4) 0.017(4) 0.010(4) C20 0.040(5) 0.020(5) 0.033(5) 0.011(4) 0.012(4) 0.006(4) C21 0.040(5) 0.019(5) 0.042(6) 0.006(4) 0.003(5) 0.007(5) C22 0.038(5) 0.035(6) 0.047(6) 0.014(5) 0.010(5) 0.008(5) C23 0.030(5) 0.027(5) 0.036(5) 0.015(4) 0.014(4) 0.001(4) C24 0.047(5) 0.029(5) 0.033(5) 0.014(4) 0.022(4) 0.010(5) C25 0.028(5) 0.035(5) 0.030(5) 0.004(4) 0.011(4) 0.004(4) C26 0.036(5) 0.041(6) 0.040(5) 0.026(5) 0.025(4) 0.014(5) N1 0.034(4) 0.052(5) 0.033(4) 0.028(4) 0.018(3) 0.023(4) N2 0.030(4) 0.031(4) 0.030(4) 0.020(3) 0.019(3) 0.012(3) N3 0.027(4) 0.028(4) 0.035(4) 0.016(3) 0.014(3) 0.011(3) N4 0.025(4) 0.030(4) 0.028(4) 0.018(3) 0.015(3) 0.014(3) N5 0.028(4) 0.035(5) 0.037(4) 0.016(4) 0.015(3) 0.007(4) N6 0.037(4) 0.036(5) 0.048(5) 0.027(4) 0.027(4) 0.020(4) N7 0.038(4) 0.035(5) 0.040(4) 0.019(4) 0.022(4) 0.013(4) N8 0.027(4) 0.029(4) 0.034(4) 0.017(3) 0.018(3) 0.009(3) O1 0.047(3) 0.048(4) 0.038(3) 0.031(3) 0.027(3) 0.013(3) O2 0.033(3) 0.057(4) 0.049(4) 0.029(3) 0.029(3) 0.020(3) O3 0.055(4) 0.056(4) 0.055(4) 0.036(4) 0.040(3) 0.027(4) O4 0.055(4) 0.053(4) 0.068(4) 0.048(4) 0.036(4) 0.028(4) O5 0.050(4) 0.053(4) 0.038(4) 0.007(3) 0.000(3) 0.014(4) O6 0.040(4) 0.027(4) 0.058(4) 0.004(3) -0.001(3) 0.003(3) O7 0.025(3) 0.037(4) 0.027(3) 0.011(3) -0.001(2) 0.003(3) O8 0.054(4) 0.102(6) 0.043(4) 0.046(4) 0.002(3) -0.003(4) O9 0.070(5) 0.084(6) 0.067(5) -0.006(4) 0.011(4) 0.053(5) O10 0.049(4) 0.031(4) 0.036(4) -0.002(3) 0.003(3) 0.008(3) S1 0.0310(12) 0.0344(14) 0.0307(13) 0.0108(11) 0.0083(10) 0.0111(11) O11 0.086(5) 0.083(6) 0.061(5) 0.005(4) 0.011(4) 0.041(5) O12 0.141(7) 0.098(6) 0.117(6) 0.063(5) 0.106(6) 0.073(6) O13 0.184(10) 0.293(15) 0.117(8) 0.084(10) 0.088(8) 0.090(11) O14 0.228(12) 0.203(13) 0.173(11) 0.024(10) -0.027(10) 0.099(11) O15 0.140(10) 0.096(10) 0.58(3) -0.005(15) -0.099(13) 0.026(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.250(6) 1_455 ? Cd1 O6 2.266(5) . ? Cd1 O3 2.335(6) . ? Cd1 O10 2.368(5) . ? Cd1 O2 2.397(5) . ? Cd1 O1 2.532(5) . ? Cd1 O4 2.563(5) . ? Cd2 N1 2.235(6) 2_765 ? Cd2 N7 2.283(6) 2_656 ? Cd2 N5 2.320(7) 2_756 ? Cd2 O7 2.337(5) 2_766 ? Cd2 O5 2.390(5) . ? Cd2 O7 2.431(5) . ? C1 C6 1.379(9) . ? C1 C2 1.382(9) . ? C1 C7 1.547(9) . ? C2 C3 1.383(9) . ? C2 H2 0.9300 . ? C3 C4 1.388(9) . ? C3 N2 1.432(9) . ? C4 C5 1.357(9) . ? C4 H4 0.9300 . ? C5 C6 1.393(9) . ? C5 N4 1.442(8) . ? C6 H6 0.9300 . ? C7 O2 1.235(9) . ? C7 O1 1.251(9) . ? C8 C9 1.349(10) . ? C8 N2 1.375(9) . ? C8 H8 0.9300 . ? C9 N1 1.384(9) . ? C9 H9 0.9300 . ? C10 N1 1.303(9) . ? C10 N2 1.346(8) . ? C10 H10 0.9300 . ? C11 C12 1.336(10) . ? C11 N4 1.379(8) . ? C11 H11 0.9300 . ? C12 N3 1.386(9) . ? C12 H12 0.9300 . ? C13 N3 1.329(8) . ? C13 N4 1.329(9) . ? C13 H13 0.9300 . ? C14 C15 1.377(10) . ? C14 C19 1.387(9) . ? C14 C20 1.513(10) . ? C15 C16 1.394(10) . ? C15 H15 0.9300 . ? C16 C17 1.384(9) . ? C16 N6 1.438(9) . ? C17 C18 1.388(10) . ? C17 H17 0.9300 . ? C18 C19 1.386(9) . ? C18 N8 1.430(8) . ? C19 H19 0.9300 . ? C20 O3 1.248(9) . ? C20 O4 1.259(9) . ? C21 N6 1.302(9) . ? C21 C22 1.357(11) . ? C21 H21 0.9300 . ? C22 N5 1.392(9) . ? C22 H22 0.9300 . ? C23 N5 1.298(9) . ? C23 N6 1.357(10) . ? C23 H23 0.9300 . ? C24 C25 1.365(9) . ? C24 N8 1.385(9) . ? C24 H24 0.9300 . ? C25 N7 1.381(9) . ? C25 H25 0.9300 . ? C26 N7 1.318(8) . ? C26 N8 1.348(8) . ? C26 H26 0.9300 . ? N1 Cd2 2.235(6) 2_765 ? N3 Cd1 2.250(6) 1_655 ? N5 Cd2 2.320(7) 2_756 ? N7 Cd2 2.283(6) 2_656 ? O6 S1 1.481(6) . ? O7 S1 1.503(5) . ? O7 Cd2 2.337(5) 2_766 ? O8 S1 1.445(6) . ? O9 S1 1.430(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 O6 93.6(2) 1_455 . ? N3 Cd1 O3 142.7(2) 1_455 . ? O6 Cd1 O3 81.1(2) . . ? N3 Cd1 O10 92.6(2) 1_455 . ? O6 Cd1 O10 168.1(2) . . ? O3 Cd1 O10 87.9(2) . . ? N3 Cd1 O2 85.4(2) 1_455 . ? O6 Cd1 O2 105.2(2) . . ? O3 Cd1 O2 131.72(19) . . ? O10 Cd1 O2 85.43(18) . . ? N3 Cd1 O1 136.9(2) 1_455 . ? O6 Cd1 O1 87.79(19) . . ? O3 Cd1 O1 80.06(18) . . ? O10 Cd1 O1 94.58(18) . . ? O2 Cd1 O1 53.04(17) . . ? N3 Cd1 O4 89.9(2) 1_455 . ? O6 Cd1 O4 86.1(2) . . ? O3 Cd1 O4 53.04(18) . . ? O10 Cd1 O4 83.76(19) . . ? O2 Cd1 O4 168.01(18) . . ? O1 Cd1 O4 133.08(19) . . ? N1 Cd2 N7 177.8(2) 2_765 2_656 ? N1 Cd2 N5 95.9(2) 2_765 2_756 ? N7 Cd2 N5 82.5(2) 2_656 2_756 ? N1 Cd2 O7 96.8(2) 2_765 2_766 ? N7 Cd2 O7 85.3(2) 2_656 2_766 ? N5 Cd2 O7 120.3(2) 2_756 2_766 ? N1 Cd2 O5 89.9(2) 2_765 . ? N7 Cd2 O5 88.4(2) 2_656 . ? N5 Cd2 O5 81.5(2) 2_756 . ? O7 Cd2 O5 156.11(19) 2_766 . ? N1 Cd2 O7 88.6(2) 2_765 . ? N7 Cd2 O7 92.6(2) 2_656 . ? N5 Cd2 O7 164.3(2) 2_756 . ? O7 Cd2 O7 73.81(17) 2_766 . ? O5 Cd2 O7 83.51(19) . . ? C6 C1 C2 120.5(6) . . ? C6 C1 C7 121.0(7) . . ? C2 C1 C7 118.4(7) . . ? C1 C2 C3 119.3(6) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 120.5(7) . . ? C2 C3 N2 120.5(6) . . ? C4 C3 N2 119.0(6) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.9(7) . . ? C4 C5 N4 117.7(6) . . ? C6 C5 N4 121.4(6) . . ? C1 C6 C5 119.2(7) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O2 C7 O1 125.0(7) . . ? O2 C7 C1 117.6(8) . . ? O1 C7 C1 117.5(8) . . ? C9 C8 N2 105.8(7) . . ? C9 C8 H8 127.1 . . ? N2 C8 H8 127.1 . . ? C8 C9 N1 110.8(8) . . ? C8 C9 H9 124.6 . . ? N1 C9 H9 124.6 . . ? N1 C10 N2 113.5(7) . . ? N1 C10 H10 123.3 . . ? N2 C10 H10 123.3 . . ? C12 C11 N4 105.8(7) . . ? C12 C11 H11 127.1 . . ? N4 C11 H11 127.1 . . ? C11 C12 N3 111.4(7) . . ? C11 C12 H12 124.3 . . ? N3 C12 H12 124.3 . . ? N3 C13 N4 113.1(7) . . ? N3 C13 H13 123.4 . . ? N4 C13 H13 123.4 . . ? C15 C14 C19 121.0(7) . . ? C15 C14 C20 119.3(7) . . ? C19 C14 C20 119.6(7) . . ? C14 C15 C16 119.2(7) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 120.9(7) . . ? C17 C16 N6 118.4(7) . . ? C15 C16 N6 120.6(7) . . ? C16 C17 C18 118.4(7) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 121.6(7) . . ? C19 C18 N8 119.6(7) . . ? C17 C18 N8 118.8(7) . . ? C18 C19 C14 118.7(7) . . ? C18 C19 H19 120.7 . . ? C14 C19 H19 120.7 . . ? O3 C20 O4 122.4(8) . . ? O3 C20 C14 119.1(8) . . ? O4 C20 C14 118.5(7) . . ? N6 C21 C22 107.2(8) . . ? N6 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? C21 C22 N5 109.1(7) . . ? C21 C22 H22 125.5 . . ? N5 C22 H22 125.5 . . ? N5 C23 N6 111.8(7) . . ? N5 C23 H23 124.1 . . ? N6 C23 H23 124.1 . . ? C25 C24 N8 106.1(7) . . ? C25 C24 H24 127.0 . . ? N8 C24 H24 127.0 . . ? C24 C25 N7 109.7(7) . . ? C24 C25 H25 125.2 . . ? N7 C25 H25 125.2 . . ? N7 C26 N8 112.3(7) . . ? N7 C26 H26 123.9 . . ? N8 C26 H26 123.9 . . ? C10 N1 C9 103.8(6) . . ? C10 N1 Cd2 122.3(5) . 2_765 ? C9 N1 Cd2 133.2(5) . 2_765 ? C10 N2 C8 106.1(6) . . ? C10 N2 C3 126.7(6) . . ? C8 N2 C3 127.2(6) . . ? C13 N3 C12 103.0(7) . . ? C13 N3 Cd1 136.4(6) . 1_655 ? C12 N3 Cd1 118.8(5) . 1_655 ? C13 N4 C11 106.7(6) . . ? C13 N4 C5 127.2(6) . . ? C11 N4 C5 125.9(6) . . ? C23 N5 C22 104.0(8) . . ? C23 N5 Cd2 134.1(6) . 2_756 ? C22 N5 Cd2 120.1(5) . 2_756 ? C21 N6 C23 107.9(7) . . ? C21 N6 C16 124.5(7) . . ? C23 N6 C16 127.5(7) . . ? C26 N7 C25 105.4(6) . . ? C26 N7 Cd2 134.9(5) . 2_656 ? C25 N7 Cd2 119.5(5) . 2_656 ? C26 N8 C24 106.5(6) . . ? C26 N8 C18 129.1(7) . . ? C24 N8 C18 124.4(6) . . ? C7 O1 Cd1 87.5(5) . . ? C7 O2 Cd1 94.1(5) . . ? C20 O3 Cd1 97.7(5) . . ? C20 O4 Cd1 86.8(5) . . ? S1 O6 Cd1 132.6(4) . . ? S1 O7 Cd2 115.5(3) . 2_766 ? S1 O7 Cd2 137.9(3) . . ? Cd2 O7 Cd2 106.19(17) 2_766 . ? O9 S1 O8 111.7(5) . . ? O9 S1 O6 109.7(4) . . ? O8 S1 O6 110.2(4) . . ? O9 S1 O7 108.2(4) . . ? O8 S1 O7 109.8(3) . . ? O6 S1 O7 107.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.4(11) . . . . ? C7 C1 C2 C3 173.9(7) . . . . ? C1 C2 C3 C4 1.7(11) . . . . ? C1 C2 C3 N2 -179.6(7) . . . . ? C2 C3 C4 C5 -0.2(11) . . . . ? N2 C3 C4 C5 -178.8(6) . . . . ? C3 C4 C5 C6 -0.8(11) . . . . ? C3 C4 C5 N4 179.6(7) . . . . ? C2 C1 C6 C5 1.4(11) . . . . ? C7 C1 C6 C5 -174.8(7) . . . . ? C4 C5 C6 C1 0.2(11) . . . . ? N4 C5 C6 C1 179.8(7) . . . . ? C6 C1 C7 O2 166.2(7) . . . . ? C2 C1 C7 O2 -10.1(11) . . . . ? C6 C1 C7 O1 -12.9(11) . . . . ? C2 C1 C7 O1 170.8(7) . . . . ? N2 C8 C9 N1 -0.3(11) . . . . ? N4 C11 C12 N3 1.3(9) . . . . ? C19 C14 C15 C16 -1.9(12) . . . . ? C20 C14 C15 C16 -179.6(7) . . . . ? C14 C15 C16 C17 4.2(12) . . . . ? C14 C15 C16 N6 -175.7(7) . . . . ? C15 C16 C17 C18 -3.2(12) . . . . ? N6 C16 C17 C18 176.8(7) . . . . ? C16 C17 C18 C19 -0.1(12) . . . . ? C16 C17 C18 N8 179.1(7) . . . . ? C17 C18 C19 C14 2.3(12) . . . . ? N8 C18 C19 C14 -176.9(7) . . . . ? C15 C14 C19 C18 -1.3(12) . . . . ? C20 C14 C19 C18 176.4(7) . . . . ? C15 C14 C20 O3 10.6(12) . . . . ? C19 C14 C20 O3 -167.1(7) . . . . ? C15 C14 C20 O4 -166.4(8) . . . . ? C19 C14 C20 O4 15.9(11) . . . . ? N6 C21 C22 N5 -0.5(10) . . . . ? N8 C24 C25 N7 2.1(9) . . . . ? N2 C10 N1 C9 0.2(10) . . . . ? N2 C10 N1 Cd2 172.5(5) . . . 2_765 ? C8 C9 N1 C10 0.1(10) . . . . ? C8 C9 N1 Cd2 -171.0(6) . . . 2_765 ? N1 C10 N2 C8 -0.4(10) . . . . ? N1 C10 N2 C3 -179.8(7) . . . . ? C9 C8 N2 C10 0.4(10) . . . . ? C9 C8 N2 C3 179.8(7) . . . . ? C2 C3 N2 C10 -168.3(7) . . . . ? C4 C3 N2 C10 10.4(12) . . . . ? C2 C3 N2 C8 12.5(12) . . . . ? C4 C3 N2 C8 -168.9(8) . . . . ? N4 C13 N3 C12 -1.2(9) . . . . ? N4 C13 N3 Cd1 -164.4(5) . . . 1_655 ? C11 C12 N3 C13 -0.1(9) . . . . ? C11 C12 N3 Cd1 166.7(5) . . . 1_655 ? N3 C13 N4 C11 2.0(9) . . . . ? N3 C13 N4 C5 176.3(6) . . . . ? C12 C11 N4 C13 -1.9(9) . . . . ? C12 C11 N4 C5 -176.3(7) . . . . ? C4 C5 N4 C13 -145.8(7) . . . . ? C6 C5 N4 C13 34.7(11) . . . . ? C4 C5 N4 C11 27.5(11) . . . . ? C6 C5 N4 C11 -152.1(7) . . . . ? N6 C23 N5 C22 1.0(9) . . . . ? N6 C23 N5 Cd2 -163.0(5) . . . 2_756 ? C21 C22 N5 C23 -0.3(9) . . . . ? C21 C22 N5 Cd2 166.5(5) . . . 2_756 ? C22 C21 N6 C23 1.1(9) . . . . ? C22 C21 N6 C16 178.5(7) . . . . ? N5 C23 N6 C21 -1.3(9) . . . . ? N5 C23 N6 C16 -178.6(7) . . . . ? C17 C16 N6 C21 -128.8(8) . . . . ? C15 C16 N6 C21 51.2(12) . . . . ? C17 C16 N6 C23 48.1(12) . . . . ? C15 C16 N6 C23 -132.0(8) . . . . ? N8 C26 N7 C25 1.1(10) . . . . ? N8 C26 N7 Cd2 175.6(5) . . . 2_656 ? C24 C25 N7 C26 -1.9(9) . . . . ? C24 C25 N7 Cd2 -177.5(5) . . . 2_656 ? N7 C26 N8 C24 0.2(10) . . . . ? N7 C26 N8 C18 -178.9(7) . . . . ? C25 C24 N8 C26 -1.4(9) . . . . ? C25 C24 N8 C18 177.8(7) . . . . ? C19 C18 N8 C26 -162.0(8) . . . . ? C17 C18 N8 C26 18.8(12) . . . . ? C19 C18 N8 C24 19.0(11) . . . . ? C17 C18 N8 C24 -160.1(7) . . . . ? O2 C7 O1 Cd1 -6.7(8) . . . . ? C1 C7 O1 Cd1 172.4(6) . . . . ? N3 Cd1 O1 C7 -14.4(6) 1_455 . . . ? O6 Cd1 O1 C7 -107.4(5) . . . . ? O3 Cd1 O1 C7 171.3(5) . . . . ? O10 Cd1 O1 C7 84.3(5) . . . . ? O2 Cd1 O1 C7 3.5(4) . . . . ? O4 Cd1 O1 C7 170.0(4) . . . . ? O1 C7 O2 Cd1 7.0(9) . . . . ? C1 C7 O2 Cd1 -172.0(6) . . . . ? N3 Cd1 O2 C7 164.2(5) 1_455 . . . ? O6 Cd1 O2 C7 71.7(5) . . . . ? O3 Cd1 O2 C7 -19.8(6) . . . . ? O10 Cd1 O2 C7 -102.8(5) . . . . ? O1 Cd1 O2 C7 -3.6(5) . . . . ? O4 Cd1 O2 C7 -128.4(9) . . . . ? O4 C20 O3 Cd1 3.8(9) . . . . ? C14 C20 O3 Cd1 -173.1(6) . . . . ? N3 Cd1 O3 C20 5.7(7) 1_455 . . . ? O6 Cd1 O3 C20 89.9(5) . . . . ? O10 Cd1 O3 C20 -85.8(5) . . . . ? O2 Cd1 O3 C20 -167.7(4) . . . . ? O1 Cd1 O3 C20 179.2(5) . . . . ? O4 Cd1 O3 C20 -2.0(5) . . . . ? O3 C20 O4 Cd1 -3.5(8) . . . . ? C14 C20 O4 Cd1 173.5(6) . . . . ? N3 Cd1 O4 C20 -173.4(5) 1_455 . . . ? O6 Cd1 O4 C20 -79.8(5) . . . . ? O3 Cd1 O4 C20 2.0(4) . . . . ? O10 Cd1 O4 C20 94.0(5) . . . . ? O2 Cd1 O4 C20 119.7(10) . . . . ? O1 Cd1 O4 C20 3.5(6) . . . . ? N3 Cd1 O6 S1 -51.3(5) 1_455 . . . ? O3 Cd1 O6 S1 165.9(5) . . . . ? O10 Cd1 O6 S1 -172.6(7) . . . . ? O2 Cd1 O6 S1 34.9(5) . . . . ? O1 Cd1 O6 S1 85.6(5) . . . . ? O4 Cd1 O6 S1 -141.0(5) . . . . ? N1 Cd2 O7 S1 90.4(5) 2_765 . . . ? N7 Cd2 O7 S1 -87.7(5) 2_656 . . . ? N5 Cd2 O7 S1 -16.5(10) 2_756 . . . ? O7 Cd2 O7 S1 -172.1(6) 2_766 . . . ? O5 Cd2 O7 S1 0.3(4) . . . . ? N1 Cd2 O7 Cd2 -97.5(2) 2_765 . . 2_766 ? N7 Cd2 O7 Cd2 84.4(2) 2_656 . . 2_766 ? N5 Cd2 O7 Cd2 155.6(6) 2_756 . . 2_766 ? O7 Cd2 O7 Cd2 0.0 2_766 . . 2_766 ? O5 Cd2 O7 Cd2 172.4(2) . . . 2_766 ? Cd1 O6 S1 O9 94.5(5) . . . . ? Cd1 O6 S1 O8 -28.8(6) . . . . ? Cd1 O6 S1 O7 -148.3(4) . . . . ? Cd2 O7 S1 O9 -22.8(4) 2_766 . . . ? Cd2 O7 S1 O9 148.8(5) . . . . ? Cd2 O7 S1 O8 99.3(4) 2_766 . . . ? Cd2 O7 S1 O8 -89.1(5) . . . . ? Cd2 O7 S1 O6 -141.0(3) 2_766 . . . ? Cd2 O7 S1 O6 30.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.765 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.123 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 727678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd N8 O4, (H2O)' _chemical_formula_sum 'C26 H20 Cd N8 O5' _chemical_formula_weight 636.88 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 ' C 2/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 32.732(3) _cell_length_b 8.3330(8) _cell_length_c 17.4514(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.845(2) _cell_angle_gamma 90.00 _cell_volume 4757.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5906 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6408 _exptl_absorpt_correction_T_max 0.9620 _exptl_absorpt_process_details 'sadabs, bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12344 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4664 _reflns_number_gt 4278 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+4.9657P] 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 4664 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.116670(7) 0.55461(3) 0.683820(13) 0.02330(11) Uani 1 1 d . . . C1 C -0.01237(10) 0.1396(4) 0.38082(18) 0.0235(7) Uani 1 1 d . . . C2 C 0.01306(11) 0.1967(4) 0.43968(19) 0.0254(7) Uani 1 1 d . . . H2 H 0.0070 0.2929 0.4638 0.030 Uiso 1 1 calc R . . C3 C 0.04741(10) 0.1109(4) 0.46248(19) 0.0231(7) Uani 1 1 d . . . C4 C 0.05661(11) -0.0323(4) 0.4276(2) 0.0256(8) Uani 1 1 d . . . H4 H 0.0801 -0.0887 0.4423 0.031 Uiso 1 1 calc R . . C5 C 0.03057(11) -0.0908(4) 0.3708(2) 0.0254(7) Uani 1 1 d . . . C6 C -0.00399(11) -0.0068(4) 0.34706(19) 0.0258(7) Uani 1 1 d . . . H6 H -0.0214 -0.0480 0.3088 0.031 Uiso 1 1 calc R . . C7 C -0.04844(11) 0.2394(4) 0.3534(2) 0.0296(8) Uani 1 1 d . . . C8 C 0.09919(11) 0.0741(4) 0.5696(2) 0.0277(8) Uani 1 1 d . . . H8 H 0.1030 -0.0363 0.5664 0.033 Uiso 1 1 calc R . . C9 C 0.11761(11) 0.1753(4) 0.6199(2) 0.0313(8) Uani 1 1 d . . . H9 H 0.1366 0.1449 0.6579 0.038 Uiso 1 1 calc R . . C10 C 0.07793(11) 0.3194(4) 0.5487(2) 0.0270(8) Uani 1 1 d . . . H10 H 0.0639 0.4065 0.5273 0.032 Uiso 1 1 calc R . . C11 C 0.02168(15) -0.3826(6) 0.3451(3) 0.0528(13) Uani 1 1 d . . . H11 H -0.0020 -0.4011 0.3719 0.063 Uiso 1 1 calc R . . C12 C 0.04399(16) -0.4928(6) 0.3071(3) 0.0524(13) Uani 1 1 d . . . H12 H 0.0381 -0.6019 0.3043 0.063 Uiso 1 1 calc R . . C13 C 0.07389(12) -0.2696(5) 0.2936(2) 0.0358(9) Uani 1 1 d . . . H13 H 0.0926 -0.1913 0.2802 0.043 Uiso 1 1 calc R . . C14 C 0.23188(11) 0.5546(4) 1.0880(2) 0.0269(8) Uani 1 1 d . . . C15 C 0.26578(12) 0.4669(4) 1.0677(2) 0.0294(8) Uani 1 1 d . . . H15 H 0.2834 0.4252 1.1055 0.035 Uiso 1 1 calc R . . C16 C 0.27345(11) 0.4414(4) 0.9914(2) 0.0255(8) Uani 1 1 d . . . C17 C 0.24803(11) 0.5052(5) 0.9340(2) 0.0277(8) Uani 1 1 d . . . H17 H 0.2538 0.4911 0.8826 0.033 Uiso 1 1 calc R . . C18 C 0.21370(11) 0.5909(4) 0.9552(2) 0.0253(7) Uani 1 1 d . . . C19 C 0.20574(11) 0.6145(4) 1.03185(19) 0.0256(7) Uani 1 1 d . . . H19 H 0.1826 0.6712 1.0454 0.031 Uiso 1 1 calc R . . C20 C 0.33556(11) 0.2799(4) 1.0250(2) 0.0301(8) Uani 1 1 d . . . H20 H 0.3360 0.2930 1.0780 0.036 Uiso 1 1 calc R . . C21 C 0.36175(11) 0.1925(4) 0.9841(2) 0.0293(8) Uani 1 1 d . . . H21 H 0.3838 0.1349 1.0048 0.035 Uiso 1 1 calc R . . C22 C 0.31872(11) 0.2939(4) 0.9026(2) 0.0285(8) Uani 1 1 d . . . H22 H 0.3049 0.3205 0.8570 0.034 Uiso 1 1 calc R . . C23 C 0.13538(12) 0.7711(5) 0.8381(2) 0.0364(9) Uani 1 1 d . . . H23 H 0.1136 0.8400 0.8268 0.044 Uiso 1 1 calc R . . C24 C 0.15667(12) 0.7658(5) 0.9057(2) 0.0364(9) Uani 1 1 d . . . H24 H 0.1524 0.8286 0.9488 0.044 Uiso 1 1 calc R . . C25 C 0.18076(12) 0.5890(5) 0.8264(2) 0.0303(8) Uani 1 1 d . . . H25 H 0.1967 0.5076 0.8064 0.036 Uiso 1 1 calc R . . C26 C 0.22308(13) 0.5791(4) 1.1719(2) 0.0310(8) Uani 1 1 d . . . N1 N 0.10442(9) 0.3296(4) 0.60717(17) 0.0283(7) Uani 1 1 d . . . N2 N 0.07371(8) 0.1667(3) 0.52381(15) 0.0234(6) Uani 1 1 d . . . N3 N 0.07636(11) -0.4205(4) 0.27362(18) 0.0349(8) Uani 1 1 d . . . N4 N 0.04084(9) -0.2413(4) 0.33612(17) 0.0286(7) Uani 1 1 d . . . N5 N 0.15065(9) 0.6597(4) 0.78855(17) 0.0308(7) Uani 1 1 d . . . N6 N 0.18583(9) 0.6488(4) 0.89782(16) 0.0262(6) Uani 1 1 d . . . N7 N 0.35118(9) 0.2009(4) 0.90747(16) 0.0264(6) Uani 1 1 d . . . N8 N 0.30800(9) 0.3460(4) 0.97255(16) 0.0261(6) Uani 1 1 d . . . O1 O -0.05618(8) 0.3627(3) 0.39161(18) 0.0419(7) Uani 1 1 d . . . O2 O -0.06850(8) 0.1963(4) 0.29577(16) 0.0423(7) Uani 1 1 d . . . O3 O 0.18649(8) 0.6150(4) 1.18675(14) 0.0375(6) Uani 1 1 d . . . O4 O 0.25151(9) 0.5629(4) 1.22024(16) 0.0452(8) Uani 1 1 d . . . O5 O 0.17457(10) 0.8694(4) 0.28382(18) 0.0538(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 0.02630(16) 0.02775(17) 0.01561(15) 0.00166(9) -0.00314(10) -0.00455(10) C1 0.0213(17) 0.0300(19) 0.0192(17) 0.0040(14) 0.0001(13) 0.0001(14) C2 0.0280(19) 0.0225(18) 0.0256(18) 0.0008(14) 0.0020(14) 0.0028(14) C3 0.0226(17) 0.0269(18) 0.0196(17) -0.0029(14) -0.0029(13) -0.0029(15) C4 0.0225(18) 0.0280(19) 0.0261(19) 0.0003(14) -0.0028(14) 0.0051(14) C5 0.0258(18) 0.0280(18) 0.0225(18) -0.0034(14) 0.0017(14) 0.0005(15) C6 0.0270(19) 0.0323(19) 0.0178(17) -0.0014(14) -0.0036(14) -0.0002(16) C7 0.0216(18) 0.032(2) 0.035(2) 0.0123(16) 0.0017(15) -0.0016(15) C8 0.029(2) 0.0276(19) 0.0265(19) 0.0015(14) -0.0040(15) 0.0044(15) C9 0.029(2) 0.037(2) 0.0272(19) 0.0010(16) -0.0042(15) 0.0023(16) C10 0.0275(19) 0.0282(19) 0.0250(18) -0.0017(14) -0.0043(14) 0.0021(15) C11 0.053(3) 0.045(3) 0.062(3) -0.017(2) 0.030(2) -0.010(2) C12 0.065(3) 0.036(2) 0.058(3) -0.014(2) 0.026(3) -0.012(2) C13 0.038(2) 0.038(2) 0.032(2) -0.0048(17) 0.0087(17) -0.0011(17) C14 0.0279(19) 0.033(2) 0.0198(18) -0.0023(14) 0.0016(15) -0.0012(15) C15 0.030(2) 0.038(2) 0.0197(18) -0.0005(15) -0.0032(15) 0.0042(16) C16 0.0223(18) 0.032(2) 0.0225(18) -0.0028(14) 0.0039(14) -0.0010(14) C17 0.030(2) 0.037(2) 0.0158(17) -0.0030(15) -0.0002(14) 0.0003(17) C18 0.0214(17) 0.0327(19) 0.0218(18) -0.0002(14) -0.0032(14) -0.0028(15) C19 0.0238(18) 0.0332(19) 0.0198(17) -0.0011(15) 0.0025(14) 0.0012(15) C20 0.032(2) 0.039(2) 0.0198(17) -0.0019(15) -0.0020(14) 0.0013(16) C21 0.0267(19) 0.032(2) 0.0286(19) 0.0003(15) -0.0017(15) 0.0022(15) C22 0.0291(19) 0.036(2) 0.0206(18) -0.0034(15) 0.0003(14) -0.0014(16) C23 0.034(2) 0.043(2) 0.032(2) -0.0052(17) -0.0112(16) 0.0107(18) C24 0.036(2) 0.044(2) 0.029(2) -0.0107(17) -0.0071(16) 0.0118(18) C25 0.030(2) 0.040(2) 0.0203(18) -0.0050(15) -0.0037(15) 0.0059(17) C26 0.036(2) 0.036(2) 0.0210(19) -0.0010(15) 0.0010(16) 0.0033(17) N1 0.0262(16) 0.0325(17) 0.0260(16) -0.0012(13) -0.0052(12) 0.0011(13) N2 0.0224(15) 0.0270(15) 0.0205(14) -0.0027(12) -0.0043(11) -0.0004(12) N3 0.045(2) 0.0320(18) 0.0282(18) -0.0048(13) 0.0071(15) 0.0043(14) N4 0.0286(16) 0.0329(17) 0.0244(16) -0.0071(13) 0.0015(12) 0.0033(13) N5 0.0290(17) 0.0399(18) 0.0229(15) -0.0037(13) -0.0069(12) 0.0055(14) N6 0.0240(15) 0.0372(17) 0.0170(14) -0.0021(12) -0.0039(11) 0.0028(13) N7 0.0209(15) 0.0352(17) 0.0230(15) -0.0045(12) -0.0005(12) -0.0011(13) N8 0.0220(15) 0.0348(17) 0.0215(15) -0.0020(12) 0.0000(12) 0.0032(13) O1 0.0286(15) 0.0341(16) 0.063(2) -0.0027(14) -0.0045(13) 0.0117(12) O2 0.0337(15) 0.0548(19) 0.0375(16) 0.0098(13) -0.0148(12) 0.0036(13) O3 0.0374(16) 0.0532(17) 0.0221(13) 0.0008(12) 0.0046(11) 0.0110(14) O4 0.0368(17) 0.077(2) 0.0217(14) -0.0011(13) -0.0035(12) 0.0079(14) O5 0.0492(19) 0.067(2) 0.0446(18) -0.0245(16) -0.0056(15) -0.0018(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.283(3) . ? Cd1 N7 2.289(3) 4_556 ? Cd1 N1 2.331(3) . ? Cd1 N3 2.362(3) 6_556 ? Cd1 O1 2.441(3) 5_566 ? C1 C6 1.385(5) . ? C1 C2 1.385(5) . ? C1 C7 1.510(5) . ? C2 C3 1.380(5) . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 N2 1.429(4) . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.383(5) . ? C5 N4 1.437(4) . ? C6 H6 0.9300 . ? C7 O2 1.237(5) . ? C7 O1 1.255(5) . ? C8 C9 1.346(5) . ? C8 N2 1.373(4) . ? C8 H8 0.9300 . ? C9 N1 1.372(5) . ? C9 H9 0.9300 . ? C10 N1 1.320(4) . ? C10 N2 1.351(4) . ? C10 H10 0.9300 . ? C11 N4 1.345(5) . ? C11 C12 1.360(6) . ? C11 H11 0.9300 . ? C12 N3 1.367(6) . ? C12 H12 0.9300 . ? C13 N3 1.307(5) . ? C13 N4 1.352(5) . ? C13 H13 0.9300 . ? C14 C19 1.374(5) . ? C14 C15 1.384(5) . ? C14 C26 1.516(5) . ? C15 C16 1.379(5) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C16 N8 1.430(4) . ? C17 C18 1.391(5) . ? C17 H17 0.9300 . ? C18 C19 1.385(5) . ? C18 N6 1.417(4) . ? C19 H19 0.9300 . ? C20 C21 1.347(5) . ? C20 N8 1.379(4) . ? C20 H20 0.9300 . ? C21 N7 1.372(4) . ? C21 H21 0.9300 . ? C22 N7 1.316(5) . ? C22 N8 1.352(4) . ? C22 H22 0.9300 . ? C23 C24 1.351(5) . ? C23 N5 1.374(5) . ? C23 H23 0.9300 . ? C24 N6 1.374(5) . ? C24 H24 0.9300 . ? C25 N5 1.308(5) . ? C25 N6 1.348(4) . ? C25 H25 0.9300 . ? C26 O4 1.242(5) . ? C26 O3 1.269(5) . ? N3 Cd1 2.362(3) 6 ? N7 Cd1 2.289(3) 4_546 ? O1 Cd1 2.441(3) 5_566 ? O2 Cd1 2.638(3) 5_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cd1 N7 97.46(11) . 4_556 ? N5 Cd1 N1 146.96(11) . . ? N7 Cd1 N1 95.94(10) 4_556 . ? N5 Cd1 N3 85.32(12) . 6_556 ? N7 Cd1 N3 173.18(11) 4_556 6_556 ? N1 Cd1 N3 84.87(11) . 6_556 ? N5 Cd1 O1 133.56(10) . 5_566 ? N7 Cd1 O1 81.81(10) 4_556 5_566 ? N1 Cd1 O1 78.23(10) . 5_566 ? N3 Cd1 O1 91.76(11) 6_556 5_566 ? N5 Cd1 O2 82.42(10) . 5_566 ? N7 Cd1 O2 88.00(10) 4_556 5_566 ? N1 Cd1 O2 128.18(9) . 5_566 ? N3 Cd1 O2 86.20(10) 6_556 5_566 ? O1 Cd1 O2 51.16(9) 5_566 5_566 ? N5 Cd1 O3 78.13(10) . 6_565 ? N7 Cd1 O3 83.31(9) 4_556 6_565 ? N1 Cd1 O3 73.63(9) . 6_565 ? N3 Cd1 O3 103.39(10) 6_556 6_565 ? O1 Cd1 O3 146.46(9) 5_566 6_565 ? O2 Cd1 O3 157.42(9) 5_566 6_565 ? C6 C1 C2 119.7(3) . . ? C6 C1 C7 120.9(3) . . ? C2 C1 C7 119.4(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.6(3) . . ? C4 C3 N2 118.5(3) . . ? C2 C3 N2 120.8(3) . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 N4 117.7(3) . . ? C6 C5 N4 121.1(3) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? O2 C7 O1 124.0(4) . . ? O2 C7 C1 119.1(3) . . ? O1 C7 C1 116.9(3) . . ? C9 C8 N2 106.2(3) . . ? C9 C8 H8 126.9 . . ? N2 C8 H8 126.9 . . ? C8 C9 N1 110.4(3) . . ? C8 C9 H9 124.8 . . ? N1 C9 H9 124.8 . . ? N1 C10 N2 111.5(3) . . ? N1 C10 H10 124.2 . . ? N2 C10 H10 124.2 . . ? N4 C11 C12 105.9(4) . . ? N4 C11 H11 127.0 . . ? C12 C11 H11 127.0 . . ? C11 C12 N3 110.3(4) . . ? C11 C12 H12 124.9 . . ? N3 C12 H12 124.9 . . ? N3 C13 N4 111.8(4) . . ? N3 C13 H13 124.1 . . ? N4 C13 H13 124.1 . . ? C19 C14 C15 119.7(3) . . ? C19 C14 C26 120.5(3) . . ? C15 C14 C26 119.8(3) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 N8 118.5(3) . . ? C17 C16 N8 120.5(3) . . ? C16 C17 C18 118.4(3) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 120.6(3) . . ? C19 C18 N6 119.8(3) . . ? C17 C18 N6 119.6(3) . . ? C14 C19 C18 120.3(3) . . ? C14 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 N8 106.1(3) . . ? C21 C20 H20 126.9 . . ? N8 C20 H20 126.9 . . ? C20 C21 N7 110.1(3) . . ? C20 C21 H21 124.9 . . ? N7 C21 H21 124.9 . . ? N7 C22 N8 111.3(3) . . ? N7 C22 H22 124.3 . . ? N8 C22 H22 124.3 . . ? C24 C23 N5 109.8(3) . . ? C24 C23 H23 125.1 . . ? N5 C23 H23 125.1 . . ? C23 C24 N6 106.1(3) . . ? C23 C24 H24 127.0 . . ? N6 C24 H24 127.0 . . ? N5 C25 N6 111.6(3) . . ? N5 C25 H25 124.2 . . ? N6 C25 H25 124.2 . . ? O4 C26 O3 125.4(4) . . ? O4 C26 C14 118.7(4) . . ? O3 C26 C14 116.0(3) . . ? C10 N1 C9 105.1(3) . . ? C10 N1 Cd1 126.3(2) . . ? C9 N1 Cd1 127.9(2) . . ? C10 N2 C8 106.8(3) . . ? C10 N2 C3 126.9(3) . . ? C8 N2 C3 126.3(3) . . ? C13 N3 C12 104.8(3) . . ? C13 N3 Cd1 132.2(3) . 6 ? C12 N3 Cd1 122.2(3) . 6 ? C11 N4 C13 107.2(3) . . ? C11 N4 C5 126.7(3) . . ? C13 N4 C5 125.8(3) . . ? C25 N5 C23 105.7(3) . . ? C25 N5 Cd1 124.8(3) . . ? C23 N5 Cd1 125.8(2) . . ? C25 N6 C24 106.8(3) . . ? C25 N6 C18 125.8(3) . . ? C24 N6 C18 127.2(3) . . ? C22 N7 C21 105.7(3) . . ? C22 N7 Cd1 131.1(2) . 4_546 ? C21 N7 Cd1 123.0(2) . 4_546 ? C22 N8 C20 106.7(3) . . ? C22 N8 C16 128.1(3) . . ? C20 N8 C16 125.1(3) . . ? C7 O1 Cd1 96.8(2) . 5_566 ? C7 O2 Cd1 88.0(2) . 5_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.4(5) . . . . ? C7 C1 C2 C3 -176.4(3) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C1 C2 C3 N2 -179.1(3) . . . . ? C2 C3 C4 C5 -1.5(6) . . . . ? N2 C3 C4 C5 177.2(3) . . . . ? C3 C4 C5 C6 1.5(6) . . . . ? C3 C4 C5 N4 -179.4(3) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? N4 C5 C6 C1 -178.6(3) . . . . ? C2 C1 C6 C5 -2.4(5) . . . . ? C7 C1 C6 C5 176.5(3) . . . . ? C6 C1 C7 O2 -6.4(5) . . . . ? C2 C1 C7 O2 172.5(3) . . . . ? C6 C1 C7 O1 173.4(3) . . . . ? C2 C1 C7 O1 -7.7(5) . . . . ? N2 C8 C9 N1 0.0(4) . . . . ? N4 C11 C12 N3 -1.0(6) . . . . ? C19 C14 C15 C16 0.7(6) . . . . ? C26 C14 C15 C16 178.6(3) . . . . ? C14 C15 C16 C17 1.3(6) . . . . ? C14 C15 C16 N8 -178.0(3) . . . . ? C15 C16 C17 C18 -2.3(6) . . . . ? N8 C16 C17 C18 177.0(3) . . . . ? C16 C17 C18 C19 1.4(6) . . . . ? C16 C17 C18 N6 -176.1(3) . . . . ? C15 C14 C19 C18 -1.6(6) . . . . ? C26 C14 C19 C18 -179.5(3) . . . . ? C17 C18 C19 C14 0.5(6) . . . . ? N6 C18 C19 C14 178.0(3) . . . . ? N8 C20 C21 N7 -0.5(4) . . . . ? N5 C23 C24 N6 0.1(5) . . . . ? C19 C14 C26 O4 -161.1(4) . . . . ? C15 C14 C26 O4 21.0(5) . . . . ? C19 C14 C26 O3 18.9(5) . . . . ? C15 C14 C26 O3 -159.0(4) . . . . ? N2 C10 N1 C9 0.0(4) . . . . ? N2 C10 N1 Cd1 -170.5(2) . . . . ? C8 C9 N1 C10 0.0(4) . . . . ? C8 C9 N1 Cd1 170.3(3) . . . . ? N5 Cd1 N1 C10 175.4(3) . . . . ? N7 Cd1 N1 C10 -71.1(3) 4_556 . . . ? N3 Cd1 N1 C10 102.1(3) 6_556 . . . ? O1 Cd1 N1 C10 9.2(3) 5_566 . . . ? O2 Cd1 N1 C10 21.0(4) 5_566 . . . ? N5 Cd1 N1 C9 7.0(4) . . . . ? N7 Cd1 N1 C9 120.5(3) 4_556 . . . ? N3 Cd1 N1 C9 -66.3(3) 6_556 . . . ? O1 Cd1 N1 C9 -159.1(3) 5_566 . . . ? O2 Cd1 N1 C9 -147.3(3) 5_566 . . . ? N1 C10 N2 C8 0.0(4) . . . . ? N1 C10 N2 C3 179.2(3) . . . . ? C9 C8 N2 C10 0.0(4) . . . . ? C9 C8 N2 C3 -179.2(3) . . . . ? C4 C3 N2 C10 157.8(4) . . . . ? C2 C3 N2 C10 -23.6(5) . . . . ? C4 C3 N2 C8 -23.3(5) . . . . ? C2 C3 N2 C8 155.4(4) . . . . ? N4 C13 N3 C12 -1.9(5) . . . . ? N4 C13 N3 Cd1 167.5(3) . . . 6 ? C11 C12 N3 C13 1.8(6) . . . . ? C11 C12 N3 Cd1 -168.9(4) . . . 6 ? C12 C11 N4 C13 -0.2(6) . . . . ? C12 C11 N4 C5 -174.9(4) . . . . ? N3 C13 N4 C11 1.4(5) . . . . ? N3 C13 N4 C5 176.2(3) . . . . ? C4 C5 N4 C11 108.7(5) . . . . ? C6 C5 N4 C11 -72.2(6) . . . . ? C4 C5 N4 C13 -65.0(5) . . . . ? C6 C5 N4 C13 114.0(4) . . . . ? N6 C25 N5 C23 0.0(5) . . . . ? N6 C25 N5 Cd1 -159.3(2) . . . . ? C24 C23 N5 C25 -0.1(5) . . . . ? C24 C23 N5 Cd1 158.9(3) . . . . ? N7 Cd1 N5 C25 -101.4(3) 4_556 . . . ? N1 Cd1 N5 C25 11.7(4) . . . . ? N3 Cd1 N5 C25 84.9(3) 6_556 . . . ? O1 Cd1 N5 C25 172.8(3) 5_566 . . . ? O2 Cd1 N5 C25 171.6(3) 5_566 . . . ? N7 Cd1 N5 C23 103.4(3) 4_556 . . . ? N1 Cd1 N5 C23 -143.4(3) . . . . ? N3 Cd1 N5 C23 -70.3(3) 6_556 . . . ? O1 Cd1 N5 C23 17.7(4) 5_566 . . . ? O2 Cd1 N5 C23 16.5(3) 5_566 . . . ? N5 C25 N6 C24 0.1(5) . . . . ? N5 C25 N6 C18 175.1(3) . . . . ? C23 C24 N6 C25 -0.2(5) . . . . ? C23 C24 N6 C18 -175.1(4) . . . . ? C19 C18 N6 C25 -154.2(4) . . . . ? C17 C18 N6 C25 23.3(6) . . . . ? C19 C18 N6 C24 19.8(6) . . . . ? C17 C18 N6 C24 -162.7(4) . . . . ? N8 C22 N7 C21 0.1(4) . . . . ? N8 C22 N7 Cd1 174.3(2) . . . 4_546 ? C20 C21 N7 C22 0.2(4) . . . . ? C20 C21 N7 Cd1 -174.6(2) . . . 4_546 ? N7 C22 N8 C20 -0.4(4) . . . . ? N7 C22 N8 C16 -176.4(3) . . . . ? C21 C20 N8 C22 0.6(4) . . . . ? C21 C20 N8 C16 176.6(3) . . . . ? C15 C16 N8 C22 173.1(4) . . . . ? C17 C16 N8 C22 -6.1(6) . . . . ? C15 C16 N8 C20 -2.1(5) . . . . ? C17 C16 N8 C20 178.6(4) . . . . ? O2 C7 O1 Cd1 1.6(4) . . . 5_566 ? C1 C7 O1 Cd1 -178.2(3) . . . 5_566 ? O1 C7 O2 Cd1 -1.4(4) . . . 5_566 ? C1 C7 O2 Cd1 178.3(3) . . . 5_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.922 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.098 #====END