# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _publ_contact_author_name 'Prof Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; _publ_contact_author_email Zhangjie@fjirsm.ac.cn _publ_author_name 'Jie Zhang' data_Cd(ClO4) _database_code_depnum_ccdc_archive 'CCDC 863618' #TrackingRef 'Cif-1-5-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H54 Cd Cl2 N4 O23' _chemical_formula_sum 'C52 H54 Cd Cl2 N4 O23' _chemical_formula_weight 1286.29 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' Cl Cl 0.1484 0.1585 '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 Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y+1/2, -z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' 'x+1/2, -y+1, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y-1/2, z-1/2' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' '-x+1/2, y, z-1/2' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.348(18) _cell_length_b 31.17(3) _cell_length_c 9.522(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5743(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6393 _cell_measurement_theta_min 3.2736 _cell_measurement_theta_max 27.4758 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1980 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 20766 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3261 _reflns_number_gt 2252 _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^)+(0.0750P)^2^+16.0000P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3261 _refine_ls_number_parameters 232 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.7500 0.2500 0.0523(3) Uani 1 4 d S . . Cl1 Cl 0.2500 0.5000 0.7573(10) 0.257(4) Uani 1 2 d SD . . O1 O 0.4124(2) 0.75008(12) 0.4549(7) 0.1067(17) Uani 1 1 d . . . O1W O 0.4724(8) 0.7500 0.7500 0.212(9) Uani 1 2 d SU . . O2 O 0.43886(18) 0.69174(13) 0.3421(4) 0.0816(11) Uani 1 1 d U . . O2W O 0.0650(9) 0.5352(4) 0.932(2) 0.314(9) Uani 0.75 1 d PU . . O3 O 0.2564(11) 0.5444(4) 0.814(3) 0.217(7) Uani 0.50 1 d PDU A 1 O3B O 0.2551(18) 0.5215(8) 0.6150(18) 0.234(9) Uani 0.25 1 d PDU . 2 O3W O 0.0000 0.5999(5) 0.7500 0.178(7) Uani 0.713(14) 2 d SPU . . O4 O 0.3158(10) 0.4958(8) 0.668(3) 0.252(8) Uani 0.50 1 d PDU A 1 O4B O 0.3223(9) 0.4916(12) 0.813(4) 0.232(9) Uani 0.25 1 d PDU . 2 O4W O 0.0000 0.5425(5) 0.7500 0.142(11) Uani 0.287(14) 2 d SPU . . O5B O 0.2118(18) 0.5289(8) 0.858(3) 0.233(9) Uani 0.25 1 d PDU . 2 O6B O 0.2119(18) 0.4579(7) 0.743(3) 0.230(9) Uani 0.25 1 d PDU . 2 N1 N 0.11890(19) 0.61890(12) 0.5263(4) 0.0594(9) Uani 1 1 d . . . C1 C 0.4041(2) 0.71120(17) 0.4309(6) 0.0642(12) Uani 1 1 d . . . C2 C 0.3487(2) 0.68695(15) 0.5092(5) 0.0572(10) Uani 1 1 d . . . C3 C 0.2968(3) 0.70863(16) 0.5797(6) 0.0728(14) Uani 1 1 d . . . H3 H 0.3008 0.7380 0.5940 0.087 Uiso 1 1 calc R . . C4 C 0.3455(2) 0.64249(15) 0.5016(5) 0.0591(11) Uani 1 1 d . . . H4 H 0.3821 0.6273 0.4626 0.071 Uiso 1 1 calc R . . C5 C 0.2394(3) 0.68731(17) 0.6292(6) 0.0761(15) Uani 1 1 d . . . H5 H 0.2044 0.7024 0.6743 0.091 Uiso 1 1 calc R . . C6 C 0.2886(2) 0.62073(15) 0.5513(5) 0.0626(11) Uani 1 1 d . . . H6 H 0.2869 0.5910 0.5445 0.075 Uiso 1 1 calc R . . C7 C 0.2339(2) 0.64277(16) 0.6112(5) 0.0607(11) Uani 1 1 d . . . C8 C 0.1677(3) 0.61925(18) 0.6495(5) 0.0718(13) Uani 1 1 d . . . H8B H 0.1785 0.5900 0.6766 0.086 Uiso 1 1 calc R . . H8A H 0.1458 0.6333 0.7287 0.086 Uiso 1 1 calc R . . C9 C 0.0830(3) 0.65385(19) 0.4972(7) 0.0907(18) Uani 1 1 d . . . H9 H 0.0893 0.6785 0.5510 0.109 Uiso 1 1 calc R . . C10 C 0.1108(3) 0.58470(17) 0.4489(7) 0.0905(19) Uani 1 1 d . . . H10 H 0.1375 0.5605 0.4676 0.109 Uiso 1 1 calc R . . C11 C 0.0372(4) 0.65411(18) 0.3896(7) 0.0935(19) Uani 1 1 d . . . H11 H 0.0127 0.6791 0.3703 0.112 Uiso 1 1 calc R . . C12 C 0.0642(3) 0.58350(15) 0.3408(7) 0.093(2) Uani 1 1 d . . . H12 H 0.0587 0.5584 0.2892 0.111 Uiso 1 1 calc R . . C13 C 0.0259(2) 0.61847(13) 0.3084(5) 0.0572(10) 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 0.0426(4) 0.0458(4) 0.0684(5) 0.000 0.000 0.000 Cl1 0.296(9) 0.091(3) 0.384(12) 0.000 0.000 -0.002(4) O1 0.083(3) 0.067(2) 0.170(5) -0.001(2) 0.043(3) -0.020(2) O1W 0.25(2) 0.135(8) 0.246(13) -0.023(9) 0.000 0.000 O2 0.069(2) 0.095(3) 0.081(3) -0.007(2) 0.0214(19) -0.020(2) O2W 0.301(16) 0.185(12) 0.46(2) -0.107(14) 0.088(18) -0.036(12) O3 0.221(16) 0.168(12) 0.262(16) 0.009(13) 0.062(13) -0.006(12) O3B 0.249(17) 0.173(14) 0.281(17) 0.055(14) 0.055(15) 0.001(14) O3W 0.142(10) 0.147(12) 0.245(15) 0.000 0.113(10) 0.000 O4 0.215(15) 0.214(14) 0.327(18) -0.013(15) 0.127(14) 0.032(13) O4B 0.237(17) 0.172(15) 0.288(18) 0.033(14) 0.043(15) 0.008(14) O4W 0.165(18) 0.022(7) 0.24(2) 0.000 0.174(17) 0.000 O5B 0.247(18) 0.163(15) 0.288(18) 0.008(14) 0.052(16) 0.018(14) O6B 0.244(17) 0.167(14) 0.279(18) 0.045(14) 0.055(15) 0.008(14) N1 0.058(2) 0.056(2) 0.065(2) -0.0017(18) 0.0089(17) -0.0117(17) C1 0.046(2) 0.072(3) 0.074(3) 0.005(3) 0.000(2) -0.007(2) C2 0.050(2) 0.065(3) 0.056(2) 0.000(2) 0.0011(19) -0.008(2) C3 0.070(3) 0.056(3) 0.092(4) -0.012(3) 0.017(3) -0.010(2) C4 0.056(2) 0.062(3) 0.059(3) -0.001(2) 0.004(2) 0.004(2) C5 0.067(3) 0.071(3) 0.090(4) -0.014(3) 0.025(3) -0.006(3) C6 0.068(3) 0.055(2) 0.065(3) 0.005(2) 0.001(2) -0.004(2) C7 0.057(3) 0.073(3) 0.052(2) 0.002(2) 0.004(2) -0.012(2) C8 0.068(3) 0.081(3) 0.067(3) 0.010(3) 0.007(2) -0.017(3) C9 0.108(5) 0.065(3) 0.099(4) -0.028(3) -0.025(4) 0.014(3) C10 0.102(4) 0.053(3) 0.116(5) -0.010(3) -0.032(4) 0.014(3) C11 0.106(5) 0.058(3) 0.117(5) -0.027(3) -0.029(4) 0.025(3) C12 0.112(5) 0.045(3) 0.121(5) -0.022(3) -0.041(4) 0.008(3) C13 0.058(2) 0.043(2) 0.071(3) 0.002(2) 0.011(2) -0.0019(19) _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 2.338(4) 2_665 ? Cd1 O2 2.338(4) . ? Cd1 O2 2.338(4) 3_565 ? Cd1 O2 2.338(4) 4_655 ? Cd1 O1 2.585(5) 3_565 ? Cd1 O1 2.585(5) 2_665 ? Cd1 O1 2.585(5) 4_655 ? Cd1 O1 2.585(5) . ? Cl1 O3 1.491(10) 6 ? Cl1 O3 1.491(10) . ? Cl1 O6B 1.510(12) . ? Cl1 O6B 1.510(12) 6 ? Cl1 O5B 1.512(11) . ? Cl1 O5B 1.512(11) 6 ? Cl1 O3B 1.515(11) 6 ? Cl1 O3B 1.515(11) . ? Cl1 O4B 1.520(12) . ? Cl1 O4B 1.520(11) 6 ? Cl1 O4 1.535(10) 6 ? Cl1 O4 1.535(10) . ? O1 C1 1.244(6) . ? O1W O1W 1.07(3) 2_665 ? O2 C1 1.239(6) . ? O3B O3B 1.36(5) 6 ? O3B O6B 1.52(4) 6 ? O3W O4W 1.79(2) . ? O4B O5B 1.01(4) 6 ? O5B O4B 1.01(4) 6 ? O6B O3B 1.52(4) 6 ? N1 C10 1.305(6) . ? N1 C9 1.321(7) . ? N1 C8 1.506(6) . ? C1 C2 1.508(6) . ? C2 C3 1.384(7) . ? C2 C4 1.389(6) . ? C3 C5 1.378(7) . ? C3 H3 0.9300 . ? C4 C6 1.376(6) . ? C4 H4 0.9300 . ? C5 C7 1.403(7) . ? C5 H5 0.9300 . ? C6 C7 1.385(7) . ? C6 H6 0.9300 . ? C7 C8 1.521(6) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 C11 1.356(8) . ? C9 H9 0.9300 . ? C10 C12 1.370(8) . ? C10 H10 0.9300 . ? C11 C13 1.371(7) . ? C11 H11 0.9300 . ? C12 C13 1.353(7) . ? C12 H12 0.9300 . ? C13 C13 1.498(10) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 135.95(19) 2_665 . ? O2 Cd1 O2 78.1(2) 2_665 3_565 ? O2 Cd1 O2 119.2(2) . 3_565 ? O2 Cd1 O2 119.2(2) 2_665 4_655 ? O2 Cd1 O2 78.1(2) . 4_655 ? O2 Cd1 O2 135.95(19) 3_565 4_655 ? O2 Cd1 O1 128.00(13) 2_665 3_565 ? O2 Cd1 O1 87.16(16) . 3_565 ? O2 Cd1 O1 52.11(13) 3_565 3_565 ? O2 Cd1 O1 92.76(15) 4_655 3_565 ? O2 Cd1 O1 52.11(13) 2_665 2_665 ? O2 Cd1 O1 92.76(15) . 2_665 ? O2 Cd1 O1 128.00(13) 3_565 2_665 ? O2 Cd1 O1 87.16(16) 4_655 2_665 ? O1 Cd1 O1 179.89(17) 3_565 2_665 ? O2 Cd1 O1 87.16(16) 2_665 4_655 ? O2 Cd1 O1 128.00(13) . 4_655 ? O2 Cd1 O1 92.76(15) 3_565 4_655 ? O2 Cd1 O1 52.11(13) 4_655 4_655 ? O1 Cd1 O1 82.0(3) 3_565 4_655 ? O1 Cd1 O1 98.0(3) 2_665 4_655 ? O2 Cd1 O1 92.76(15) 2_665 . ? O2 Cd1 O1 52.11(13) . . ? O2 Cd1 O1 87.16(16) 3_565 . ? O2 Cd1 O1 128.00(13) 4_655 . ? O1 Cd1 O1 98.0(3) 3_565 . ? O1 Cd1 O1 82.0(3) 2_665 . ? O1 Cd1 O1 179.89(17) 4_655 . ? O3 Cl1 O3 137(2) 6 . ? O3 Cl1 O6B 35.5(13) 6 . ? O3 Cl1 O6B 151.5(14) . . ? O3 Cl1 O6B 151.5(14) 6 6 ? O3 Cl1 O6B 35.5(13) . 6 ? O6B Cl1 O6B 169.9(19) . 6 ? O3 Cl1 O5B 106.3(18) 6 . ? O3 Cl1 O5B 41.9(13) . . ? O6B Cl1 O5B 109.6(6) . . ? O6B Cl1 O5B 77.1(13) 6 . ? O3 Cl1 O5B 41.9(13) 6 6 ? O3 Cl1 O5B 106.3(18) . 6 ? O6B Cl1 O5B 77.1(13) . 6 ? O6B Cl1 O5B 109.6(6) 6 6 ? O5B Cl1 O5B 101(3) . 6 ? O3 Cl1 O3B 84.8(13) 6 6 ? O3 Cl1 O3B 137.8(16) . 6 ? O6B Cl1 O3B 60.3(18) . 6 ? O6B Cl1 O3B 109.7(6) 6 6 ? O5B Cl1 O3B 143(3) . 6 ? O5B Cl1 O3B 109.7(6) 6 6 ? O3 Cl1 O3B 137.8(16) 6 . ? O3 Cl1 O3B 84.8(13) . . ? O6B Cl1 O3B 109.7(6) . . ? O6B Cl1 O3B 60.3(18) 6 . ? O5B Cl1 O3B 109.7(6) . . ? O5B Cl1 O3B 143(3) 6 . ? O3B Cl1 O3B 53(2) 6 . ? O3 Cl1 O4B 77.8(14) 6 . ? O3 Cl1 O4B 87.4(19) . . ? O6B Cl1 O4B 109.2(6) . . ? O6B Cl1 O4B 74.5(9) 6 . ? O5B Cl1 O4B 109.2(6) . . ? O5B Cl1 O4B 39.0(17) 6 . ? O3B Cl1 O4B 107(3) 6 . ? O3B Cl1 O4B 109.3(6) . . ? O3 Cl1 O4B 87.4(19) 6 6 ? O3 Cl1 O4B 77.8(14) . 6 ? O6B Cl1 O4B 74.5(9) . 6 ? O6B Cl1 O4B 109.2(6) 6 6 ? O5B Cl1 O4B 39.0(17) . 6 ? O5B Cl1 O4B 109.2(6) 6 6 ? O3B Cl1 O4B 109.3(6) 6 6 ? O3B Cl1 O4B 107(3) . 6 ? O4B Cl1 O4B 139(3) . 6 ? O3 Cl1 O4 102.2(11) 6 6 ? O3 Cl1 O4 101.1(13) . 6 ? O6B Cl1 O4 67.7(14) . 6 ? O6B Cl1 O4 106.4(16) 6 6 ? O5B Cl1 O4 84(2) . 6 ? O5B Cl1 O4 143.9(16) 6 6 ? O3B Cl1 O4 59.3(14) 6 6 ? O3B Cl1 O4 61.4(17) . 6 ? O4B Cl1 O4 166(2) . 6 ? O4B Cl1 O4 54.4(16) 6 6 ? O3 Cl1 O4 101.1(13) 6 . ? O3 Cl1 O4 102.2(11) . . ? O6B Cl1 O4 106.4(16) . . ? O6B Cl1 O4 67.7(14) 6 . ? O5B Cl1 O4 143.9(16) . . ? O5B Cl1 O4 84(2) 6 . ? O3B Cl1 O4 61.4(17) 6 . ? O3B Cl1 O4 59.3(14) . . ? O4B Cl1 O4 54.4(16) . . ? O4B Cl1 O4 166(2) 6 . ? O4 Cl1 O4 113(2) 6 . ? C1 O1 Cd1 86.8(4) . . ? C1 O2 Cd1 98.7(3) . . ? O3B O3B Cl1 63.4(10) 6 . ? O3B O3B O6B 118.6(17) 6 6 ? Cl1 O3B O6B 59.7(9) . 6 ? O5B O4B Cl1 70.0(10) 6 . ? O4B O5B Cl1 70.9(10) 6 . ? Cl1 O6B O3B 60.0(10) . 6 ? C10 N1 C9 119.5(5) . . ? C10 N1 C8 121.4(5) . . ? C9 N1 C8 119.1(4) . . ? O2 C1 O1 122.2(5) . . ? O2 C1 C2 118.5(5) . . ? O1 C1 C2 119.3(5) . . ? C3 C2 C4 118.7(4) . . ? C3 C2 C1 120.7(4) . . ? C4 C2 C1 120.4(4) . . ? C5 C3 C2 121.0(5) . . ? C5 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C6 C4 C2 120.7(4) . . ? C6 C4 H4 119.7 . . ? C2 C4 H4 119.7 . . ? C3 C5 C7 119.8(5) . . ? C3 C5 H5 120.1 . . ? C7 C5 H5 120.1 . . ? C4 C6 C7 120.5(4) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C5 118.9(4) . . ? C6 C7 C8 120.2(5) . . ? C5 C7 C8 120.8(5) . . ? N1 C8 C7 110.2(4) . . ? N1 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? N1 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? H8B C8 H8A 108.1 . . ? N1 C9 C11 120.5(5) . . ? N1 C9 H9 119.8 . . ? C11 C9 H9 119.8 . . ? N1 C10 C12 121.7(5) . . ? N1 C10 H10 119.2 . . ? C12 C10 H10 119.2 . . ? C9 C11 C13 121.7(5) . . ? C9 C11 H11 119.2 . . ? C13 C11 H11 119.2 . . ? C13 C12 C10 120.7(5) . . ? C13 C12 H12 119.7 . . ? C10 C12 H12 119.7 . . ? C12 C13 C11 115.9(5) . . ? C12 C13 C13 122.4(4) . 4 ? C11 C13 C13 121.7(4) . 4 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.945 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.098 #===END data_CdCl2 _database_code_depnum_ccdc_archive 'CCDC 863619' #TrackingRef 'Cif-1-5-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H29 Cd Cl2 N2 O8.50' _chemical_formula_sum 'C26 H29 Cd Cl2 N2 O8.50' _chemical_formula_weight 688.81 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.1787(12) _cell_length_b 9.8431(5) _cell_length_c 18.6902(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.982(2) _cell_angle_gamma 90.00 _cell_volume 2697.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5077 _cell_measurement_theta_min 2.0696 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour 'yellowish white' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7799 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Rigaku Mercury' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 20174 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6180 _reflns_number_gt 5052 _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^)+(0.1060P)^2^+3.3436P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6180 _refine_ls_number_parameters 356 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.092 _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 0.79575(2) 0.74700(3) 0.026307(18) 0.04703(16) Uani 1 1 d . . . Cl1 Cl 0.87422(13) 0.9054(2) -0.02827(10) 0.1017(6) Uani 1 1 d . . . Cl2 Cl 0.72247(11) 0.90694(19) 0.08627(9) 0.0820(5) Uani 1 1 d . . . O1 O 0.6624(2) 0.7105(4) -0.0994(2) 0.0661(10) Uani 1 1 d . . . O1W O 0.7886(5) 1.3355(7) -0.0438(3) 0.146(3) Uani 1 1 d . . . O2 O 0.6879(2) 0.5756(4) 0.0002(2) 0.0707(11) Uani 1 1 d . . . O2W O 0.9405(9) 1.2128(12) -0.0237(6) 0.220(6) Uani 1 1 d . . . O3 O -0.5967(2) 0.9299(4) -0.4543(2) 0.0676(10) Uani 1 1 d . . . O3W O 0.6613(7) 1.1514(9) -0.0436(5) 0.188(4) Uani 1 1 d . . . O4 O -0.5805(2) 0.8136(4) -0.3493(2) 0.0621(9) Uani 1 1 d . . . O4W O 0.4811(9) 1.0942(12) 0.0505(8) 0.190(8) Uani 0.50 1 d PD . . O5W O 0.6297(11) 1.2186(14) 0.0794(11) 0.288(8) Uiso 1 1 d D . . N1 N 0.2023(2) 0.5094(3) -0.2192(2) 0.0401(7) Uani 1 1 d . . . N2 N -0.1182(2) 0.9918(3) -0.2217(2) 0.0403(7) Uani 1 1 d . . . C1 C 0.6384(3) 0.6181(5) -0.0669(3) 0.0461(9) Uani 1 1 d . . . C2 C 0.5430(3) 0.5596(4) -0.1089(2) 0.0399(8) Uani 1 1 d . . . C3 C 0.4799(3) 0.6173(5) -0.1776(2) 0.0456(9) Uani 1 1 d . . . H3 H 0.4973 0.6918 -0.2006 0.055 Uiso 1 1 calc R . . C4 C 0.5172(3) 0.4483(4) -0.0776(2) 0.0442(9) Uani 1 1 d . . . H4 H 0.5606 0.4056 -0.0315 0.053 Uiso 1 1 calc R . . C5 C 0.3920(3) 0.5680(5) -0.2132(3) 0.0501(10) Uani 1 1 d . . . H5 H 0.3493 0.6084 -0.2606 0.060 Uiso 1 1 calc R . . C6 C 0.4293(3) 0.3989(4) -0.1127(2) 0.0432(9) Uani 1 1 d . . . H6 H 0.4125 0.3231 -0.0904 0.052 Uiso 1 1 calc R . . C7 C 0.3658(3) 0.4591(4) -0.1800(2) 0.0398(8) Uani 1 1 d . . . C8 C 0.2695(3) 0.4053(5) -0.2184(3) 0.0511(10) Uani 1 1 d . . . H8A H 0.2553 0.3775 -0.2733 0.061 Uiso 1 1 calc R . . H8B H 0.2644 0.3241 -0.1893 0.061 Uiso 1 1 calc R . . C9 C 0.2186(3) 0.5825(5) -0.1543(3) 0.0506(10) Uani 1 1 d . . . H9 H 0.2738 0.5696 -0.1084 0.061 Uiso 1 1 calc R . . C10 C 0.1236(3) 0.5251(4) -0.2847(3) 0.0439(9) Uani 1 1 d . . . H10 H 0.1128 0.4715 -0.3301 0.053 Uiso 1 1 calc R . . C11 C 0.1556(3) 0.6765(5) -0.1537(2) 0.0479(10) Uani 1 1 d . . . H11 H 0.1675 0.7269 -0.1070 0.057 Uiso 1 1 calc R . . C12 C 0.0593(2) 0.6174(4) -0.2865(2) 0.0408(8) Uani 1 1 d . . . H12 H 0.0039 0.6265 -0.3327 0.049 Uiso 1 1 calc R . . C13 C 0.0751(3) 0.6982(4) -0.2203(2) 0.0375(8) Uani 1 1 d . . . C14 C 0.0077(3) 0.8018(4) -0.2210(2) 0.0375(8) Uani 1 1 d . . . C15 C 0.0310(3) 0.9034(5) -0.1644(3) 0.0565(12) Uani 1 1 d . . . H15 H 0.0916 0.9089 -0.1245 0.068 Uiso 1 1 calc R . . C16 C -0.0806(3) 0.8008(5) -0.2787(2) 0.0423(9) Uani 1 1 d . . . H16 H -0.0990 0.7334 -0.3188 0.051 Uiso 1 1 calc R . . C17 C -0.0329(3) 0.9957(5) -0.1657(3) 0.0568(12) Uani 1 1 d . . . H17 H -0.0162 1.0639 -0.1261 0.068 Uiso 1 1 calc R . . C18 C -0.1427(3) 0.8970(4) -0.2784(3) 0.0448(9) Uani 1 1 d . . . H18 H -0.2032 0.8960 -0.3187 0.054 Uiso 1 1 calc R . . C19 C -0.1831(3) 1.1010(5) -0.2225(3) 0.0557(12) Uani 1 1 d . . . H19A H -0.1748 1.1815 -0.2505 0.067 Uiso 1 1 calc R . . H19B H -0.1687 1.1283 -0.1675 0.067 Uiso 1 1 calc R . . C20 C -0.2810(3) 1.0554(4) -0.2620(2) 0.0407(8) Uani 1 1 d . . . C21 C -0.3349(3) 1.0932(5) -0.3389(3) 0.0495(10) Uani 1 1 d . . . H21 H -0.3110 1.1524 -0.3657 0.059 Uiso 1 1 calc R . . C22 C -0.3176(3) 0.9737(4) -0.2212(2) 0.0426(9) Uani 1 1 d . . . H22 H -0.2821 0.9508 -0.1674 0.051 Uiso 1 1 calc R . . C23 C -0.4231(3) 1.0456(5) -0.3773(3) 0.0482(10) Uani 1 1 d . . . H23 H -0.4595 1.0718 -0.4304 0.058 Uiso 1 1 calc R . . C24 C -0.4060(3) 0.9267(4) -0.2600(2) 0.0414(8) Uani 1 1 d . . . H24 H -0.4311 0.8710 -0.2326 0.050 Uiso 1 1 calc R . . C25 C -0.4588(3) 0.9601(4) -0.3389(2) 0.0383(8) Uani 1 1 d . . . C26 C -0.5516(3) 0.8972(5) -0.3829(3) 0.0445(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0351(2) 0.0587(3) 0.0407(2) 0.00182(13) 0.00965(15) -0.00333(12) Cl1 0.0907(11) 0.1334(16) 0.0652(9) 0.0097(10) 0.0174(8) -0.0482(11) Cl2 0.0756(9) 0.1037(12) 0.0589(8) -0.0014(7) 0.0207(7) 0.0307(8) O1 0.0442(18) 0.086(2) 0.059(2) 0.009(2) 0.0124(16) -0.0169(18) O1W 0.225(8) 0.112(5) 0.081(4) 0.001(3) 0.045(4) -0.008(5) O2 0.0432(17) 0.082(3) 0.062(2) 0.0168(19) -0.0021(16) -0.0088(17) O2W 0.284(14) 0.234(10) 0.145(8) -0.029(7) 0.092(9) -0.086(10) O3 0.0498(18) 0.092(3) 0.0494(19) 0.0047(18) 0.0094(15) -0.0055(18) O3W 0.248(9) 0.166(8) 0.124(6) 0.057(5) 0.054(6) 0.044(7) O4 0.0485(18) 0.072(2) 0.056(2) 0.0038(18) 0.0121(15) -0.0166(17) O4W 0.200(14) 0.115(9) 0.121(9) -0.014(8) -0.061(10) 0.074(10) N1 0.0312(15) 0.0429(18) 0.0448(18) 0.0035(14) 0.0145(13) -0.0030(13) N2 0.0333(15) 0.0405(17) 0.0475(18) -0.0045(14) 0.0174(14) -0.0054(13) C1 0.0366(19) 0.053(2) 0.046(2) -0.0016(19) 0.0152(18) 0.0020(18) C2 0.0337(18) 0.046(2) 0.039(2) -0.0008(16) 0.0143(15) 0.0007(16) C3 0.040(2) 0.052(2) 0.041(2) 0.0065(18) 0.0135(17) -0.0041(18) C4 0.040(2) 0.049(2) 0.041(2) 0.0049(17) 0.0140(17) 0.0059(17) C5 0.038(2) 0.057(3) 0.045(2) 0.016(2) 0.0075(17) 0.0061(19) C6 0.043(2) 0.043(2) 0.045(2) 0.0041(17) 0.0206(17) 0.0024(17) C7 0.0323(17) 0.041(2) 0.044(2) -0.0019(16) 0.0146(16) 0.0010(15) C8 0.035(2) 0.045(2) 0.065(3) -0.003(2) 0.0139(19) 0.0005(17) C9 0.046(2) 0.063(3) 0.037(2) 0.0048(19) 0.0125(18) 0.007(2) C10 0.0368(19) 0.048(2) 0.045(2) -0.0054(18) 0.0152(17) -0.0049(17) C11 0.042(2) 0.064(3) 0.034(2) -0.0030(19) 0.0124(17) 0.005(2) C12 0.0289(17) 0.053(2) 0.0364(19) -0.0041(17) 0.0093(15) -0.0027(16) C13 0.0297(17) 0.046(2) 0.0391(19) 0.0042(17) 0.0168(15) -0.0027(16) C14 0.0327(18) 0.046(2) 0.0360(19) 0.0009(16) 0.0170(15) -0.0034(16) C15 0.034(2) 0.073(3) 0.052(3) -0.018(2) 0.0084(18) -0.001(2) C16 0.0326(18) 0.045(2) 0.045(2) -0.0083(18) 0.0130(16) -0.0023(17) C17 0.041(2) 0.067(3) 0.056(3) -0.027(2) 0.015(2) -0.006(2) C18 0.0353(19) 0.048(2) 0.047(2) -0.0081(18) 0.0135(17) -0.0053(17) C19 0.041(2) 0.046(2) 0.078(3) -0.017(2) 0.023(2) -0.0050(18) C20 0.0384(19) 0.0344(19) 0.050(2) -0.0048(16) 0.0198(17) 0.0035(16) C21 0.056(2) 0.048(2) 0.055(3) 0.0056(19) 0.034(2) -0.0016(19) C22 0.041(2) 0.039(2) 0.043(2) 0.0025(16) 0.0126(17) 0.0022(16) C23 0.050(2) 0.056(3) 0.038(2) 0.0060(18) 0.0187(18) 0.0037(19) C24 0.0391(19) 0.041(2) 0.047(2) 0.0023(17) 0.0207(17) 0.0027(16) C25 0.0357(18) 0.039(2) 0.041(2) -0.0020(16) 0.0168(16) 0.0037(15) C26 0.0358(19) 0.050(2) 0.046(2) -0.0083(18) 0.0152(17) 0.0077(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 O2 2.325(4) . ? Cd1 O3 2.379(4) 4_776 ? Cd1 O4 2.417(3) 4_776 ? Cd1 O1 2.454(4) . ? Cd1 Cl1 2.4854(17) . ? Cd1 Cl2 2.5026(15) . ? Cd1 C1 2.717(4) . ? Cd1 C26 2.730(4) 4_776 ? O1 C1 1.243(6) . ? O2 C1 1.241(5) . ? O3 C26 1.263(5) . ? O3 Cd1 2.379(4) 4_475 ? O4 C26 1.240(6) . ? O4 Cd1 2.417(3) 4_475 ? N1 C9 1.338(6) . ? N1 C10 1.351(5) . ? N1 C8 1.490(5) . ? N2 C17 1.335(5) . ? N2 C18 1.339(5) . ? N2 C19 1.499(5) . ? C1 C2 1.519(5) . ? C2 C3 1.381(6) . ? C2 C4 1.386(6) . ? C3 C5 1.379(6) . ? C3 H3 0.9500 . ? C4 C6 1.379(6) . ? C4 H4 0.9500 . ? C5 C7 1.391(6) . ? C5 H5 0.9500 . ? C6 C7 1.377(6) . ? C6 H6 0.9500 . ? C7 C8 1.510(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.381(6) . ? C9 H9 0.9500 . ? C10 C12 1.372(6) . ? C10 H10 0.9500 . ? C11 C13 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.401(6) . ? C12 H12 0.9500 . ? C13 C14 1.488(6) . ? C14 C16 1.380(5) . ? C14 C15 1.388(6) . ? C15 C17 1.368(7) . ? C15 H15 0.9500 . ? C16 C18 1.382(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.506(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.381(6) . ? C20 C22 1.401(6) . ? C21 C23 1.382(6) . ? C21 H21 0.9500 . ? C22 C24 1.381(6) . ? C22 H22 0.9500 . ? C23 C25 1.380(6) . ? C23 H23 0.9500 . ? C24 C25 1.396(6) . ? C24 H24 0.9500 . ? C25 C26 1.508(6) . ? C26 Cd1 2.730(4) 4_475 ? 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 O3 86.34(15) . 4_776 ? O2 Cd1 O4 105.44(13) . 4_776 ? O3 Cd1 O4 54.36(12) 4_776 4_776 ? O2 Cd1 O1 54.15(12) . . ? O3 Cd1 O1 109.24(14) 4_776 . ? O4 Cd1 O1 157.12(15) 4_776 . ? O2 Cd1 Cl1 146.79(11) . . ? O3 Cd1 Cl1 93.12(12) 4_776 . ? O4 Cd1 Cl1 100.99(11) 4_776 . ? O1 Cd1 Cl1 95.39(9) . . ? O2 Cd1 Cl2 95.47(12) . . ? O3 Cd1 Cl2 147.85(9) 4_776 . ? O4 Cd1 Cl2 94.64(9) 4_776 . ? O1 Cd1 Cl2 97.43(11) . . ? Cl1 Cd1 Cl2 102.12(8) . . ? O2 Cd1 C1 27.10(13) . . ? O3 Cd1 C1 100.53(13) 4_776 . ? O4 Cd1 C1 132.31(14) 4_776 . ? O1 Cd1 C1 27.21(12) . . ? Cl1 Cd1 C1 122.18(10) . . ? Cl2 Cd1 C1 95.05(10) . . ? O2 Cd1 C26 98.90(12) . 4_776 ? O3 Cd1 C26 27.55(13) 4_776 4_776 ? O4 Cd1 C26 27.02(12) 4_776 4_776 ? O1 Cd1 C26 135.88(14) . 4_776 ? Cl1 Cd1 C26 95.54(10) . 4_776 ? Cl2 Cd1 C26 121.59(10) . 4_776 ? C1 Cd1 C26 120.84(14) . 4_776 ? C1 O1 Cd1 88.3(3) . . ? C1 O2 Cd1 94.3(3) . . ? C26 O3 Cd1 91.9(3) . 4_475 ? C26 O4 Cd1 90.7(3) . 4_475 ? C9 N1 C10 120.7(4) . . ? C9 N1 C8 119.8(3) . . ? C10 N1 C8 119.5(4) . . ? C17 N2 C18 120.2(4) . . ? C17 N2 C19 118.3(4) . . ? C18 N2 C19 121.3(3) . . ? O2 C1 O1 122.5(4) . . ? O2 C1 C2 118.4(4) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 Cd1 58.6(2) . . ? O1 C1 Cd1 64.5(2) . . ? C2 C1 Cd1 168.8(3) . . ? C3 C2 C4 118.8(4) . . ? C3 C2 C1 121.0(4) . . ? C4 C2 C1 120.2(4) . . ? C5 C3 C2 120.7(4) . . ? C5 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C6 C4 C2 120.7(4) . . ? C6 C4 H4 119.6 . . ? C2 C4 H4 119.6 . . ? C3 C5 C7 120.1(4) . . ? C3 C5 H5 119.9 . . ? C7 C5 H5 119.9 . . ? C7 C6 C4 120.3(4) . . ? C7 C6 H6 119.9 . . ? C4 C6 H6 119.9 . . ? C6 C7 C5 119.3(4) . . ? C6 C7 C8 120.3(4) . . ? C5 C7 C8 120.4(4) . . ? N1 C8 C7 111.5(3) . . ? N1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 C11 120.3(4) . . ? N1 C9 H9 119.9 . . ? C11 C9 H9 119.9 . . ? N1 C10 C12 120.8(4) . . ? N1 C10 H10 119.6 . . ? C12 C10 H10 119.6 . . ? C9 C11 C13 120.8(4) . . ? C9 C11 H11 119.6 . . ? C13 C11 H11 119.6 . . ? C10 C12 C13 120.1(4) . . ? C10 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C13 C12 117.2(4) . . ? C11 C13 C14 121.4(4) . . ? C12 C13 C14 121.4(4) . . ? C16 C14 C15 117.3(4) . . ? C16 C14 C13 121.1(4) . . ? C15 C14 C13 121.7(4) . . ? C17 C15 C14 120.4(4) . . ? C17 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C14 C16 C18 120.5(4) . . ? C14 C16 H16 119.8 . . ? C18 C16 H16 119.8 . . ? N2 C17 C15 121.2(4) . . ? N2 C17 H17 119.4 . . ? C15 C17 H17 119.4 . . ? N2 C18 C16 120.5(4) . . ? N2 C18 H18 119.8 . . ? C16 C18 H18 119.8 . . ? N2 C19 C20 112.3(3) . . ? N2 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N2 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C22 119.8(4) . . ? C21 C20 C19 120.1(4) . . ? C22 C20 C19 120.2(4) . . ? C20 C21 C23 120.6(4) . . ? C20 C21 H21 119.7 . . ? C23 C21 H21 119.7 . . ? C24 C22 C20 119.2(4) . . ? C24 C22 H22 120.4 . . ? C20 C22 H22 120.4 . . ? C25 C23 C21 120.3(4) . . ? C25 C23 H23 119.9 . . ? C21 C23 H23 119.9 . . ? C22 C24 C25 120.8(4) . . ? C22 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C23 C25 C24 119.3(4) . . ? C23 C25 C26 120.4(4) . . ? C24 C25 C26 120.2(4) . . ? O4 C26 O3 122.1(4) . . ? O4 C26 C25 119.9(4) . . ? O3 C26 C25 118.0(4) . . ? O4 C26 Cd1 62.3(2) . 4_475 ? O3 C26 Cd1 60.6(2) . 4_475 ? C25 C26 Cd1 169.7(3) . 4_475 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.387 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.109 #===END data_CdI2 _database_code_depnum_ccdc_archive 'CCDC 863620' #TrackingRef 'Cif-1-5-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Cd I2 N2 O4' _chemical_formula_sum 'C26 H20 Cd I2 N2 O4' _chemical_formula_weight 790.64 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.753(8) _cell_length_b 8.840(4) _cell_length_c 18.010(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.511(8) _cell_angle_gamma 90.00 _cell_volume 2498(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2345 _cell_measurement_theta_min 2.3037 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.381 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4996 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Rigaku SCXmini diffractometer' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 18514 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5645 _reflns_number_gt 4674 _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^)+(0.0587P)^2^+4.1682P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5645 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.244901(18) 0.64205(4) 0.502106(15) 0.04481(12) Uani 1 1 d . . . I1 I 0.10789(2) 0.43392(5) 0.458129(19) 0.06712(14) Uani 1 1 d . . . I2 I 0.38231(2) 0.43344(4) 0.543084(18) 0.06014(13) Uani 1 1 d . . . O1 O 0.2355(2) 0.7313(4) 0.62832(19) 0.0592(8) Uani 1 1 d . . . O2 O 0.1635(2) 0.8465(5) 0.5175(2) 0.0762(12) Uani 1 1 d . . . O3 O -0.6656(2) 0.6518(4) 0.99777(17) 0.0584(8) Uani 1 1 d . . . O4 O -0.7448(2) 0.7481(4) 0.88310(18) 0.0569(8) Uani 1 1 d . . . N1 N -0.1117(2) 0.9649(4) 0.7358(2) 0.0554(9) Uani 1 1 d . . . N2 N -0.4103(2) 0.4441(4) 0.7779(2) 0.0477(8) Uani 1 1 d . . . C1 C 0.1813(3) 0.8203(6) 0.5922(3) 0.0536(11) Uani 1 1 d . . . C2 C 0.1287(3) 0.9075(6) 0.6308(3) 0.0532(11) Uani 1 1 d . . . C3 C 0.1360(3) 0.8782(5) 0.7068(3) 0.0446(9) Uani 1 1 d . . . H3 H 0.1802 0.8138 0.7385 0.054 Uiso 1 1 calc R . . C4 C 0.0715(4) 1.0199(7) 0.5893(3) 0.0716(15) Uani 1 1 d . . . H4 H 0.0731 1.0555 0.5401 0.086 Uiso 1 1 calc R . . C5 C 0.0793(3) 0.9418(5) 0.7385(3) 0.0487(10) Uani 1 1 d . . . H5 H 0.0870 0.9239 0.7926 0.058 Uiso 1 1 calc R . . C6 C 0.0123(4) 1.0800(7) 0.6197(3) 0.0738(16) Uani 1 1 d . . . H6 H -0.0276 1.1539 0.5907 0.089 Uiso 1 1 calc R . . C7 C 0.0125(3) 1.0295(6) 0.6938(3) 0.0578(11) Uani 1 1 d . . . C8 C -0.0544(3) 1.0875(6) 0.7253(4) 0.0643(13) Uani 1 1 d . . . H8A H -0.0258 1.1375 0.7770 0.077 Uiso 1 1 calc R . . H8B H -0.0897 1.1644 0.6882 0.077 Uiso 1 1 calc R . . C9 C -0.1533(4) 0.8743(7) 0.6757(3) 0.0709(15) Uani 1 1 d . . . H9 H -0.1431 0.8826 0.6271 0.085 Uiso 1 1 calc R . . C10 C -0.1257(3) 0.9545(6) 0.8044(3) 0.0642(13) Uani 1 1 d . . . H10 H -0.0952 1.0182 0.8475 0.077 Uiso 1 1 calc R . . C11 C -0.2110(3) 0.7684(6) 0.6826(3) 0.0656(13) Uani 1 1 d . . . H11 H -0.2394 0.7038 0.6392 0.079 Uiso 1 1 calc R . . C12 C -0.1835(3) 0.8533(6) 0.8134(3) 0.0616(12) Uani 1 1 d . . . H12 H -0.1934 0.8497 0.8622 0.074 Uiso 1 1 calc R . . C13 C -0.2279(3) 0.7557(5) 0.7525(2) 0.0499(10) Uani 1 1 d . . . C14 C -0.2919(3) 0.6465(5) 0.7614(2) 0.0454(9) Uani 1 1 d . . . C15 C -0.3427(3) 0.5608(6) 0.6976(3) 0.0532(11) Uani 1 1 d . . . H15 H -0.3369 0.5711 0.6472 0.064 Uiso 1 1 calc R . . C16 C -0.3036(3) 0.6249(6) 0.8338(3) 0.0577(12) Uani 1 1 d . . . H16 H -0.2705 0.6817 0.8788 0.069 Uiso 1 1 calc R . . C17 C -0.4011(3) 0.4614(6) 0.7073(3) 0.0545(11) Uani 1 1 d . . . H17 H -0.4356 0.4037 0.6632 0.065 Uiso 1 1 calc R . . C18 C -0.3617(3) 0.5240(6) 0.8406(3) 0.0574(11) Uani 1 1 d . . . H18 H -0.3679 0.5097 0.8906 0.069 Uiso 1 1 calc R . . C19 C -0.4733(3) 0.3326(5) 0.7879(3) 0.0577(12) Uani 1 1 d . . . H19A H -0.4423 0.2518 0.8248 0.069 Uiso 1 1 calc R . . H19B H -0.5046 0.2851 0.7360 0.069 Uiso 1 1 calc R . . C20 C -0.5364(3) 0.4064(5) 0.8196(3) 0.0460(9) Uani 1 1 d . . . C21 C -0.5340(3) 0.3734(5) 0.8949(3) 0.0496(10) Uani 1 1 d . . . H21 H -0.4963 0.2979 0.9254 0.059 Uiso 1 1 calc R . . C22 C -0.5964(3) 0.5100(4) 0.7732(2) 0.0425(8) Uani 1 1 d . . . H22 H -0.6015 0.5274 0.7197 0.051 Uiso 1 1 calc R . . C23 C -0.5866(3) 0.4502(5) 0.9261(2) 0.0477(10) Uani 1 1 d . . . H23 H -0.5852 0.4258 0.9779 0.057 Uiso 1 1 calc R . . C24 C -0.6484(3) 0.5872(4) 0.8056(2) 0.0400(8) Uani 1 1 d . . . H24 H -0.6890 0.6577 0.7742 0.048 Uiso 1 1 calc R . . C25 C -0.6413(3) 0.5620(4) 0.8835(2) 0.0394(8) Uani 1 1 d . . . C26 C -0.6889(3) 0.6597(5) 0.9230(2) 0.0455(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04502(19) 0.0552(2) 0.03750(18) 0.00300(12) 0.01861(14) 0.00008(12) I1 0.0558(2) 0.0988(3) 0.0478(2) -0.00423(16) 0.01949(16) -0.02146(17) I2 0.0564(2) 0.0756(2) 0.04527(19) -0.00234(14) 0.01382(15) 0.01671(15) O1 0.064(2) 0.067(2) 0.0526(18) 0.0028(16) 0.0281(16) 0.0111(17) O2 0.070(2) 0.116(3) 0.0454(18) 0.002(2) 0.0228(17) 0.031(2) O3 0.065(2) 0.076(2) 0.0365(15) 0.0039(15) 0.0207(14) 0.0202(17) O4 0.0632(19) 0.066(2) 0.0417(16) 0.0045(15) 0.0191(15) 0.0194(16) N1 0.046(2) 0.058(2) 0.066(2) -0.0131(19) 0.0233(18) 0.0111(17) N2 0.0449(19) 0.053(2) 0.0442(19) -0.0054(16) 0.0143(16) 0.0151(16) C1 0.038(2) 0.071(3) 0.054(2) -0.017(2) 0.0188(19) -0.002(2) C2 0.041(2) 0.070(3) 0.047(2) -0.005(2) 0.0136(19) 0.009(2) C3 0.041(2) 0.042(2) 0.052(2) -0.0005(18) 0.0175(18) 0.0042(17) C4 0.070(3) 0.084(4) 0.053(3) -0.001(3) 0.011(3) 0.020(3) C5 0.052(2) 0.045(2) 0.054(2) -0.0005(18) 0.025(2) 0.0044(18) C6 0.061(3) 0.087(4) 0.062(3) -0.007(3) 0.008(3) 0.024(3) C7 0.049(2) 0.064(3) 0.064(3) -0.008(2) 0.025(2) 0.008(2) C8 0.057(3) 0.062(3) 0.079(4) -0.012(3) 0.032(3) 0.013(2) C9 0.065(3) 0.093(4) 0.063(3) -0.021(3) 0.032(3) 0.000(3) C10 0.064(3) 0.073(3) 0.051(3) -0.015(2) 0.014(2) 0.002(3) C11 0.063(3) 0.079(3) 0.061(3) -0.028(3) 0.029(2) -0.004(3) C12 0.066(3) 0.075(3) 0.042(2) -0.009(2) 0.017(2) 0.001(3) C13 0.043(2) 0.059(3) 0.046(2) -0.006(2) 0.0131(18) 0.0186(19) C14 0.040(2) 0.053(2) 0.039(2) -0.0077(17) 0.0090(17) 0.0158(17) C15 0.052(2) 0.068(3) 0.036(2) -0.007(2) 0.0121(19) 0.009(2) C16 0.059(3) 0.071(3) 0.042(2) -0.016(2) 0.015(2) 0.006(2) C17 0.054(3) 0.066(3) 0.040(2) -0.010(2) 0.0106(19) 0.012(2) C18 0.054(3) 0.076(3) 0.044(2) -0.010(2) 0.018(2) 0.005(2) C19 0.063(3) 0.049(2) 0.066(3) -0.013(2) 0.028(2) 0.005(2) C20 0.046(2) 0.041(2) 0.051(2) -0.0113(18) 0.0173(19) -0.0005(17) C21 0.056(2) 0.046(2) 0.041(2) -0.0029(18) 0.0091(19) 0.0093(19) C22 0.051(2) 0.0378(19) 0.042(2) -0.0010(16) 0.0212(18) -0.0004(17) C23 0.057(3) 0.048(2) 0.0360(19) 0.0011(17) 0.0143(18) 0.0057(19) C24 0.041(2) 0.0397(19) 0.0380(19) 0.0011(15) 0.0131(16) 0.0008(16) C25 0.0385(19) 0.042(2) 0.0389(19) -0.0030(15) 0.0149(16) -0.0040(15) C26 0.040(2) 0.053(2) 0.044(2) -0.0041(18) 0.0153(17) -0.0015(18) _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 2.338(4) . ? Cd1 O3 2.379(3) 4_675 ? Cd1 O4 2.413(3) 4_675 ? Cd1 O1 2.463(3) . ? Cd1 C26 2.728(4) 4_675 ? Cd1 C1 2.733(4) . ? Cd1 I1 2.8298(10) . ? Cd1 I2 2.8380(10) . ? O1 C1 1.206(6) . ? O2 C1 1.294(6) . ? O3 C26 1.267(5) . ? O3 Cd1 2.379(3) 4_476 ? O4 C26 1.238(5) . ? O4 Cd1 2.413(3) 4_476 ? N1 C9 1.331(6) . ? N1 C10 1.340(6) . ? N1 C8 1.502(7) . ? N2 C18 1.340(6) . ? N2 C17 1.342(6) . ? N2 C19 1.500(6) . ? C1 C2 1.510(6) . ? C2 C3 1.357(6) . ? C2 C4 1.400(7) . ? C3 C5 1.387(6) . ? C3 H3 0.9500 . ? C4 C6 1.394(8) . ? C4 H4 0.9500 . ? C5 C7 1.367(6) . ? C5 H5 0.9500 . ? C6 C7 1.407(8) . ? C6 H6 0.9500 . ? C7 C8 1.513(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.384(8) . ? C9 H9 0.9500 . ? C10 C12 1.368(8) . ? C10 H10 0.9500 . ? C11 C13 1.388(6) . ? C11 H11 0.9500 . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 C14 1.492(6) . ? C14 C15 1.390(6) . ? C14 C16 1.398(6) . ? C15 C17 1.371(7) . ? C15 H15 0.9500 . ? C16 C18 1.357(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.515(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.374(6) . ? C20 C22 1.400(6) . ? C21 C23 1.378(6) . ? C21 H21 0.9500 . ? C22 C24 1.385(5) . ? C22 H22 0.9500 . ? C23 C25 1.383(6) . ? C23 H23 0.9500 . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 C26 1.511(6) . ? C26 Cd1 2.728(4) 4_476 ? 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 O3 79.17(17) . 4_675 ? O2 Cd1 O4 91.16(13) . 4_675 ? O3 Cd1 O4 54.60(10) 4_675 4_675 ? O2 Cd1 O1 54.16(11) . . ? O3 Cd1 O1 91.72(11) 4_675 . ? O4 Cd1 O1 137.60(13) 4_675 . ? O2 Cd1 C26 85.77(14) . 4_675 ? O3 Cd1 C26 27.65(11) 4_675 4_675 ? O4 Cd1 C26 26.99(11) 4_675 4_675 ? O1 Cd1 C26 116.49(13) . 4_675 ? O2 Cd1 C1 28.21(14) . . ? O3 Cd1 C1 87.67(13) 4_675 . ? O4 Cd1 C1 117.36(15) 4_675 . ? O1 Cd1 C1 26.18(13) . . ? C26 Cd1 C1 104.76(16) 4_675 . ? O2 Cd1 I1 94.96(12) . . ? O3 Cd1 I1 161.42(8) 4_675 . ? O4 Cd1 I1 108.44(8) 4_675 . ? O1 Cd1 I1 99.12(9) . . ? C26 Cd1 I1 135.23(9) 4_675 . ? C1 Cd1 I1 95.41(10) . . ? O2 Cd1 I2 157.67(9) . . ? O3 Cd1 I2 92.47(10) 4_675 . ? O4 Cd1 I2 100.87(9) 4_675 . ? O1 Cd1 I2 106.06(8) . . ? C26 Cd1 I2 96.42(9) 4_675 . ? C1 Cd1 I2 132.07(11) . . ? I1 Cd1 I2 98.90(4) . . ? C1 O1 Cd1 89.5(3) . . ? C1 O2 Cd1 93.1(3) . . ? C26 O3 Cd1 91.7(3) . 4_476 ? C26 O4 Cd1 90.8(3) . 4_476 ? C9 N1 C10 119.9(5) . . ? C9 N1 C8 120.4(5) . . ? C10 N1 C8 119.5(4) . . ? C18 N2 C17 120.1(4) . . ? C18 N2 C19 119.4(4) . . ? C17 N2 C19 120.5(4) . . ? O1 C1 O2 122.2(4) . . ? O1 C1 C2 122.4(4) . . ? O2 C1 C2 115.4(4) . . ? O1 C1 Cd1 64.3(2) . . ? O2 C1 Cd1 58.7(2) . . ? C2 C1 Cd1 168.3(3) . . ? C3 C2 C4 118.5(4) . . ? C3 C2 C1 120.4(4) . . ? C4 C2 C1 121.2(5) . . ? C2 C3 C5 120.3(4) . . ? C2 C3 H3 119.8 . . ? C5 C3 H3 119.8 . . ? C6 C4 C2 120.6(5) . . ? C6 C4 H4 119.7 . . ? C2 C4 H4 119.7 . . ? C7 C5 C3 121.7(4) . . ? C7 C5 H5 119.2 . . ? C3 C5 H5 119.2 . . ? C4 C6 C7 119.1(5) . . ? C4 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C5 C7 C6 117.9(4) . . ? C5 C7 C8 122.2(5) . . ? C6 C7 C8 119.5(5) . . ? N1 C8 C7 113.1(4) . . ? N1 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C11 121.1(5) . . ? N1 C9 H9 119.4 . . ? C11 C9 H9 119.4 . . ? N1 C10 C12 120.9(5) . . ? N1 C10 H10 119.5 . . ? C12 C10 H10 119.5 . . ? C9 C11 C13 120.5(5) . . ? C9 C11 H11 119.7 . . ? C13 C11 H11 119.7 . . ? C10 C12 C13 121.2(5) . . ? C10 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C11 C13 C12 116.3(5) . . ? C11 C13 C14 122.1(4) . . ? C12 C13 C14 121.6(4) . . ? C15 C14 C16 116.8(4) . . ? C15 C14 C13 121.3(4) . . ? C16 C14 C13 122.0(4) . . ? C17 C15 C14 120.1(4) . . ? C17 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C18 C16 C14 121.0(4) . . ? C18 C16 H16 119.5 . . ? C14 C16 H16 119.5 . . ? N2 C17 C15 121.2(4) . . ? N2 C17 H17 119.4 . . ? C15 C17 H17 119.4 . . ? N2 C18 C16 120.9(4) . . ? N2 C18 H18 119.6 . . ? C16 C18 H18 119.6 . . ? N2 C19 C20 112.1(3) . . ? N2 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N2 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C22 119.7(4) . . ? C21 C20 C19 119.9(4) . . ? C22 C20 C19 120.4(4) . . ? C20 C21 C23 119.7(4) . . ? C20 C21 H21 120.1 . . ? C23 C21 H21 120.1 . . ? C24 C22 C20 119.7(4) . . ? C24 C22 H22 120.1 . . ? C20 C22 H22 120.1 . . ? C21 C23 C25 121.3(4) . . ? C21 C23 H23 119.3 . . ? C25 C23 H23 119.3 . . ? C25 C24 C22 120.3(4) . . ? C25 C24 H24 119.9 . . ? C22 C24 H24 119.9 . . ? C23 C25 C24 118.8(4) . . ? C23 C25 C26 120.3(4) . . ? C24 C25 C26 120.8(4) . . ? O4 C26 O3 122.7(4) . . ? O4 C26 C25 120.4(4) . . ? O3 C26 C25 116.8(4) . . ? O4 C26 Cd1 62.2(2) . 4_476 ? O3 C26 Cd1 60.6(2) . 4_476 ? C25 C26 Cd1 172.3(3) . 4_476 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.043 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.104 #===END data_CdN3 _database_code_depnum_ccdc_archive 'CCDC 863621' #TrackingRef 'Cif-1-5-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cd N8 O7' _chemical_formula_sum 'C26 H26 Cd N8 O7' _chemical_formula_weight 674.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.687(5) _cell_length_b 10.020(2) _cell_length_c 17.913(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.571(3) _cell_angle_gamma 90.00 _cell_volume 2701.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6157 _cell_measurement_theta_min 3.0038 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_process_details ? _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 'Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 20306 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6067 _reflns_number_gt 4933 _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^)+(0.0605P)^2^+0.3515P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6067 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 -0.736201(14) 0.77565(2) 0.979454(12) 0.04332(10) Uani 1 1 d . . . O1 O -0.72848(15) 0.8166(2) 0.85212(12) 0.0516(5) Uani 1 1 d . . . O1W O -1.0634(2) 0.7125(3) 1.06934(17) 0.0787(8) Uani 1 1 d . . . H1B H -1.0414 0.6802 1.0383 0.094 Uiso 1 1 d R . . H1A H -1.1197 0.7084 1.0492 0.094 Uiso 1 1 d R . . N1 N -0.39349(13) 0.9653(2) 0.72374(12) 0.0331(4) Uani 1 1 d . . . C1 C -0.66918(17) 0.9024(2) 0.88599(15) 0.0351(5) Uani 1 1 d . . . O2 O -0.64870(13) 0.94329(19) 0.95851(11) 0.0421(4) Uani 1 1 d . . . O2W O -0.7583(2) 0.3680(3) 1.02936(17) 0.0962(10) Uani 1 1 d . . . H2A H -0.7555 0.3955 0.9857 0.115 Uiso 1 1 d R . . H2B H -0.7245 0.3001 1.0415 0.115 Uiso 1 1 d R . . N2 N -0.07542(14) 0.4986(2) 0.73699(13) 0.0339(4) Uani 1 1 d . . . C2 C -0.61902(15) 0.9560(2) 0.84008(14) 0.0296(5) Uani 1 1 d . . . O3 O 0.26590(14) 0.6792(2) 0.61381(12) 0.0487(5) Uani 1 1 d . . . O3W O -0.62918(17) 0.1907(2) 1.03801(15) 0.0665(6) Uani 1 1 d . . . H3A H -0.5915 0.2347 1.0278 0.080 Uiso 1 1 d R . . H3B H -0.6282 0.1127 1.0197 0.080 Uiso 1 1 d R . . N3 N -0.6209(2) 0.6292(3) 1.02461(18) 0.0655(8) Uani 1 1 d . . . C3 C -0.63916(17) 0.9126(3) 0.76008(15) 0.0358(5) Uani 1 1 d . . . H3 H -0.6881 0.8544 0.7324 0.043 Uiso 1 1 calc R . . O4 O 0.17798(14) 0.5665(2) 0.50315(12) 0.0507(5) Uani 1 1 d . . . N4 N -0.5619(2) 0.6508(2) 1.00663(15) 0.0516(6) Uani 1 1 d . . . C4 C -0.54867(17) 1.0430(2) 0.87934(15) 0.0349(5) Uani 1 1 d . . . H4 H -0.5357 1.0747 0.9333 0.042 Uiso 1 1 calc R . . N5 N -0.5048(2) 0.6674(3) 0.9878(2) 0.0727(9) Uani 1 1 d . . . C5 C -0.58802(18) 0.9540(3) 0.72083(15) 0.0388(6) Uani 1 1 d . . . H5 H -0.6026 0.9254 0.6659 0.047 Uiso 1 1 calc R . . N6 N -0.8499(2) 0.6295(3) 0.9365(2) 0.0733(9) Uani 1 1 d . . . C6 C -0.49680(17) 1.0841(3) 0.83982(15) 0.0369(5) Uani 1 1 d . . . H6 H -0.4488 1.1441 0.8668 0.044 Uiso 1 1 calc R . . N7 N -0.88983(19) 0.6249(2) 0.97772(17) 0.0540(6) Uani 1 1 d . . . C7 C -0.51539(16) 1.0373(2) 0.76139(15) 0.0330(5) Uani 1 1 d . . . N8 N -0.9286(2) 0.6193(4) 1.0162(2) 0.0779(9) Uani 1 1 d . . . C8 C -0.45593(19) 1.0758(3) 0.72120(18) 0.0419(6) Uani 1 1 d . . . H8A H -0.4207 1.1552 0.7497 0.050 Uiso 1 1 calc R . . H8B H -0.4932 1.1005 0.6628 0.050 Uiso 1 1 calc R . . C9 C -0.36332(18) 0.8766(3) 0.78514(16) 0.0404(6) Uani 1 1 d . . . H9 H -0.3842 0.8791 0.8268 0.048 Uiso 1 1 calc R . . C10 C -0.3651(2) 0.9629(3) 0.66469(18) 0.0551(8) Uani 1 1 d . . . H10 H -0.3877 1.0258 0.6208 0.066 Uiso 1 1 calc R . . C11 C -0.30189(19) 0.7809(2) 0.78884(17) 0.0378(6) Uani 1 1 d . . . H11 H -0.2812 0.7179 0.8327 0.045 Uiso 1 1 calc R . . C12 C -0.3037(2) 0.8705(3) 0.66650(18) 0.0563(8) Uani 1 1 d . . . H12 H -0.2836 0.8711 0.6243 0.068 Uiso 1 1 calc R . . C13 C -0.27061(16) 0.7768(2) 0.72902(15) 0.0301(5) Uani 1 1 d . . . C14 C -0.20312(15) 0.6777(2) 0.73215(14) 0.0300(5) Uani 1 1 d . . . C15 C -0.15614(19) 0.5996(3) 0.80226(16) 0.0419(6) Uani 1 1 d . . . H15 H -0.1681 0.6077 0.8494 0.050 Uiso 1 1 calc R . . C16 C -0.18333(17) 0.6600(3) 0.66484(15) 0.0384(6) Uani 1 1 d . . . H16 H -0.2141 0.7108 0.6159 0.046 Uiso 1 1 calc R . . C17 C -0.09305(19) 0.5116(3) 0.80319(17) 0.0426(6) Uani 1 1 d . . . H17 H -0.0613 0.4591 0.8511 0.051 Uiso 1 1 calc R . . C18 C -0.11974(18) 0.5700(3) 0.66842(16) 0.0390(6) Uani 1 1 d . . . H18 H -0.1072 0.5584 0.6219 0.047 Uiso 1 1 calc R . . C19 C -0.0078(2) 0.3976(3) 0.73922(19) 0.0456(7) Uani 1 1 d . . . H19A H -0.0386 0.3157 0.7099 0.055 Uiso 1 1 calc R . . H19B H 0.0308 0.3735 0.7974 0.055 Uiso 1 1 calc R . . C20 C 0.04902(17) 0.4509(2) 0.69919(16) 0.0349(5) Uani 1 1 d . . . C21 C 0.03936(17) 0.3970(3) 0.62423(16) 0.0377(5) Uani 1 1 d . . . H21 H -0.0020 0.3271 0.5993 0.045 Uiso 1 1 calc R . . C22 C 0.11029(19) 0.5516(3) 0.73546(16) 0.0427(6) Uani 1 1 d . . . H22 H 0.1179 0.5876 0.7872 0.051 Uiso 1 1 calc R . . C23 C 0.08993(16) 0.4451(3) 0.58586(15) 0.0352(5) Uani 1 1 d . . . H23 H 0.0830 0.4084 0.5345 0.042 Uiso 1 1 calc R . . C24 C 0.16063(18) 0.6003(3) 0.69719(16) 0.0403(6) Uani 1 1 d . . . H24 H 0.2020 0.6703 0.7223 0.048 Uiso 1 1 calc R . . C25 C 0.15077(16) 0.5472(2) 0.62234(14) 0.0321(5) Uani 1 1 d . . . C26 C 0.20271(17) 0.6016(3) 0.57778(16) 0.0372(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 Cd1 0.05250(16) 0.04645(15) 0.04315(14) -0.00017(8) 0.03209(11) -0.00171(9) O1 0.0605(13) 0.0610(12) 0.0402(10) -0.0070(10) 0.0283(10) -0.0230(11) O1W 0.095(2) 0.0857(19) 0.0700(17) 0.0182(14) 0.0495(16) 0.0250(15) N1 0.0344(11) 0.0379(11) 0.0314(10) 0.0019(9) 0.0184(8) 0.0024(9) C1 0.0366(13) 0.0367(12) 0.0358(13) 0.0040(10) 0.0191(10) 0.0033(10) O2 0.0498(11) 0.0497(11) 0.0343(9) -0.0048(8) 0.0253(8) -0.0061(9) O2W 0.111(3) 0.086(2) 0.088(2) 0.0238(15) 0.0402(19) 0.0391(17) N2 0.0351(11) 0.0376(11) 0.0365(11) 0.0026(9) 0.0226(9) 0.0017(9) C2 0.0310(12) 0.0314(11) 0.0286(11) 0.0013(9) 0.0151(9) 0.0041(9) O3 0.0472(11) 0.0627(12) 0.0409(10) -0.0061(10) 0.0234(9) -0.0189(10) O3W 0.0801(17) 0.0590(13) 0.0736(16) -0.0090(12) 0.0457(14) 0.0045(12) N3 0.095(2) 0.0578(16) 0.0634(18) 0.0205(14) 0.0529(18) 0.0269(16) C3 0.0365(13) 0.0379(12) 0.0342(12) -0.0051(10) 0.0164(10) -0.0007(10) O4 0.0615(13) 0.0633(12) 0.0396(10) -0.0126(9) 0.0334(10) -0.0170(10) N4 0.0634(17) 0.0453(14) 0.0413(13) -0.0075(11) 0.0181(12) 0.0122(12) C4 0.0379(13) 0.0408(13) 0.0277(11) -0.0030(10) 0.0157(10) 0.0013(11) N5 0.0587(18) 0.0647(18) 0.099(2) -0.0217(18) 0.0386(18) -0.0040(15) C5 0.0456(15) 0.0436(14) 0.0310(12) -0.0072(11) 0.0202(11) 0.0018(11) N6 0.092(2) 0.082(2) 0.0690(19) -0.0255(16) 0.0569(18) -0.0361(18) C6 0.0342(13) 0.0421(13) 0.0365(13) -0.0038(11) 0.0172(10) -0.0031(11) N7 0.0602(17) 0.0470(13) 0.0590(16) 0.0012(12) 0.0296(14) -0.0091(12) C7 0.0349(13) 0.0338(12) 0.0351(12) 0.0054(10) 0.0197(10) 0.0095(10) N8 0.086(2) 0.082(2) 0.095(2) 0.0064(18) 0.067(2) -0.0097(18) C8 0.0504(16) 0.0372(13) 0.0510(15) 0.0092(12) 0.0339(13) 0.0105(12) C9 0.0466(15) 0.0450(14) 0.0424(14) 0.0106(12) 0.0313(12) 0.0090(12) C10 0.070(2) 0.0665(19) 0.0437(15) 0.0221(14) 0.0384(15) 0.0287(16) C11 0.0428(14) 0.0403(14) 0.0393(14) 0.0093(11) 0.0262(12) 0.0073(11) C12 0.072(2) 0.073(2) 0.0405(15) 0.0190(15) 0.0400(15) 0.0324(17) C13 0.0294(12) 0.0355(12) 0.0277(11) -0.0032(9) 0.0146(9) -0.0007(9) C14 0.0289(11) 0.0350(11) 0.0279(11) -0.0042(9) 0.0141(9) -0.0038(9) C15 0.0496(15) 0.0523(15) 0.0328(12) 0.0081(12) 0.0264(12) 0.0105(13) C16 0.0403(14) 0.0507(15) 0.0272(11) 0.0032(11) 0.0173(10) 0.0069(12) C17 0.0481(16) 0.0495(15) 0.0391(14) 0.0136(12) 0.0273(12) 0.0117(12) C18 0.0426(14) 0.0487(14) 0.0326(12) 0.0034(11) 0.0228(11) 0.0071(12) C19 0.0563(17) 0.0378(13) 0.0609(17) 0.0128(13) 0.0426(15) 0.0138(12) C20 0.0364(13) 0.0358(12) 0.0396(13) 0.0075(10) 0.0232(11) 0.0077(10) C21 0.0374(13) 0.0378(13) 0.0411(13) -0.0034(11) 0.0200(11) -0.0033(10) C22 0.0518(16) 0.0470(15) 0.0354(13) -0.0076(12) 0.0247(12) 0.0019(12) C23 0.0365(13) 0.0415(13) 0.0312(12) -0.0042(10) 0.0181(10) -0.0013(10) C24 0.0419(14) 0.0432(14) 0.0384(13) -0.0087(11) 0.0197(11) -0.0091(11) C25 0.0313(12) 0.0385(12) 0.0298(11) 0.0004(10) 0.0163(10) 0.0030(10) C26 0.0374(13) 0.0415(13) 0.0397(13) 0.0018(11) 0.0232(11) 0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N6 2.253(3) . ? Cd1 N3 2.273(3) . ? Cd1 O4 2.293(2) 4_476 ? Cd1 O2 2.3595(19) . ? Cd1 O1 2.375(2) . ? Cd1 O3 2.434(2) 4_476 ? Cd1 C26 2.684(2) 4_476 ? Cd1 C1 2.699(2) . ? O1 C1 1.252(3) . ? O1W H1B 0.8500 . ? O1W H1A 0.8501 . ? N1 C9 1.332(3) . ? N1 C10 1.333(3) . ? N1 C8 1.507(3) . ? C1 O2 1.261(3) . ? C1 C2 1.503(3) . ? O2W H2A 0.8500 . ? O2W H2B 0.8500 . ? N2 C18 1.335(3) . ? N2 C17 1.346(3) . ? N2 C19 1.504(3) . ? C2 C4 1.385(3) . ? C2 C3 1.393(3) . ? O3 C26 1.243(3) . ? O3 Cd1 2.434(2) 4_675 ? O3W H3A 0.8499 . ? O3W H3B 0.8501 . ? N3 N4 1.180(4) . ? C3 C5 1.383(4) . ? C3 H3 0.9500 . ? O4 C26 1.267(3) . ? O4 Cd1 2.293(2) 4_675 ? N4 N5 1.151(4) . ? C4 C6 1.396(3) . ? C4 H4 0.9500 . ? C5 C7 1.390(4) . ? C5 H5 0.9500 . ? N6 N7 1.190(4) . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? N7 N8 1.132(4) . ? C7 C8 1.506(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.384(3) . ? C9 H9 0.9500 . ? C10 C12 1.371(4) . ? C10 H10 0.9500 . ? C11 C13 1.380(3) . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.484(3) . ? C14 C16 1.392(3) . ? C14 C15 1.398(3) . ? C15 C17 1.368(4) . ? C15 H15 0.9500 . ? C16 C18 1.373(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.511(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C22 1.383(4) . ? C20 C21 1.390(4) . ? C21 C23 1.385(3) . ? C21 H21 0.9500 . ? C22 C24 1.382(4) . ? C22 H22 0.9500 . ? C23 C25 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.385(3) . ? C24 H24 0.9500 . ? C25 C26 1.511(3) . ? C26 Cd1 2.684(2) 4_675 ? 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 N6 Cd1 N3 99.26(15) . . ? N6 Cd1 O4 90.60(11) . 4_476 ? N3 Cd1 O4 151.63(9) . 4_476 ? N6 Cd1 O2 153.65(10) . . ? N3 Cd1 O2 91.67(10) . . ? O4 Cd1 O2 90.97(8) 4_476 . ? N6 Cd1 O1 99.85(9) . . ? N3 Cd1 O1 93.71(9) . . ? O4 Cd1 O1 110.84(8) 4_476 . ? O2 Cd1 O1 55.29(6) . . ? N6 Cd1 O3 96.27(9) . 4_476 ? N3 Cd1 O3 96.87(8) . 4_476 ? O4 Cd1 O3 55.41(7) 4_476 4_476 ? O2 Cd1 O3 106.19(7) . 4_476 ? O1 Cd1 O3 159.02(9) . 4_476 ? N6 Cd1 C26 91.12(10) . 4_476 ? N3 Cd1 C26 124.42(9) . 4_476 ? O4 Cd1 C26 28.12(7) 4_476 4_476 ? O2 Cd1 C26 102.38(7) . 4_476 ? O1 Cd1 C26 138.12(8) . 4_476 ? O3 Cd1 C26 27.55(7) 4_476 4_476 ? N6 Cd1 C1 127.41(9) . . ? N3 Cd1 C1 90.61(9) . . ? O4 Cd1 C1 104.43(7) 4_476 . ? O2 Cd1 C1 27.84(7) . . ? O1 Cd1 C1 27.65(7) . . ? O3 Cd1 C1 133.85(8) 4_476 . ? C26 Cd1 C1 124.60(8) 4_476 . ? C1 O1 Cd1 90.70(15) . . ? H1B O1W H1A 114.4 . . ? C9 N1 C10 120.4(2) . . ? C9 N1 C8 121.7(2) . . ? C10 N1 C8 117.9(2) . . ? O1 C1 O2 121.9(2) . . ? O1 C1 C2 119.4(2) . . ? O2 C1 C2 118.7(2) . . ? O1 C1 Cd1 61.65(13) . . ? O2 C1 Cd1 60.94(13) . . ? C2 C1 Cd1 170.15(17) . . ? C1 O2 Cd1 91.23(15) . . ? H2A O2W H2B 101.6 . . ? C18 N2 C17 120.9(2) . . ? C18 N2 C19 119.8(2) . . ? C17 N2 C19 119.3(2) . . ? C4 C2 C3 119.6(2) . . ? C4 C2 C1 119.8(2) . . ? C3 C2 C1 120.5(2) . . ? C26 O3 Cd1 87.47(15) . 4_675 ? H3A O3W H3B 104.8 . . ? N4 N3 Cd1 117.5(2) . . ? C5 C3 C2 120.1(2) . . ? C5 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C26 O4 Cd1 93.35(16) . 4_675 ? N5 N4 N3 177.6(3) . . ? C2 C4 C6 120.2(2) . . ? C2 C4 H4 119.9 . . ? C6 C4 H4 119.9 . . ? C3 C5 C7 120.3(2) . . ? C3 C5 H5 119.9 . . ? C7 C5 H5 119.9 . . ? N7 N6 Cd1 115.3(2) . . ? C7 C6 C4 119.9(2) . . ? C7 C6 H6 120.0 . . ? C4 C6 H6 120.0 . . ? N8 N7 N6 179.1(4) . . ? C6 C7 C5 119.8(2) . . ? C6 C7 C8 119.6(2) . . ? C5 C7 C8 120.6(2) . . ? C7 C8 N1 112.8(2) . . ? C7 C8 H8A 109.0 . . ? N1 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? N1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C11 120.7(2) . . ? N1 C9 H9 119.7 . . ? C11 C9 H9 119.7 . . ? N1 C10 C12 120.8(3) . . ? N1 C10 H10 119.6 . . ? C12 C10 H10 119.6 . . ? C13 C11 C9 120.3(2) . . ? C13 C11 H11 119.9 . . ? C9 C11 H11 119.9 . . ? C10 C12 C13 120.7(2) . . ? C10 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C11 C13 C12 117.1(2) . . ? C11 C13 C14 121.7(2) . . ? C12 C13 C14 121.1(2) . . ? C16 C14 C15 117.2(2) . . ? C16 C14 C13 120.8(2) . . ? C15 C14 C13 122.0(2) . . ? C17 C15 C14 120.1(2) . . ? C17 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C18 C16 C14 120.7(2) . . ? C18 C16 H16 119.7 . . ? C14 C16 H16 119.7 . . ? N2 C17 C15 120.8(2) . . ? N2 C17 H17 119.6 . . ? C15 C17 H17 119.6 . . ? N2 C18 C16 120.3(2) . . ? N2 C18 H18 119.8 . . ? C16 C18 H18 119.8 . . ? N2 C19 C20 111.5(2) . . ? N2 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N2 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C22 C20 C21 119.4(2) . . ? C22 C20 C19 121.5(2) . . ? C21 C20 C19 119.1(2) . . ? C23 C21 C20 120.2(2) . . ? C23 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C24 C22 C20 120.6(2) . . ? C24 C22 H22 119.7 . . ? C20 C22 H22 119.7 . . ? C21 C23 C25 120.1(2) . . ? C21 C23 H23 120.0 . . ? C25 C23 H23 120.0 . . ? C22 C24 C25 120.0(2) . . ? C22 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C23 119.7(2) . . ? C24 C25 C26 121.1(2) . . ? C23 C25 C26 119.1(2) . . ? O3 C26 O4 122.6(2) . . ? O3 C26 C25 120.2(2) . . ? O4 C26 C25 117.2(2) . . ? O3 C26 Cd1 64.98(14) . 4_675 ? O4 C26 Cd1 58.53(13) . 4_675 ? C25 C26 Cd1 168.24(18) . 4_675 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.708 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.070 #===END data_CdSCN _database_code_depnum_ccdc_archive 'CCDC 863622' #TrackingRef 'Cif-1-5-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Cd N4 O4 S2' _chemical_formula_sum 'C28 H20 Cd N4 O4 S2' _chemical_formula_weight 653.00 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.478(6) _cell_length_b 9.716(3) _cell_length_c 18.084(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.075(4) _cell_angle_gamma 90.00 _cell_volume 2643.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6157 _cell_measurement_theta_min 3.0038 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Saturn 70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 19992 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5968 _reflns_number_gt 4220 _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^)+(0.0816P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5968 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 -0.760037(18) 0.23449(3) 0.516999(16) 0.04732(13) Uani 1 1 d . . . S1 S -0.59036(12) -0.16076(13) 0.53415(9) 0.0958(5) Uani 1 1 d . . . S2 S -0.90979(15) -0.20871(15) 0.46016(9) 0.1092(7) Uani 1 1 d . . . O1 O -0.75291(19) 0.2872(3) 0.38946(16) 0.0553(7) Uani 1 1 d . . . O2 O -0.67263(18) 0.4060(3) 0.49793(16) 0.0578(7) Uani 1 1 d . . . O3 O 0.15148(18) 0.0976(3) 0.03349(16) 0.0582(7) Uani 1 1 d . . . O4 O 0.2355(2) 0.2052(3) 0.14575(17) 0.0579(7) Uani 1 1 d . . . N1 N -0.41182(18) 0.5103(3) 0.27142(17) 0.0388(6) Uani 1 1 d . . . N2 N -0.11080(18) 0.0127(3) 0.25725(17) 0.0397(6) Uani 1 1 d . . . N3 N -0.6412(3) 0.0945(5) 0.5694(2) 0.0857(13) Uani 1 1 d . . . N4 N -0.8613(3) 0.0678(4) 0.4747(2) 0.0879(14) Uani 1 1 d . . . C1 C -0.6933(2) 0.3733(3) 0.4252(2) 0.0422(8) Uani 1 1 d . . . C2 C -0.6424(2) 0.4400(3) 0.38231(19) 0.0357(7) Uani 1 1 d . . . C3 C -0.6484(2) 0.3921(3) 0.3082(2) 0.0392(7) Uani 1 1 d . . . H3 H -0.6881 0.3193 0.2816 0.047 Uiso 1 1 calc R . . C4 C -0.5857(2) 0.5501(3) 0.4192(2) 0.0425(8) Uani 1 1 d . . . H4 H -0.5832 0.5858 0.4690 0.051 Uiso 1 1 calc R . . C5 C -0.5959(2) 0.4510(3) 0.2729(2) 0.0440(8) Uani 1 1 d . . . H5 H -0.6003 0.4184 0.2218 0.053 Uiso 1 1 calc R . . C6 C -0.5336(2) 0.6072(3) 0.3844(2) 0.0412(7) Uani 1 1 d . . . H6 H -0.4949 0.6814 0.4105 0.049 Uiso 1 1 calc R . . C7 C -0.5372(2) 0.5569(3) 0.3113(2) 0.0402(7) Uani 1 1 d . . . C8 C -0.4761(3) 0.6157(3) 0.2753(2) 0.0492(9) Uani 1 1 d . . . H8A H -0.5121 0.6503 0.2200 0.059 Uiso 1 1 calc R . . H8B H -0.4427 0.6944 0.3086 0.059 Uiso 1 1 calc R . . C9 C -0.3613(2) 0.4400(3) 0.3390(2) 0.0458(8) Uani 1 1 d . . . H9 H -0.3675 0.4573 0.3882 0.055 Uiso 1 1 calc R . . C10 C -0.4020(2) 0.4903(4) 0.2025(2) 0.0445(8) Uani 1 1 d . . . H10 H -0.4364 0.5430 0.1559 0.053 Uiso 1 1 calc R . . C11 C -0.3017(2) 0.3448(3) 0.3374(2) 0.0439(8) Uani 1 1 d . . . H11 H -0.2669 0.2958 0.3854 0.053 Uiso 1 1 calc R . . C12 C -0.3430(2) 0.3946(4) 0.1980(2) 0.0447(8) Uani 1 1 d . . . H12 H -0.3376 0.3805 0.1483 0.054 Uiso 1 1 calc R . . C13 C -0.2910(2) 0.3181(3) 0.2660(2) 0.0365(7) Uani 1 1 d . . . C14 C -0.2271(2) 0.2127(3) 0.2625(2) 0.0371(7) Uani 1 1 d . . . C15 C -0.1918(3) 0.1152(4) 0.3234(2) 0.0561(10) Uani 1 1 d . . . H15 H -0.2080 0.1163 0.3682 0.067 Uiso 1 1 calc R . . C16 C -0.2015(2) 0.2060(4) 0.1986(2) 0.0468(8) Uani 1 1 d . . . H16 H -0.2239 0.2713 0.1559 0.056 Uiso 1 1 calc R . . C17 C -0.1340(3) 0.0175(4) 0.3195(2) 0.0553(10) Uani 1 1 d . . . H17 H -0.1100 -0.0479 0.3619 0.066 Uiso 1 1 calc R . . C18 C -0.1437(2) 0.1050(3) 0.1966(2) 0.0467(8) Uani 1 1 d . . . H18 H -0.1270 0.1003 0.1522 0.056 Uiso 1 1 calc R . . C19 C -0.0525(2) -0.1015(3) 0.2516(2) 0.0465(8) Uani 1 1 d . . . H19A H -0.0901 -0.1749 0.2161 0.056 Uiso 1 1 calc R . . H19B H -0.0195 -0.1415 0.3061 0.056 Uiso 1 1 calc R . . C20 C 0.0129(2) -0.0532(3) 0.2185(2) 0.0385(7) Uani 1 1 d . . . C21 C 0.0029(2) -0.0943(3) 0.1421(2) 0.0442(8) Uani 1 1 d . . . H21 H -0.0419 -0.1592 0.1130 0.053 Uiso 1 1 calc R . . C22 C 0.0829(2) 0.0347(3) 0.2625(2) 0.0413(7) Uani 1 1 d . . . H22 H 0.0931 0.0588 0.3165 0.050 Uiso 1 1 calc R . . C23 C 0.0574(2) -0.0421(3) 0.1075(2) 0.0429(8) Uani 1 1 d . . . H23 H 0.0495 -0.0707 0.0548 0.052 Uiso 1 1 calc R . . C24 C 0.1375(2) 0.0868(3) 0.22827(19) 0.0372(7) Uani 1 1 d . . . H24 H 0.1848 0.1469 0.2587 0.045 Uiso 1 1 calc R . . C25 C 0.1236(2) 0.0522(3) 0.14975(19) 0.0358(7) Uani 1 1 d . . . C26 C 0.1737(2) 0.1227(3) 0.1075(2) 0.0418(7) Uani 1 1 d . . . C27 C -0.6220(3) -0.0128(5) 0.5533(2) 0.0602(10) Uani 1 1 d . . . C28 C -0.8806(3) -0.0478(5) 0.4689(3) 0.0727(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 0.0552(2) 0.05138(18) 0.03900(18) -0.00063(10) 0.02286(14) 0.00005(12) S1 0.1372(13) 0.0662(8) 0.0795(9) -0.0199(6) 0.0395(9) 0.0109(8) S2 0.1740(18) 0.0770(8) 0.0620(9) 0.0013(7) 0.0334(10) -0.0450(10) O1 0.0615(17) 0.0674(16) 0.0373(14) -0.0080(12) 0.0204(13) -0.0215(14) O2 0.0648(17) 0.0755(17) 0.0416(15) -0.0158(13) 0.0305(13) -0.0204(14) O3 0.0673(17) 0.0734(17) 0.0380(15) -0.0080(12) 0.0258(13) -0.0183(14) O4 0.0680(18) 0.0641(15) 0.0474(16) -0.0108(13) 0.0293(14) -0.0239(14) N1 0.0419(15) 0.0367(13) 0.0435(16) -0.0032(11) 0.0233(13) -0.0042(11) N2 0.0385(15) 0.0407(14) 0.0442(16) 0.0034(12) 0.0212(13) 0.0006(12) N3 0.106(3) 0.093(3) 0.062(3) 0.008(2) 0.039(2) 0.043(3) N4 0.131(4) 0.071(2) 0.055(2) -0.0087(19) 0.032(2) -0.035(3) C1 0.0452(18) 0.0465(17) 0.0343(18) -0.0029(14) 0.0156(15) 0.0026(15) C2 0.0383(16) 0.0388(15) 0.0297(16) 0.0001(12) 0.0135(13) 0.0068(13) C3 0.0411(17) 0.0415(16) 0.0344(17) -0.0064(13) 0.0149(14) -0.0032(14) C4 0.0488(19) 0.0438(17) 0.0346(18) -0.0070(13) 0.0169(15) -0.0002(15) C5 0.058(2) 0.0435(17) 0.0368(18) -0.0069(14) 0.0255(16) 0.0032(16) C6 0.0454(18) 0.0352(15) 0.0421(19) -0.0052(13) 0.0167(15) -0.0006(14) C7 0.0437(18) 0.0361(15) 0.044(2) 0.0030(13) 0.0212(16) 0.0073(14) C8 0.061(2) 0.0368(16) 0.060(2) 0.0047(15) 0.036(2) 0.0039(16) C9 0.055(2) 0.0492(18) 0.0386(19) -0.0024(15) 0.0238(17) -0.0013(16) C10 0.0439(19) 0.0517(19) 0.0395(19) 0.0041(15) 0.0186(16) 0.0028(16) C11 0.0459(19) 0.0517(19) 0.0340(18) 0.0023(14) 0.0159(15) 0.0029(16) C12 0.0466(19) 0.056(2) 0.0325(18) -0.0006(14) 0.0175(15) 0.0010(16) C13 0.0321(16) 0.0416(16) 0.0366(17) -0.0047(13) 0.0150(13) -0.0071(13) C14 0.0324(16) 0.0443(16) 0.0342(17) -0.0030(13) 0.0131(13) -0.0089(13) C15 0.069(3) 0.068(2) 0.036(2) 0.0084(17) 0.0256(19) 0.016(2) C16 0.050(2) 0.0494(18) 0.050(2) 0.0147(16) 0.0297(18) 0.0072(16) C17 0.067(3) 0.060(2) 0.041(2) 0.0135(16) 0.0246(19) 0.0139(19) C18 0.056(2) 0.0476(18) 0.050(2) 0.0125(15) 0.0350(18) 0.0084(16) C19 0.049(2) 0.0347(16) 0.062(2) 0.0069(15) 0.0288(18) 0.0030(14) C20 0.0383(17) 0.0330(15) 0.0435(19) 0.0032(13) 0.0161(15) 0.0056(13) C21 0.0434(18) 0.0418(17) 0.0393(19) -0.0024(14) 0.0086(15) -0.0062(14) C22 0.052(2) 0.0384(16) 0.0383(18) -0.0035(13) 0.0228(16) 0.0002(15) C23 0.051(2) 0.0448(17) 0.0312(17) -0.0065(13) 0.0150(15) 0.0005(15) C24 0.0387(17) 0.0354(15) 0.0341(17) -0.0063(12) 0.0114(14) -0.0013(13) C25 0.0370(16) 0.0344(14) 0.0365(17) 0.0014(12) 0.0154(14) 0.0048(13) C26 0.0455(19) 0.0428(17) 0.0386(19) 0.0009(14) 0.0187(15) 0.0064(15) C27 0.070(3) 0.071(3) 0.039(2) 0.0005(18) 0.0209(19) 0.005(2) C28 0.088(3) 0.087(3) 0.037(2) 0.002(2) 0.019(2) -0.031(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 N4 2.225(4) . ? Cd1 N3 2.251(4) . ? Cd1 O3 2.287(3) 4_466 ? Cd1 O2 2.319(3) . ? Cd1 O1 2.412(3) . ? Cd1 O4 2.431(3) 4_466 ? Cd1 C26 2.693(4) 4_466 ? Cd1 C1 2.697(4) . ? S1 C27 1.614(5) . ? S2 C28 1.625(5) . ? O1 C1 1.251(4) . ? O2 C1 1.258(4) . ? O3 C26 1.259(4) . ? O3 Cd1 2.287(3) 4_665 ? O4 C26 1.258(4) . ? O4 Cd1 2.431(3) 4_665 ? N1 C10 1.335(5) . ? N1 C9 1.350(4) . ? N1 C8 1.495(4) . ? N2 C17 1.329(5) . ? N2 C18 1.347(4) . ? N2 C19 1.499(4) . ? N3 C27 1.161(5) . ? N4 C28 1.160(6) . ? C1 C2 1.502(5) . ? C2 C3 1.384(4) . ? C2 C4 1.398(4) . ? C3 C5 1.391(5) . ? C3 H3 0.9500 . ? C4 C6 1.372(5) . ? C4 H4 0.9500 . ? C5 C7 1.389(5) . ? C5 H5 0.9500 . ? C6 C7 1.389(5) . ? C6 H6 0.9500 . ? C7 C8 1.517(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.358(5) . ? C9 H9 0.9500 . ? C10 C12 1.371(5) . ? C10 H10 0.9500 . ? C11 C13 1.398(5) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.488(5) . ? C14 C16 1.384(5) . ? C14 C15 1.389(5) . ? C15 C17 1.366(5) . ? C15 H15 0.9500 . ? C16 C18 1.379(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.505(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.381(5) . ? C20 C22 1.394(5) . ? C21 C23 1.382(5) . ? C21 H21 0.9500 . ? C22 C24 1.379(5) . ? C22 H22 0.9500 . ? C23 C25 1.390(4) . ? C23 H23 0.9500 . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 C26 1.500(5) . ? C26 Cd1 2.693(4) 4_665 ? 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 N4 Cd1 N3 96.12(19) . . ? N4 Cd1 O3 97.79(16) . 4_466 ? N3 Cd1 O3 150.15(13) . 4_466 ? N4 Cd1 O2 153.65(13) . . ? N3 Cd1 O2 90.60(15) . . ? O3 Cd1 O2 88.53(11) 4_466 . ? N4 Cd1 O1 98.49(13) . . ? N3 Cd1 O1 99.06(13) . . ? O3 Cd1 O1 104.82(10) 4_466 . ? O2 Cd1 O1 55.23(9) . . ? N4 Cd1 O4 101.15(14) . 4_466 ? N3 Cd1 O4 95.94(12) . 4_466 ? O3 Cd1 O4 55.47(9) 4_466 4_466 ? O2 Cd1 O4 103.46(10) . 4_466 ? O1 Cd1 O4 153.79(11) . 4_466 ? N4 Cd1 C26 98.68(15) . 4_466 ? N3 Cd1 C26 123.64(13) . 4_466 ? O3 Cd1 C26 27.78(9) 4_466 4_466 ? O2 Cd1 C26 98.66(10) . 4_466 ? O1 Cd1 C26 131.44(10) . 4_466 ? O4 Cd1 C26 27.82(9) 4_466 4_466 ? N4 Cd1 C1 126.08(13) . . ? N3 Cd1 C1 93.34(14) . . ? O3 Cd1 C1 99.51(10) 4_466 . ? O2 Cd1 C1 27.75(9) . . ? O1 Cd1 C1 27.63(9) . . ? O4 Cd1 C1 130.42(10) 4_466 . ? C26 Cd1 C1 118.99(11) 4_466 . ? C1 O1 Cd1 89.0(2) . . ? C1 O2 Cd1 93.1(2) . . ? C26 O3 Cd1 94.4(2) . 4_665 ? C26 O4 Cd1 87.8(2) . 4_665 ? C10 N1 C9 120.5(3) . . ? C10 N1 C8 120.1(3) . . ? C9 N1 C8 119.4(3) . . ? C17 N2 C18 120.5(3) . . ? C17 N2 C19 119.9(3) . . ? C18 N2 C19 119.5(3) . . ? C27 N3 Cd1 135.8(4) . . ? C28 N4 Cd1 151.0(5) . . ? O1 C1 O2 122.1(3) . . ? O1 C1 C2 120.5(3) . . ? O2 C1 C2 117.4(3) . . ? O1 C1 Cd1 63.4(2) . . ? O2 C1 Cd1 59.17(19) . . ? C2 C1 Cd1 170.9(2) . . ? C3 C2 C4 119.3(3) . . ? C3 C2 C1 121.4(3) . . ? C4 C2 C1 119.3(3) . . ? C2 C3 C5 119.6(3) . . ? C2 C3 H3 120.2 . . ? C5 C3 H3 120.2 . . ? C6 C4 C2 120.9(3) . . ? C6 C4 H4 119.6 . . ? C2 C4 H4 119.6 . . ? C7 C5 C3 120.8(3) . . ? C7 C5 H5 119.6 . . ? C3 C5 H5 119.6 . . ? C4 C6 C7 120.1(3) . . ? C4 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C5 C7 C6 119.2(3) . . ? C5 C7 C8 120.9(3) . . ? C6 C7 C8 119.9(3) . . ? N1 C8 C7 111.6(3) . . ? N1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 C11 120.6(3) . . ? N1 C9 H9 119.7 . . ? C11 C9 H9 119.7 . . ? N1 C10 C12 120.8(3) . . ? N1 C10 H10 119.6 . . ? C12 C10 H10 119.6 . . ? C9 C11 C13 120.8(3) . . ? C9 C11 H11 119.6 . . ? C13 C11 H11 119.6 . . ? C10 C12 C13 120.4(3) . . ? C10 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C11 116.9(3) . . ? C12 C13 C14 121.4(3) . . ? C11 C13 C14 121.7(3) . . ? C16 C14 C15 117.3(3) . . ? C16 C14 C13 122.0(3) . . ? C15 C14 C13 120.7(3) . . ? C17 C15 C14 120.6(4) . . ? C17 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C18 C16 C14 120.3(3) . . ? C18 C16 H16 119.8 . . ? C14 C16 H16 119.8 . . ? N2 C17 C15 121.0(3) . . ? N2 C17 H17 119.5 . . ? C15 C17 H17 119.5 . . ? N2 C18 C16 120.3(3) . . ? N2 C18 H18 119.8 . . ? C16 C18 H18 119.8 . . ? N2 C19 C20 112.3(3) . . ? N2 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N2 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C22 118.8(3) . . ? C21 C20 C19 119.6(3) . . ? C22 C20 C19 121.5(3) . . ? C20 C21 C23 120.8(3) . . ? C20 C21 H21 119.6 . . ? C23 C21 H21 119.6 . . ? C24 C22 C20 120.4(3) . . ? C24 C22 H22 119.8 . . ? C20 C22 H22 119.8 . . ? C21 C23 C25 120.2(3) . . ? C21 C23 H23 119.9 . . ? C25 C23 H23 119.9 . . ? C22 C24 C25 120.4(3) . . ? C22 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C23 119.1(3) . . ? C24 C25 C26 121.1(3) . . ? C23 C25 C26 119.6(3) . . ? O4 C26 O3 121.8(3) . . ? O4 C26 C25 120.1(3) . . ? O3 C26 C25 118.1(3) . . ? O4 C26 Cd1 64.4(2) . 4_665 ? O3 C26 Cd1 57.86(18) . 4_665 ? C25 C26 Cd1 171.4(2) . 4_665 ? N3 C27 S1 177.2(5) . . ? N4 C28 S2 178.7(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 N4 Cd1 O1 C1 -177.4(2) . . . . ? N3 Cd1 O1 C1 -79.8(2) . . . . ? O3 Cd1 O1 C1 82.1(2) 4_466 . . . ? O2 Cd1 O1 C1 4.6(2) . . . . ? O4 Cd1 O1 C1 44.3(3) 4_466 . . . ? C26 Cd1 O1 C1 73.0(3) 4_466 . . . ? N4 Cd1 O2 C1 -9.1(4) . . . . ? N3 Cd1 O2 C1 96.0(2) . . . . ? O3 Cd1 O2 C1 -113.8(2) 4_466 . . . ? O1 Cd1 O2 C1 -4.6(2) . . . . ? O4 Cd1 O2 C1 -167.7(2) 4_466 . . . ? C26 Cd1 O2 C1 -139.8(2) 4_466 . . . ? N4 Cd1 N3 C27 34.3(6) . . . . ? O3 Cd1 N3 C27 151.7(5) 4_466 . . . ? O2 Cd1 N3 C27 -120.2(6) . . . . ? O1 Cd1 N3 C27 -65.4(6) . . . . ? O4 Cd1 N3 C27 136.2(6) 4_466 . . . ? C26 Cd1 N3 C27 139.0(5) 4_466 . . . ? C1 Cd1 N3 C27 -92.6(6) . . . . ? N3 Cd1 N4 C28 2.9(8) . . . . ? O3 Cd1 N4 C28 -150.6(8) 4_466 . . . ? O2 Cd1 N4 C28 106.8(8) . . . . ? O1 Cd1 N4 C28 103.1(8) . . . . ? O4 Cd1 N4 C28 -94.4(8) 4_466 . . . ? C26 Cd1 N4 C28 -122.5(8) 4_466 . . . ? C1 Cd1 N4 C28 101.6(8) . . . . ? Cd1 O1 C1 O2 -8.2(4) . . . . ? Cd1 O1 C1 C2 170.7(3) . . . . ? Cd1 O2 C1 O1 8.6(4) . . . . ? Cd1 O2 C1 C2 -170.4(3) . . . . ? N4 Cd1 C1 O1 3.1(3) . . . . ? N3 Cd1 C1 O1 103.2(2) . . . . ? O3 Cd1 C1 O1 -103.8(2) 4_466 . . . ? O2 Cd1 C1 O1 -171.9(4) . . . . ? O4 Cd1 C1 O1 -156.08(19) 4_466 . . . ? C26 Cd1 C1 O1 -125.0(2) 4_466 . . . ? N4 Cd1 C1 O2 175.0(2) . . . . ? N3 Cd1 C1 O2 -84.9(2) . . . . ? O3 Cd1 C1 O2 68.0(2) 4_466 . . . ? O1 Cd1 C1 O2 171.9(4) . . . . ? O4 Cd1 C1 O2 15.8(3) 4_466 . . . ? C26 Cd1 C1 O2 46.9(2) 4_466 . . . ? N4 Cd1 C1 C2 -114.6(15) . . . . ? N3 Cd1 C1 C2 -14.6(15) . . . . ? O3 Cd1 C1 C2 138.4(15) 4_466 . . . ? O2 Cd1 C1 C2 70.4(14) . . . . ? O1 Cd1 C1 C2 -117.8(15) . . . . ? O4 Cd1 C1 C2 86.2(15) 4_466 . . . ? C26 Cd1 C1 C2 117.3(15) 4_466 . . . ? O1 C1 C2 C3 -11.4(5) . . . . ? O2 C1 C2 C3 167.6(3) . . . . ? Cd1 C1 C2 C3 101.9(15) . . . . ? O1 C1 C2 C4 170.6(3) . . . . ? O2 C1 C2 C4 -10.4(5) . . . . ? Cd1 C1 C2 C4 -76.1(15) . . . . ? C4 C2 C3 C5 2.1(5) . . . . ? C1 C2 C3 C5 -175.9(3) . . . . ? C3 C2 C4 C6 -2.6(5) . . . . ? C1 C2 C4 C6 175.4(3) . . . . ? C2 C3 C5 C7 0.4(5) . . . . ? C2 C4 C6 C7 0.6(5) . . . . ? C3 C5 C7 C6 -2.3(5) . . . . ? C3 C5 C7 C8 176.4(3) . . . . ? C4 C6 C7 C5 1.8(5) . . . . ? C4 C6 C7 C8 -176.9(3) . . . . ? C10 N1 C8 C7 129.9(3) . . . . ? C9 N1 C8 C7 -52.9(4) . . . . ? C5 C7 C8 N1 -63.3(4) . . . . ? C6 C7 C8 N1 115.4(3) . . . . ? C10 N1 C9 C11 -2.1(5) . . . . ? C8 N1 C9 C11 -179.3(3) . . . . ? C9 N1 C10 C12 2.4(5) . . . . ? C8 N1 C10 C12 179.6(3) . . . . ? N1 C9 C11 C13 0.4(5) . . . . ? N1 C10 C12 C13 -1.1(5) . . . . ? C10 C12 C13 C11 -0.5(5) . . . . ? C10 C12 C13 C14 179.4(3) . . . . ? C9 C11 C13 C12 0.9(5) . . . . ? C9 C11 C13 C14 -179.1(3) . . . . ? C12 C13 C14 C16 14.6(5) . . . . ? C11 C13 C14 C16 -165.5(3) . . . . ? C12 C13 C14 C15 -164.4(3) . . . . ? C11 C13 C14 C15 15.5(5) . . . . ? C16 C14 C15 C17 0.2(6) . . . . ? C13 C14 C15 C17 179.2(4) . . . . ? C15 C14 C16 C18 0.4(5) . . . . ? C13 C14 C16 C18 -178.5(3) . . . . ? C18 N2 C17 C15 0.3(6) . . . . ? C19 N2 C17 C15 -175.6(3) . . . . ? C14 C15 C17 N2 -0.6(6) . . . . ? C17 N2 C18 C16 0.4(5) . . . . ? C19 N2 C18 C16 176.3(3) . . . . ? C14 C16 C18 N2 -0.7(6) . . . . ? C17 N2 C19 C20 -142.5(3) . . . . ? C18 N2 C19 C20 41.5(4) . . . . ? N2 C19 C20 C21 -110.1(4) . . . . ? N2 C19 C20 C22 68.7(4) . . . . ? C22 C20 C21 C23 -4.4(5) . . . . ? C19 C20 C21 C23 174.4(3) . . . . ? C21 C20 C22 C24 4.3(5) . . . . ? C19 C20 C22 C24 -174.5(3) . . . . ? C20 C21 C23 C25 0.5(5) . . . . ? C20 C22 C24 C25 -0.2(5) . . . . ? C22 C24 C25 C23 -3.8(5) . . . . ? C22 C24 C25 C26 171.3(3) . . . . ? C21 C23 C25 C24 3.6(5) . . . . ? C21 C23 C25 C26 -171.5(3) . . . . ? Cd1 O4 C26 O3 7.7(3) 4_665 . . . ? Cd1 O4 C26 C25 -171.7(3) 4_665 . . . ? Cd1 O3 C26 O4 -8.2(4) 4_665 . . . ? Cd1 O3 C26 C25 171.2(2) 4_665 . . . ? C24 C25 C26 O4 7.0(5) . . . . ? C23 C25 C26 O4 -178.0(3) . . . . ? C24 C25 C26 O3 -172.4(3) . . . . ? C23 C25 C26 O3 2.6(5) . . . . ? C24 C25 C26 Cd1 -112.6(15) . . . 4_665 ? C23 C25 C26 Cd1 62.4(17) . . . 4_665 ? Cd1 N3 C27 S1 170(9) . . . . ? Cd1 N4 C28 S2 168(100) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.153 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.085