# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Yue-Peng Cai' _publ_contact_author_email ypcaizsu@yahoo.com.cn _publ_section_title ; Construction of four 3d-4d/4d complexes based on salen-type Schiff base ligands ; loop_ _publ_author_name 'Xue Gong' 'Yingying Ge' 'Mao Fang' 'Zhi-Gang Gu' 'Shengrun Zheng' ; Weishan Li ; 'She-Jun Hu' 'Shu-Bin Li' 'Yue-Peng Cai' data_CCDC-823146(1) _database_code_depnum_ccdc_archive 'CCDC 823146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H25 Cd N5 O11 Zn' _chemical_formula_weight 749.27 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.9306(7) _cell_length_b 18.8619(13) _cell_length_c 15.0246(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.4010(10) _cell_angle_gamma 90.00 _cell_volume 2790.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4260 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.8228 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14328 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5032 _reflns_number_gt 3899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0269P)^2^+0.8714P] 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 5032 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 0.25574(2) 1.044124(12) 0.253832(15) 0.04089(8) Uani 1 1 d . . . Zn1 Zn -0.02961(3) 0.955844(16) 0.22397(2) 0.03403(10) Uani 1 1 d . . . O1 O 0.1866(2) 1.15096(10) 0.12808(14) 0.0478(5) Uani 1 1 d . . . O2 O 0.0512(2) 1.03917(10) 0.16847(13) 0.0414(5) Uani 1 1 d . . . O3 O 0.16051(19) 0.93724(10) 0.27286(14) 0.0412(5) Uani 1 1 d . . . O4 O 0.4146(2) 0.94333(11) 0.33299(16) 0.0530(6) Uani 1 1 d . . . O5 O 0.1280(3) 1.12415(16) 0.3378(2) 0.0891(9) Uani 1 1 d . . . O6 O 0.3126(4) 1.08532(17) 0.4041(2) 0.0975(10) Uani 1 1 d . . . O7 O 0.1893(4) 1.15172(17) 0.4767(2) 0.1155(12) Uani 1 1 d . . . O8 O 0.4673(2) 1.09814(13) 0.24183(17) 0.0625(7) Uani 1 1 d . . . O9 O 0.3942(2) 1.02253(12) 0.14086(15) 0.0572(6) Uani 1 1 d . . . O10 O 0.5859(3) 1.07598(15) 0.1345(2) 0.0859(9) Uani 1 1 d . . . O11 O -0.1042(2) 0.99777(11) 0.33023(14) 0.0496(5) Uani 1 1 d . . . N1 N -0.1860(2) 0.95280(11) 0.12414(16) 0.0343(5) Uani 1 1 d . . . N2 N -0.0741(2) 0.84973(11) 0.22823(15) 0.0340(5) Uani 1 1 d . . . N3 N 0.2092(5) 1.12109(17) 0.4082(2) 0.0734(10) Uani 1 1 d . . . N4 N 0.4852(3) 1.06543(14) 0.1712(2) 0.0503(7) Uani 1 1 d . . . N5 N -0.1890(3) 1.08730(14) 0.40374(19) 0.0523(7) Uani 1 1 d . . . C1 C 0.2720(3) 1.20489(17) 0.0987(2) 0.0583(9) Uani 1 1 d . . . H1A H 0.2867 1.1956 0.0379 0.087 Uiso 1 1 calc R . . H1B H 0.3576 1.2050 0.1366 0.087 Uiso 1 1 calc R . . H1C H 0.2291 1.2503 0.1020 0.087 Uiso 1 1 calc R . . C2 C 0.0669(3) 1.13718(15) 0.07343(19) 0.0367(7) Uani 1 1 d . . . C3 C 0.0160(3) 1.17819(16) 0.0013(2) 0.0468(8) Uani 1 1 d . . . H3 H 0.0618 1.2189 -0.0127 0.056 Uiso 1 1 calc R . . C4 C -0.1043(3) 1.15863(17) -0.0509(2) 0.0498(8) Uani 1 1 d . . . H4 H -0.1384 1.1861 -0.1000 0.060 Uiso 1 1 calc R . . C5 C -0.1716(3) 1.09983(16) -0.0304(2) 0.0439(8) Uani 1 1 d . . . H5 H -0.2513 1.0872 -0.0664 0.053 Uiso 1 1 calc R . . C6 C -0.1246(3) 1.05708(14) 0.04389(19) 0.0348(7) Uani 1 1 d . . . C7 C -0.0024(3) 1.07617(14) 0.09822(19) 0.0327(6) Uani 1 1 d . . . C8 C -0.2049(3) 0.99544(15) 0.05759(19) 0.0362(7) Uani 1 1 d . . . H8 H -0.2776 0.9857 0.0138 0.043 Uiso 1 1 calc R . . C9 C -0.2680(3) 0.89210(14) 0.13158(19) 0.0357(7) Uani 1 1 d . . . C10 C -0.4020(3) 0.88561(16) 0.0924(2) 0.0469(8) Uani 1 1 d . . . H10 H -0.4437 0.9230 0.0592 0.056 Uiso 1 1 calc R . . C11 C -0.4737(3) 0.82400(18) 0.1026(2) 0.0561(9) Uani 1 1 d . . . H11 H -0.5632 0.8198 0.0760 0.067 Uiso 1 1 calc R . . C12 C -0.4119(3) 0.76876(18) 0.1526(2) 0.0587(10) Uani 1 1 d . . . H12 H -0.4598 0.7270 0.1586 0.070 Uiso 1 1 calc R . . C13 C -0.2803(3) 0.77469(16) 0.1936(2) 0.0476(8) Uani 1 1 d . . . H13 H -0.2400 0.7371 0.2271 0.057 Uiso 1 1 calc R . . C14 C -0.2078(3) 0.83633(15) 0.18511(19) 0.0363(7) Uani 1 1 d . . . C15 C 0.0072(3) 0.80126(15) 0.26219(19) 0.0403(7) Uani 1 1 d . . . H15 H -0.0261 0.7552 0.2612 0.048 Uiso 1 1 calc R . . C16 C 0.1461(3) 0.81189(15) 0.30188(19) 0.0367(7) Uani 1 1 d . . . C17 C 0.2166(3) 0.75108(16) 0.3375(2) 0.0496(8) Uani 1 1 d . . . H17 H 0.1711 0.7079 0.3370 0.060 Uiso 1 1 calc R . . C18 C 0.3503(3) 0.75449(17) 0.3729(2) 0.0572(9) Uani 1 1 d . . . H18 H 0.3943 0.7142 0.3975 0.069 Uiso 1 1 calc R . . C19 C 0.4203(3) 0.81810(18) 0.3720(2) 0.0531(9) Uani 1 1 d . . . H19 H 0.5118 0.8201 0.3951 0.064 Uiso 1 1 calc R . . C20 C 0.3559(3) 0.87767(16) 0.3375(2) 0.0403(7) Uani 1 1 d . . . C21 C 0.2165(3) 0.87680(14) 0.30261(18) 0.0338(6) Uani 1 1 d . . . C22 C 0.5548(4) 0.9493(2) 0.3639(3) 0.0938(16) Uani 1 1 d . . . H22A H 0.5707 0.9373 0.4265 0.141 Uiso 1 1 calc R . . H22B H 0.5839 0.9972 0.3558 0.141 Uiso 1 1 calc R . . H22C H 0.6049 0.9176 0.3305 0.141 Uiso 1 1 calc R . . C23 C -0.1555(3) 1.05718(17) 0.3317(2) 0.0495(8) Uani 1 1 d . . . H23 H -0.1712 1.0821 0.2779 0.059 Uiso 1 1 calc R . . C24 C -0.1650(5) 1.0519(2) 0.4899(3) 0.0924(15) Uani 1 1 d . . . H24A H -0.1402 1.0035 0.4812 0.139 Uiso 1 1 calc R . . H24B H -0.2461 1.0534 0.5183 0.139 Uiso 1 1 calc R . . H24C H -0.0927 1.0754 0.5272 0.139 Uiso 1 1 calc R . . C25 C -0.2491(6) 1.1573(2) 0.4025(3) 0.1177(19) Uani 1 1 d . . . H25A H -0.2598 1.1755 0.3423 0.177 Uiso 1 1 calc R . . H25B H -0.1911 1.1883 0.4409 0.177 Uiso 1 1 calc R . . H25C H -0.3363 1.1545 0.4234 0.177 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03964(14) 0.03826(14) 0.04459(15) -0.00303(10) 0.00468(10) -0.00658(10) Zn1 0.03471(19) 0.02969(18) 0.0370(2) 0.00202(15) 0.00186(14) -0.00092(14) O1 0.0464(13) 0.0406(12) 0.0564(14) 0.0100(10) 0.0062(11) -0.0116(10) O2 0.0425(12) 0.0362(11) 0.0432(12) 0.0126(10) -0.0028(9) -0.0052(9) O3 0.0350(11) 0.0316(11) 0.0545(13) 0.0080(9) -0.0042(10) -0.0015(8) O4 0.0362(12) 0.0479(14) 0.0713(16) 0.0061(11) -0.0071(11) -0.0027(10) O5 0.091(2) 0.088(2) 0.087(2) -0.0234(18) 0.0056(18) -0.0204(17) O6 0.130(3) 0.088(2) 0.075(2) -0.0136(17) 0.0165(19) 0.029(2) O7 0.192(4) 0.086(2) 0.075(2) -0.0346(18) 0.041(2) 0.012(2) O8 0.0613(16) 0.0608(16) 0.0660(17) -0.0117(13) 0.0104(13) -0.0126(12) O9 0.0555(15) 0.0581(15) 0.0576(15) -0.0101(12) 0.0059(12) -0.0046(12) O10 0.0645(18) 0.0741(19) 0.130(3) 0.0064(18) 0.0552(18) 0.0022(15) O11 0.0634(14) 0.0429(13) 0.0445(13) -0.0025(10) 0.0146(11) 0.0076(11) N1 0.0333(13) 0.0303(12) 0.0388(14) 0.0004(11) 0.0031(11) 0.0026(10) N2 0.0347(13) 0.0311(13) 0.0363(13) 0.0020(10) 0.0053(11) -0.0013(10) N3 0.114(3) 0.0455(19) 0.064(2) -0.0113(18) 0.024(2) -0.014(2) N4 0.0453(17) 0.0439(16) 0.064(2) 0.0064(15) 0.0149(15) 0.0093(13) N5 0.0554(17) 0.0508(17) 0.0527(18) -0.0128(14) 0.0141(14) 0.0036(14) C1 0.065(2) 0.050(2) 0.062(2) 0.0041(18) 0.0182(18) -0.0223(18) C2 0.0410(17) 0.0327(16) 0.0381(17) 0.0003(13) 0.0116(14) 0.0042(13) C3 0.059(2) 0.0364(18) 0.0481(19) 0.0073(15) 0.0205(17) 0.0029(15) C4 0.063(2) 0.0456(19) 0.0408(19) 0.0120(15) 0.0079(17) 0.0097(17) C5 0.0495(19) 0.0436(18) 0.0380(18) 0.0033(15) 0.0037(15) 0.0069(15) C6 0.0401(16) 0.0318(16) 0.0335(16) -0.0002(12) 0.0077(13) 0.0071(12) C7 0.0390(16) 0.0262(14) 0.0347(16) -0.0017(12) 0.0113(13) 0.0047(12) C8 0.0370(16) 0.0360(16) 0.0345(17) -0.0042(13) 0.0001(13) 0.0040(13) C9 0.0352(16) 0.0335(16) 0.0390(17) -0.0040(13) 0.0074(13) -0.0019(13) C10 0.0387(18) 0.0422(18) 0.058(2) -0.0021(16) -0.0014(15) 0.0027(14) C11 0.0374(18) 0.054(2) 0.075(3) -0.0028(19) -0.0006(17) -0.0073(16) C12 0.049(2) 0.045(2) 0.081(3) 0.0005(19) 0.0040(19) -0.0176(16) C13 0.0449(19) 0.0367(17) 0.060(2) 0.0051(16) 0.0037(16) -0.0026(14) C14 0.0362(16) 0.0340(16) 0.0392(17) -0.0025(13) 0.0070(13) -0.0019(13) C15 0.0473(18) 0.0278(15) 0.0474(19) 0.0033(14) 0.0115(15) -0.0005(13) C16 0.0356(16) 0.0336(16) 0.0412(17) 0.0025(13) 0.0066(13) 0.0053(13) C17 0.052(2) 0.0355(17) 0.063(2) 0.0056(16) 0.0110(17) 0.0070(15) C18 0.051(2) 0.043(2) 0.077(3) 0.0145(18) 0.0066(19) 0.0175(16) C19 0.0384(18) 0.056(2) 0.064(2) 0.0060(18) 0.0029(16) 0.0151(16) C20 0.0378(17) 0.0396(17) 0.0433(18) -0.0011(14) 0.0048(14) 0.0055(14) C21 0.0379(16) 0.0330(15) 0.0311(15) 0.0029(12) 0.0064(13) 0.0044(13) C22 0.044(2) 0.087(3) 0.142(4) 0.027(3) -0.024(3) -0.016(2) C23 0.058(2) 0.046(2) 0.046(2) 0.0029(16) 0.0144(16) -0.0033(16) C24 0.113(4) 0.113(4) 0.052(3) -0.014(2) 0.014(3) 0.036(3) C25 0.173(5) 0.064(3) 0.123(4) -0.016(3) 0.047(4) 0.039(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 O2 2.2601(19) . ? Cd1 O3 2.2606(18) . ? Cd1 O9 2.353(2) . ? Cd1 O8 2.362(2) . ? Cd1 O6 2.386(3) . ? Cd1 O5 2.428(3) . ? Cd1 Zn1 3.2674(4) . ? Zn1 O3 1.9672(19) . ? Zn1 O2 1.9954(19) . ? Zn1 O11 2.007(2) . ? Zn1 N1 2.016(2) . ? Zn1 N2 2.052(2) . ? O1 C2 1.380(3) . ? O1 C1 1.430(3) . ? O2 C7 1.319(3) . ? O3 C21 1.321(3) . ? O4 C20 1.374(3) . ? O4 C22 1.415(4) . ? O5 N3 1.246(4) . ? O6 N3 1.237(4) . ? O7 N3 1.218(4) . ? O8 N4 1.260(3) . ? O9 N4 1.254(3) . ? O10 N4 1.220(3) . ? O11 C23 1.232(4) . ? N1 C8 1.278(3) . ? N1 C9 1.417(3) . ? N2 C15 1.281(3) . ? N2 C14 1.423(3) . ? N5 C23 1.303(4) . ? N5 C25 1.448(5) . ? N5 C24 1.448(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.374(4) . ? C2 C7 1.415(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.351(4) . ? C4 H4 0.9300 . ? C5 C6 1.407(4) . ? C5 H5 0.9300 . ? C6 C7 1.419(4) . ? C6 C8 1.440(4) . ? C8 H8 0.9300 . ? C9 C10 1.389(4) . ? C9 C14 1.409(4) . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C12 C13 1.376(4) . ? C12 H12 0.9300 . ? C13 C14 1.382(4) . ? C13 H13 0.9300 . ? C15 C16 1.444(4) . ? C15 H15 0.9300 . ? C16 C21 1.409(4) . ? C16 C17 1.413(4) . ? C17 C18 1.366(4) . ? C17 H17 0.9300 . ? C18 C19 1.388(4) . ? C18 H18 0.9300 . ? C19 C20 1.362(4) . ? C19 H19 0.9300 . ? C20 C21 1.416(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O3 71.02(7) . . ? O2 Cd1 O9 98.59(8) . . ? O3 Cd1 O9 103.28(8) . . ? O2 Cd1 O8 135.85(8) . . ? O3 Cd1 O8 141.71(8) . . ? O9 Cd1 O8 53.97(8) . . ? O2 Cd1 O6 129.53(10) . . ? O3 Cd1 O6 102.87(10) . . ? O9 Cd1 O6 130.53(11) . . ? O8 Cd1 O6 80.06(11) . . ? O2 Cd1 O5 80.16(9) . . ? O3 Cd1 O5 103.51(9) . . ? O9 Cd1 O5 151.11(10) . . ? O8 Cd1 O5 107.52(9) . . ? O6 Cd1 O5 51.79(11) . . ? O2 Cd1 Zn1 36.95(5) . . ? O3 Cd1 Zn1 36.23(5) . . ? O9 Cd1 Zn1 112.93(6) . . ? O8 Cd1 Zn1 166.72(6) . . ? O6 Cd1 Zn1 113.04(9) . . ? O5 Cd1 Zn1 83.46(7) . . ? O3 Zn1 O2 83.01(8) . . ? O3 Zn1 O11 102.01(9) . . ? O2 Zn1 O11 103.39(9) . . ? O3 Zn1 N1 152.01(9) . . ? O2 Zn1 N1 91.40(9) . . ? O11 Zn1 N1 105.97(9) . . ? O3 Zn1 N2 90.82(8) . . ? O2 Zn1 N2 151.74(9) . . ? O11 Zn1 N2 104.87(9) . . ? N1 Zn1 N2 81.21(9) . . ? O3 Zn1 Cd1 42.78(5) . . ? O2 Zn1 Cd1 42.92(5) . . ? O11 Zn1 Cd1 95.30(6) . . ? N1 Zn1 Cd1 133.48(7) . . ? N2 Zn1 Cd1 132.76(6) . . ? C2 O1 C1 116.8(2) . . ? C7 O2 Zn1 127.48(17) . . ? C7 O2 Cd1 132.28(17) . . ? Zn1 O2 Cd1 100.13(8) . . ? C21 O3 Zn1 128.49(17) . . ? C21 O3 Cd1 130.37(17) . . ? Zn1 O3 Cd1 100.99(8) . . ? C20 O4 C22 117.5(3) . . ? N3 O5 Cd1 95.1(3) . . ? N3 O6 Cd1 97.3(3) . . ? N4 O8 Cd1 94.39(18) . . ? N4 O9 Cd1 94.97(18) . . ? C23 O11 Zn1 124.6(2) . . ? C8 N1 C9 122.8(2) . . ? C8 N1 Zn1 125.8(2) . . ? C9 N1 Zn1 111.07(18) . . ? C15 N2 C14 123.9(2) . . ? C15 N2 Zn1 125.53(19) . . ? C14 N2 Zn1 110.54(17) . . ? O7 N3 O6 121.8(4) . . ? O7 N3 O5 122.5(4) . . ? O6 N3 O5 115.7(4) . . ? O10 N4 O9 122.4(3) . . ? O10 N4 O8 121.0(3) . . ? O9 N4 O8 116.7(3) . . ? C23 N5 C25 122.4(3) . . ? C23 N5 C24 120.8(3) . . ? C25 N5 C24 116.9(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.4(3) . . ? C3 C2 C7 121.6(3) . . ? O1 C2 C7 114.0(2) . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.9(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 C8 116.3(3) . . ? C7 C6 C8 124.8(3) . . ? O2 C7 C2 118.8(2) . . ? O2 C7 C6 123.6(2) . . ? C2 C7 C6 117.6(3) . . ? N1 C8 C6 126.3(3) . . ? N1 C8 H8 116.9 . . ? C6 C8 H8 116.9 . . ? C10 C9 C14 119.2(3) . . ? C10 C9 N1 124.5(3) . . ? C14 C9 N1 116.3(2) . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 119.5(3) . . ? C13 C14 N2 125.0(3) . . ? C9 C14 N2 115.4(2) . . ? N2 C15 C16 125.8(3) . . ? N2 C15 H15 117.1 . . ? C16 C15 H15 117.1 . . ? C21 C16 C17 118.8(3) . . ? C21 C16 C15 124.8(2) . . ? C17 C16 C15 116.4(3) . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 O4 125.5(3) . . ? C19 C20 C21 121.4(3) . . ? O4 C20 C21 113.1(2) . . ? O3 C21 C16 124.1(2) . . ? O3 C21 C20 117.7(3) . . ? C16 C21 C20 118.2(3) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O11 C23 N5 124.1(3) . . ? O11 C23 H23 117.9 . . ? N5 C23 H23 117.9 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 Zn1 O3 154.04(13) . . . . ? O9 Cd1 Zn1 O3 81.05(11) . . . . ? O8 Cd1 Zn1 O3 89.9(3) . . . . ? O6 Cd1 Zn1 O3 -80.15(12) . . . . ? O5 Cd1 Zn1 O3 -123.66(12) . . . . ? O3 Cd1 Zn1 O2 -154.04(13) . . . . ? O9 Cd1 Zn1 O2 -72.99(11) . . . . ? O8 Cd1 Zn1 O2 -64.1(3) . . . . ? O6 Cd1 Zn1 O2 125.81(12) . . . . ? O5 Cd1 Zn1 O2 82.30(12) . . . . ? O2 Cd1 Zn1 O11 -103.99(11) . . . . ? O3 Cd1 Zn1 O11 101.97(11) . . . . ? O9 Cd1 Zn1 O11 -176.98(9) . . . . ? O8 Cd1 Zn1 O11 -168.1(3) . . . . ? O6 Cd1 Zn1 O11 21.82(11) . . . . ? O5 Cd1 Zn1 O11 -21.69(10) . . . . ? O2 Cd1 Zn1 N1 13.95(12) . . . . ? O3 Cd1 Zn1 N1 -140.09(13) . . . . ? O9 Cd1 Zn1 N1 -59.03(11) . . . . ? O8 Cd1 Zn1 N1 -50.2(3) . . . . ? O6 Cd1 Zn1 N1 139.76(13) . . . . ? O5 Cd1 Zn1 N1 96.26(12) . . . . ? O2 Cd1 Zn1 N2 140.11(13) . . . . ? O3 Cd1 Zn1 N2 -13.92(13) . . . . ? O9 Cd1 Zn1 N2 67.13(11) . . . . ? O8 Cd1 Zn1 N2 76.0(3) . . . . ? O6 Cd1 Zn1 N2 -94.07(12) . . . . ? O5 Cd1 Zn1 N2 -137.58(12) . . . . ? O3 Zn1 O2 C7 159.2(2) . . . . ? O11 Zn1 O2 C7 -100.1(2) . . . . ? N1 Zn1 O2 C7 6.7(2) . . . . ? N2 Zn1 O2 C7 80.6(3) . . . . ? Cd1 Zn1 O2 C7 176.6(3) . . . . ? O3 Zn1 O2 Cd1 -17.43(8) . . . . ? O11 Zn1 O2 Cd1 83.30(9) . . . . ? N1 Zn1 O2 Cd1 -169.92(9) . . . . ? N2 Zn1 O2 Cd1 -96.03(17) . . . . ? O3 Cd1 O2 C7 -160.5(3) . . . . ? O9 Cd1 O2 C7 -59.3(2) . . . . ? O8 Cd1 O2 C7 -13.7(3) . . . . ? O6 Cd1 O2 C7 108.3(3) . . . . ? O5 Cd1 O2 C7 91.4(2) . . . . ? Zn1 Cd1 O2 C7 -176.4(3) . . . . ? O3 Cd1 O2 Zn1 15.88(8) . . . . ? O9 Cd1 O2 Zn1 117.05(9) . . . . ? O8 Cd1 O2 Zn1 162.74(9) . . . . ? O6 Cd1 O2 Zn1 -75.36(13) . . . . ? O5 Cd1 O2 Zn1 -92.20(11) . . . . ? O2 Zn1 O3 C21 -158.4(2) . . . . ? O11 Zn1 O3 C21 99.3(2) . . . . ? N1 Zn1 O3 C21 -78.7(3) . . . . ? N2 Zn1 O3 C21 -6.1(2) . . . . ? Cd1 Zn1 O3 C21 -175.9(3) . . . . ? O2 Zn1 O3 Cd1 17.48(8) . . . . ? O11 Zn1 O3 Cd1 -84.79(9) . . . . ? N1 Zn1 O3 Cd1 97.20(18) . . . . ? N2 Zn1 O3 Cd1 169.82(9) . . . . ? O2 Cd1 O3 C21 159.6(3) . . . . ? O9 Cd1 O3 C21 65.0(2) . . . . ? O8 Cd1 O3 C21 17.5(3) . . . . ? O6 Cd1 O3 C21 -72.6(3) . . . . ? O5 Cd1 O3 C21 -125.9(2) . . . . ? Zn1 Cd1 O3 C21 175.8(3) . . . . ? O2 Cd1 O3 Zn1 -16.16(8) . . . . ? O9 Cd1 O3 Zn1 -110.81(9) . . . . ? O8 Cd1 O3 Zn1 -158.24(10) . . . . ? O6 Cd1 O3 Zn1 111.56(11) . . . . ? O5 Cd1 O3 Zn1 58.26(12) . . . . ? O2 Cd1 O5 N3 161.5(2) . . . . ? O3 Cd1 O5 N3 93.9(2) . . . . ? O9 Cd1 O5 N3 -108.5(3) . . . . ? O8 Cd1 O5 N3 -63.3(2) . . . . ? O6 Cd1 O5 N3 -1.9(2) . . . . ? Zn1 Cd1 O5 N3 124.3(2) . . . . ? O2 Cd1 O6 N3 -19.3(3) . . . . ? O3 Cd1 O6 N3 -95.2(2) . . . . ? O9 Cd1 O6 N3 144.4(2) . . . . ? O8 Cd1 O6 N3 123.8(2) . . . . ? O5 Cd1 O6 N3 2.0(2) . . . . ? Zn1 Cd1 O6 N3 -58.5(3) . . . . ? O2 Cd1 O8 N4 -60.8(2) . . . . ? O3 Cd1 O8 N4 62.7(2) . . . . ? O9 Cd1 O8 N4 0.27(16) . . . . ? O6 Cd1 O8 N4 160.89(19) . . . . ? O5 Cd1 O8 N4 -154.66(18) . . . . ? Zn1 Cd1 O8 N4 -9.8(4) . . . . ? O2 Cd1 O9 N4 141.68(17) . . . . ? O3 Cd1 O9 N4 -145.91(17) . . . . ? O8 Cd1 O9 N4 -0.27(16) . . . . ? O6 Cd1 O9 N4 -25.7(2) . . . . ? O5 Cd1 O9 N4 56.5(3) . . . . ? Zn1 Cd1 O9 N4 177.23(15) . . . . ? O3 Zn1 O11 C23 121.2(3) . . . . ? O2 Zn1 O11 C23 35.6(3) . . . . ? N1 Zn1 O11 C23 -59.8(3) . . . . ? N2 Zn1 O11 C23 -144.7(3) . . . . ? Cd1 Zn1 O11 C23 78.4(3) . . . . ? O3 Zn1 N1 C8 -78.6(3) . . . . ? O2 Zn1 N1 C8 -0.9(2) . . . . ? O11 Zn1 N1 C8 103.4(2) . . . . ? N2 Zn1 N1 C8 -153.5(2) . . . . ? Cd1 Zn1 N1 C8 -10.4(3) . . . . ? O3 Zn1 N1 C9 95.5(2) . . . . ? O2 Zn1 N1 C9 173.19(18) . . . . ? O11 Zn1 N1 C9 -82.46(19) . . . . ? N2 Zn1 N1 C9 20.59(18) . . . . ? Cd1 Zn1 N1 C9 163.73(14) . . . . ? O3 Zn1 N2 C15 5.8(2) . . . . ? O2 Zn1 N2 C15 82.5(3) . . . . ? O11 Zn1 N2 C15 -96.8(2) . . . . ? N1 Zn1 N2 C15 158.9(3) . . . . ? Cd1 Zn1 N2 C15 15.2(3) . . . . ? O3 Zn1 N2 C14 -172.19(18) . . . . ? O2 Zn1 N2 C14 -95.5(2) . . . . ? O11 Zn1 N2 C14 85.16(18) . . . . ? N1 Zn1 N2 C14 -19.13(18) . . . . ? Cd1 Zn1 N2 C14 -162.78(14) . . . . ? Cd1 O6 N3 O7 177.3(3) . . . . ? Cd1 O6 N3 O5 -3.3(4) . . . . ? Cd1 O5 N3 O7 -177.3(3) . . . . ? Cd1 O5 N3 O6 3.3(4) . . . . ? Cd1 O9 N4 O10 -178.9(3) . . . . ? Cd1 O9 N4 O8 0.5(3) . . . . ? Cd1 O8 N4 O10 178.9(3) . . . . ? Cd1 O8 N4 O9 -0.5(3) . . . . ? C1 O1 C2 C3 -10.1(4) . . . . ? C1 O1 C2 C7 170.4(3) . . . . ? O1 C2 C3 C4 178.5(3) . . . . ? C7 C2 C3 C4 -2.0(4) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C4 C5 C6 C8 -179.3(3) . . . . ? Zn1 O2 C7 C2 175.08(19) . . . . ? Cd1 O2 C7 C2 -9.4(4) . . . . ? Zn1 O2 C7 C6 -6.9(4) . . . . ? Cd1 O2 C7 C6 168.64(19) . . . . ? C3 C2 C7 O2 -179.6(3) . . . . ? O1 C2 C7 O2 -0.1(4) . . . . ? C3 C2 C7 C6 2.2(4) . . . . ? O1 C2 C7 C6 -178.2(2) . . . . ? C5 C6 C7 O2 -179.0(3) . . . . ? C8 C6 C7 O2 -0.4(4) . . . . ? C5 C6 C7 C2 -0.9(4) . . . . ? C8 C6 C7 C2 177.7(3) . . . . ? C9 N1 C8 C6 -178.4(3) . . . . ? Zn1 N1 C8 C6 -4.9(4) . . . . ? C5 C6 C8 N1 -174.5(3) . . . . ? C7 C6 C8 N1 6.8(5) . . . . ? C8 N1 C9 C10 -26.7(4) . . . . ? Zn1 N1 C9 C10 159.0(2) . . . . ? C8 N1 C9 C14 155.4(3) . . . . ? Zn1 N1 C9 C14 -18.9(3) . . . . ? C14 C9 C10 C11 -2.8(5) . . . . ? N1 C9 C10 C11 179.4(3) . . . . ? C9 C10 C11 C12 0.4(5) . . . . ? C10 C11 C12 C13 1.1(6) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? C12 C13 C14 C9 -2.2(5) . . . . ? C12 C13 C14 N2 176.6(3) . . . . ? C10 C9 C14 C13 3.7(4) . . . . ? N1 C9 C14 C13 -178.3(3) . . . . ? C10 C9 C14 N2 -175.2(3) . . . . ? N1 C9 C14 N2 2.8(4) . . . . ? C15 N2 C14 C13 17.5(5) . . . . ? Zn1 N2 C14 C13 -164.4(3) . . . . ? C15 N2 C14 C9 -163.6(3) . . . . ? Zn1 N2 C14 C9 14.4(3) . . . . ? C14 N2 C15 C16 176.2(3) . . . . ? Zn1 N2 C15 C16 -1.5(4) . . . . ? N2 C15 C16 C21 -5.4(5) . . . . ? N2 C15 C16 C17 178.4(3) . . . . ? C21 C16 C17 C18 0.5(5) . . . . ? C15 C16 C17 C18 176.9(3) . . . . ? C16 C17 C18 C19 -1.7(5) . . . . ? C17 C18 C19 C20 1.2(5) . . . . ? C18 C19 C20 O4 -180.0(3) . . . . ? C18 C19 C20 C21 0.7(5) . . . . ? C22 O4 C20 C19 2.3(5) . . . . ? C22 O4 C20 C21 -178.3(3) . . . . ? Zn1 O3 C21 C16 1.9(4) . . . . ? Cd1 O3 C21 C16 -172.8(2) . . . . ? Zn1 O3 C21 C20 -177.99(19) . . . . ? Cd1 O3 C21 C20 7.3(4) . . . . ? C17 C16 C21 O3 -178.6(3) . . . . ? C15 C16 C21 O3 5.3(5) . . . . ? C17 C16 C21 C20 1.3(4) . . . . ? C15 C16 C21 C20 -174.8(3) . . . . ? C19 C20 C21 O3 178.0(3) . . . . ? O4 C20 C21 O3 -1.5(4) . . . . ? C19 C20 C21 C16 -1.9(4) . . . . ? O4 C20 C21 C16 178.7(3) . . . . ? Zn1 O11 C23 N5 -171.5(2) . . . . ? C25 N5 C23 O11 -180.0(4) . . . . ? C24 N5 C23 O11 1.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.308 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.060 ################# END ###################### data_CCDC823147(4) _database_code_depnum_ccdc_archive 'CCDC 823147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 Cd2 Cl2 N6 O8' _chemical_formula_weight 956.42 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.6799(12) _cell_length_b 10.6208(8) _cell_length_c 21.4547(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.3120(10) _cell_angle_gamma 90.00 _cell_volume 3797.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3434 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 23.11 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7603 _exptl_absorpt_correction_T_max 0.8686 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18537 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 24.85 _reflns_number_total 6566 _reflns_number_gt 4690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0363P)^2^+3.5809P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6566 _refine_ls_number_parameters 487 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _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 0.00366(2) 0.22559(4) 0.177492(16) 0.03623(12) Uani 1 1 d . . . Cd2 Cd 0.00786(2) 0.21178(4) 0.342914(17) 0.04041(13) Uani 1 1 d . . . Cl1 Cl -0.07634(11) 0.33702(19) 0.41184(9) 0.0860(6) Uani 1 1 d . . . Cl2 Cl 0.09237(9) 0.04413(16) 0.39502(7) 0.0643(4) Uani 1 1 d . . . O1 O -0.1040(2) 0.0501(4) 0.35671(16) 0.0553(10) Uani 1 1 d . . . O2 O -0.07499(18) 0.1791(3) 0.25756(14) 0.0388(8) Uani 1 1 d . . . O3 O 0.1110(2) 0.3825(4) 0.36962(16) 0.0575(11) Uani 1 1 d . . . O4 O 0.08274(19) 0.2709(3) 0.26324(15) 0.0400(8) Uani 1 1 d . . . O5 O 0.0271(3) 0.0051(4) 0.1707(2) 0.0649(11) Uani 1 1 d . . . O6 O -0.0148(2) 0.4491(4) 0.1674(2) 0.0634(11) Uani 1 1 d . . . O7 O 0.5940(3) 0.1353(5) 0.1094(3) 0.1008(18) Uani 1 1 d D . . H7A H 0.561(4) 0.174(6) 0.086(4) 0.151 Uiso 1 1 d D . . H7B H 0.587(5) 0.0573(18) 0.113(4) 0.151 Uiso 1 1 d D . . O8 O 0.4690(5) 0.2693(5) 0.0552(3) 0.115(2) Uani 1 1 d D . . H8A H 0.450(6) 0.339(4) 0.066(4) 0.172 Uiso 1 1 d D . . H8B H 0.478(7) 0.262(8) 0.0169(14) 0.172 Uiso 1 1 d D . . N1 N -0.2401(2) 0.1803(4) 0.10075(19) 0.0410(10) Uani 1 1 d . . . H1 H -0.2884 0.1536 0.1041 0.049 Uiso 1 1 calc R . . N2 N -0.1113(2) 0.2118(4) 0.12298(18) 0.0390(10) Uani 1 1 d . . . N3 N 0.1184(2) 0.2523(4) 0.13178(18) 0.0370(10) Uani 1 1 d . . . N4 N 0.2373(2) 0.3290(4) 0.11078(19) 0.0435(11) Uani 1 1 d . . . H4 H 0.2811 0.3714 0.1149 0.052 Uiso 1 1 calc R . . N5 N 0.0744(3) -0.1721(5) 0.2188(3) 0.0661(15) Uani 1 1 d . . . N6 N -0.0871(3) 0.6246(5) 0.1777(3) 0.0782(17) Uani 1 1 d . . . C1 C -0.1234(4) -0.0026(6) 0.4152(3) 0.0648(17) Uani 1 1 d . . . H1A H -0.1749 0.0278 0.4267 0.097 Uiso 1 1 calc R . . H1B H -0.0835 0.0216 0.4464 0.097 Uiso 1 1 calc R . . H1C H -0.1249 -0.0927 0.4119 0.097 Uiso 1 1 calc R . . C2 C -0.1557(3) 0.0309(5) 0.3065(2) 0.0432(13) Uani 1 1 d . . . C3 C -0.2190(3) -0.0507(5) 0.3065(3) 0.0491(14) Uani 1 1 d . . . H3 H -0.2299 -0.0954 0.3425 0.059 Uiso 1 1 calc R . . C4 C -0.2671(3) -0.0668(5) 0.2524(3) 0.0506(15) Uani 1 1 d . . . H4A H -0.3098 -0.1231 0.2519 0.061 Uiso 1 1 calc R . . C5 C -0.2512(3) 0.0005(5) 0.2002(3) 0.0431(13) Uani 1 1 d . . . H5 H -0.2834 -0.0109 0.1642 0.052 Uiso 1 1 calc R . . C6 C -0.1876(3) 0.0861(5) 0.1995(2) 0.0344(11) Uani 1 1 d . . . C7 C -0.1366(3) 0.1016(5) 0.2531(2) 0.0350(11) Uani 1 1 d . . . C8 C -0.1774(3) 0.1596(5) 0.1426(2) 0.0352(11) Uani 1 1 d . . . C9 C -0.2124(3) 0.2511(5) 0.0523(2) 0.0425(13) Uani 1 1 d . . . C10 C -0.2497(3) 0.3016(6) -0.0009(3) 0.0568(16) Uani 1 1 d . . . H10 H -0.3040 0.2889 -0.0104 0.068 Uiso 1 1 calc R . . C11 C -0.2027(4) 0.3711(6) -0.0388(3) 0.0668(18) Uani 1 1 d . . . H11 H -0.2259 0.4059 -0.0750 0.080 Uiso 1 1 calc R . . C12 C -0.1221(4) 0.3915(7) -0.0253(3) 0.0705(19) Uani 1 1 d . . . H12 H -0.0925 0.4406 -0.0520 0.085 Uiso 1 1 calc R . . C13 C -0.0851(3) 0.3400(6) 0.0271(3) 0.0575(16) Uani 1 1 d . . . H13 H -0.0305 0.3513 0.0359 0.069 Uiso 1 1 calc R . . C14 C -0.1319(3) 0.2706(5) 0.0666(2) 0.0433(13) Uani 1 1 d . . . C15 C 0.1212(4) 0.4481(6) 0.4274(3) 0.0713(19) Uani 1 1 d . . . H15A H 0.1757 0.4393 0.4430 0.107 Uiso 1 1 calc R . . H15B H 0.0856 0.4135 0.4571 0.107 Uiso 1 1 calc R . . H15C H 0.1092 0.5357 0.4211 0.107 Uiso 1 1 calc R . . C16 C 0.1582(3) 0.4189(5) 0.3217(2) 0.0411(13) Uani 1 1 d . . . C17 C 0.2185(3) 0.5078(5) 0.3276(3) 0.0491(14) Uani 1 1 d . . . H17 H 0.2299 0.5461 0.3659 0.059 Uiso 1 1 calc R . . C18 C 0.2616(3) 0.5395(5) 0.2764(3) 0.0544(15) Uani 1 1 d . . . H18 H 0.3018 0.6000 0.2802 0.065 Uiso 1 1 calc R . . C19 C 0.2458(3) 0.4833(5) 0.2205(3) 0.0471(14) Uani 1 1 d . . . H19 H 0.2749 0.5072 0.1863 0.057 Uiso 1 1 calc R . . C20 C 0.1865(3) 0.3899(5) 0.2127(2) 0.0359(12) Uani 1 1 d . . . C21 C 0.1394(3) 0.3559(5) 0.2642(2) 0.0363(12) Uani 1 1 d . . . C22 C 0.1780(3) 0.3254(5) 0.1526(2) 0.0373(12) Uani 1 1 d . . . C23 C 0.1412(3) 0.2049(5) 0.0746(2) 0.0402(12) Uani 1 1 d . . . C24 C 0.1028(4) 0.1195(6) 0.0350(2) 0.0555(16) Uani 1 1 d . . . H24 H 0.0527 0.0871 0.0437 0.067 Uiso 1 1 calc R . . C25 C 0.1413(4) 0.0841(6) -0.0178(3) 0.0651(17) Uani 1 1 d . . . H25 H 0.1175 0.0258 -0.0451 0.078 Uiso 1 1 calc R . . C26 C 0.2153(4) 0.1349(7) -0.0303(3) 0.0686(19) Uani 1 1 d . . . H26 H 0.2399 0.1099 -0.0664 0.082 Uiso 1 1 calc R . . C27 C 0.2537(3) 0.2197(6) 0.0077(3) 0.0570(16) Uani 1 1 d . . . H27 H 0.3033 0.2532 -0.0017 0.068 Uiso 1 1 calc R . . C28 C 0.2154(3) 0.2539(5) 0.0612(2) 0.0429(13) Uani 1 1 d . . . C29 C 0.0378(3) -0.0626(6) 0.2173(3) 0.0629(17) Uani 1 1 d . . . H29 H 0.0182 -0.0332 0.2546 0.076 Uiso 1 1 calc R . . C30 C 0.1117(5) -0.2221(7) 0.1666(4) 0.114(3) Uani 1 1 d . . . H30A H 0.0990 -0.1708 0.1307 0.171 Uiso 1 1 calc R . . H30B H 0.0928 -0.3064 0.1590 0.171 Uiso 1 1 calc R . . H30C H 0.1688 -0.2234 0.1745 0.171 Uiso 1 1 calc R . . C31 C 0.0853(5) -0.2429(7) 0.2774(4) 0.115(3) Uani 1 1 d . . . H31A H 0.0579 -0.2004 0.3098 0.173 Uiso 1 1 calc R . . H31B H 0.1415 -0.2483 0.2887 0.173 Uiso 1 1 calc R . . H31C H 0.0637 -0.3261 0.2720 0.173 Uiso 1 1 calc R . . C32 C -0.0492(3) 0.5262(6) 0.1992(3) 0.0619(17) Uani 1 1 d . . . H32 H -0.0480 0.5132 0.2421 0.074 Uiso 1 1 calc R . . C33 C -0.0950(6) 0.6462(10) 0.1118(5) 0.152(4) Uani 1 1 d . . . H33A H -0.0583 0.5927 0.0908 0.227 Uiso 1 1 calc R . . H33B H -0.0830 0.7327 0.1031 0.227 Uiso 1 1 calc R . . H33C H -0.1489 0.6276 0.0973 0.227 Uiso 1 1 calc R . . C34 C -0.1281(5) 0.7113(7) 0.2177(5) 0.136(4) Uani 1 1 d . . . H34A H -0.1849 0.7064 0.2088 0.203 Uiso 1 1 calc R . . H34B H -0.1098 0.7955 0.2103 0.203 Uiso 1 1 calc R . . H34C H -0.1167 0.6893 0.2606 0.203 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02763(19) 0.0425(2) 0.0387(2) 0.00070(17) 0.00217(15) -0.00390(17) Cd2 0.0394(2) 0.0455(3) 0.0366(2) -0.00185(18) 0.00391(16) -0.00263(18) Cl1 0.0780(12) 0.0851(14) 0.0975(14) -0.0163(11) 0.0352(10) 0.0037(11) Cl2 0.0499(9) 0.0703(11) 0.0722(10) 0.0126(8) -0.0046(7) 0.0055(8) O1 0.053(2) 0.066(3) 0.046(2) 0.016(2) -0.0031(19) -0.018(2) O2 0.0303(18) 0.048(2) 0.0383(19) 0.0002(16) 0.0004(14) -0.0123(16) O3 0.067(3) 0.063(3) 0.043(2) -0.016(2) 0.0060(19) -0.021(2) O4 0.0334(18) 0.047(2) 0.0402(19) -0.0029(16) 0.0050(15) -0.0106(17) O5 0.074(3) 0.050(3) 0.071(3) 0.005(2) 0.008(2) -0.001(2) O6 0.058(3) 0.044(3) 0.088(3) 0.000(2) 0.002(2) 0.013(2) O7 0.052(3) 0.081(4) 0.166(5) 0.021(4) -0.029(3) -0.007(3) O8 0.128(5) 0.082(4) 0.129(5) 0.000(4) -0.048(4) 0.013(4) N1 0.028(2) 0.044(3) 0.050(3) -0.004(2) -0.005(2) 0.004(2) N2 0.036(2) 0.044(3) 0.037(2) 0.003(2) 0.0001(19) -0.001(2) N3 0.030(2) 0.043(3) 0.038(2) -0.0011(19) 0.0050(18) -0.002(2) N4 0.033(2) 0.050(3) 0.048(3) 0.010(2) 0.008(2) -0.003(2) N5 0.056(3) 0.040(3) 0.102(4) -0.016(3) -0.005(3) 0.003(3) N6 0.065(4) 0.040(3) 0.132(5) 0.008(4) 0.023(4) 0.007(3) C1 0.069(4) 0.071(5) 0.055(4) 0.015(3) 0.005(3) -0.010(3) C2 0.036(3) 0.040(3) 0.053(3) 0.006(3) -0.001(3) -0.004(2) C3 0.049(3) 0.040(3) 0.059(4) 0.014(3) 0.010(3) -0.007(3) C4 0.036(3) 0.037(3) 0.079(4) -0.002(3) 0.004(3) -0.010(3) C5 0.034(3) 0.038(3) 0.058(4) -0.003(3) 0.002(2) -0.002(2) C6 0.030(3) 0.031(3) 0.042(3) -0.002(2) 0.002(2) 0.003(2) C7 0.034(3) 0.029(3) 0.043(3) -0.001(2) 0.008(2) 0.004(2) C8 0.031(3) 0.030(3) 0.044(3) -0.005(2) -0.003(2) 0.003(2) C9 0.046(3) 0.040(3) 0.041(3) -0.006(2) -0.007(2) 0.007(3) C10 0.053(4) 0.065(4) 0.051(4) -0.008(3) -0.016(3) 0.008(3) C11 0.077(5) 0.074(5) 0.048(4) 0.005(3) -0.008(3) 0.016(4) C12 0.078(5) 0.081(5) 0.053(4) 0.016(4) 0.006(3) -0.005(4) C13 0.052(4) 0.066(4) 0.054(4) 0.009(3) 0.000(3) -0.008(3) C14 0.042(3) 0.047(3) 0.041(3) -0.004(3) 0.001(2) -0.001(3) C15 0.079(5) 0.082(5) 0.052(4) -0.021(4) -0.003(3) -0.010(4) C16 0.038(3) 0.036(3) 0.048(3) -0.003(3) -0.004(2) 0.000(2) C17 0.047(3) 0.040(3) 0.060(4) -0.017(3) -0.006(3) -0.007(3) C18 0.041(3) 0.038(4) 0.084(4) -0.013(3) -0.003(3) -0.012(3) C19 0.038(3) 0.038(3) 0.066(4) 0.003(3) 0.004(3) -0.002(3) C20 0.024(2) 0.032(3) 0.051(3) 0.005(2) -0.002(2) -0.002(2) C21 0.036(3) 0.030(3) 0.043(3) 0.000(2) -0.004(2) -0.001(2) C22 0.033(3) 0.039(3) 0.040(3) 0.010(2) 0.002(2) 0.004(2) C23 0.039(3) 0.041(3) 0.042(3) 0.000(3) 0.009(2) 0.005(2) C24 0.061(4) 0.058(4) 0.048(3) -0.009(3) 0.009(3) -0.009(3) C25 0.083(5) 0.060(4) 0.053(4) -0.014(3) 0.007(3) 0.002(4) C26 0.078(5) 0.081(5) 0.048(4) -0.007(4) 0.019(3) 0.018(4) C27 0.051(4) 0.067(5) 0.054(4) 0.014(3) 0.020(3) 0.007(3) C28 0.040(3) 0.048(4) 0.040(3) 0.013(3) 0.007(2) 0.008(3) C29 0.055(4) 0.051(4) 0.083(5) -0.021(4) -0.002(3) -0.002(3) C30 0.096(6) 0.084(6) 0.166(9) -0.051(6) 0.048(6) -0.009(5) C31 0.145(8) 0.072(6) 0.124(8) 0.013(5) -0.056(6) 0.007(5) C32 0.050(4) 0.043(4) 0.093(5) 0.007(4) 0.009(3) -0.008(3) C33 0.149(9) 0.129(9) 0.175(11) 0.056(8) -0.023(8) 0.055(8) C34 0.094(6) 0.052(5) 0.267(13) -0.031(6) 0.086(7) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.204(4) . ? Cd1 N2 2.210(4) . ? Cd1 O2 2.258(3) . ? Cd1 O4 2.272(3) . ? Cd1 O5 2.379(4) . ? Cd1 O6 2.403(4) . ? Cd2 O4 2.247(3) . ? Cd2 O2 2.276(3) . ? Cd2 Cl1 2.4690(17) . ? Cd2 Cl2 2.5060(16) . ? Cd2 O3 2.549(4) . ? Cd2 O1 2.561(4) . ? O1 C2 1.368(6) . ? O1 C1 1.423(6) . ? O2 C7 1.317(5) . ? O3 C16 1.375(6) . ? O3 C15 1.427(6) . ? O4 C21 1.306(5) . ? O5 C29 1.238(7) . ? O6 C32 1.224(7) . ? O7 H7A 0.838(10) . ? O7 H7B 0.842(10) . ? O8 H8A 0.843(10) . ? O8 H8B 0.845(10) . ? N1 C8 1.368(6) . ? N1 C9 1.379(6) . ? N1 H1 0.8600 . ? N2 C8 1.319(6) . ? N2 C14 1.392(6) . ? N3 C22 1.325(6) . ? N3 C23 1.393(6) . ? N4 C22 1.363(6) . ? N4 C28 1.368(6) . ? N4 H4 0.8600 . ? N5 C29 1.313(7) . ? N5 C30 1.407(8) . ? N5 C31 1.471(9) . ? N6 C32 1.297(8) . ? N6 C33 1.434(10) . ? N6 C34 1.448(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.365(7) . ? C2 C7 1.416(7) . ? C3 C4 1.396(7) . ? C3 H3 0.9300 . ? C4 C5 1.363(7) . ? C4 H4A 0.9300 . ? C5 C6 1.397(7) . ? C5 H5 0.9300 . ? C6 C7 1.413(6) . ? C6 C8 1.465(7) . ? C9 C14 1.381(7) . ? C9 C10 1.386(7) . ? C10 C11 1.367(8) . ? C10 H10 0.9300 . ? C11 C12 1.381(8) . ? C11 H11 0.9300 . ? C12 C13 1.376(8) . ? C12 H12 0.9300 . ? C13 C14 1.387(7) . ? C13 H13 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.381(7) . ? C16 C21 1.427(6) . ? C17 C18 1.379(7) . ? C17 H17 0.9300 . ? C18 C19 1.356(7) . ? C18 H18 0.9300 . ? C19 C20 1.406(7) . ? C19 H19 0.9300 . ? C20 C21 1.429(6) . ? C20 C22 1.461(7) . ? C23 C24 1.381(7) . ? C23 C28 1.384(7) . ? C24 C25 1.377(7) . ? C24 H24 0.9300 . ? C25 C26 1.384(8) . ? C25 H25 0.9300 . ? C26 C27 1.359(8) . ? C26 H26 0.9300 . ? C27 C28 1.384(7) . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N2 121.57(14) . . ? N3 Cd1 O2 155.29(13) . . ? N2 Cd1 O2 82.52(13) . . ? N3 Cd1 O4 81.18(13) . . ? N2 Cd1 O4 154.91(13) . . ? O2 Cd1 O4 76.49(11) . . ? N3 Cd1 O5 87.23(14) . . ? N2 Cd1 O5 92.52(15) . . ? O2 Cd1 O5 86.17(13) . . ? O4 Cd1 O5 99.57(14) . . ? N3 Cd1 O6 86.72(14) . . ? N2 Cd1 O6 84.97(14) . . ? O2 Cd1 O6 102.05(13) . . ? O4 Cd1 O6 86.10(13) . . ? O5 Cd1 O6 170.98(15) . . ? O4 Cd2 O2 76.62(11) . . ? O4 Cd2 Cl1 130.71(10) . . ? O2 Cd2 Cl1 102.86(10) . . ? O4 Cd2 Cl2 102.59(9) . . ? O2 Cd2 Cl2 124.25(10) . . ? Cl1 Cd2 Cl2 116.04(6) . . ? O4 Cd2 O3 65.25(11) . . ? O2 Cd2 O3 132.21(12) . . ? Cl1 Cd2 O3 82.94(10) . . ? Cl2 Cd2 O3 92.46(10) . . ? O4 Cd2 O1 134.84(12) . . ? O2 Cd2 O1 64.48(11) . . ? Cl1 Cd2 O1 81.80(10) . . ? Cl2 Cd2 O1 82.61(9) . . ? O3 Cd2 O1 159.89(11) . . ? C2 O1 C1 118.5(4) . . ? C2 O1 Cd2 116.6(3) . . ? C1 O1 Cd2 123.9(3) . . ? C7 O2 Cd1 123.9(3) . . ? C7 O2 Cd2 126.9(3) . . ? Cd1 O2 Cd2 103.07(12) . . ? C16 O3 C15 117.4(4) . . ? C16 O3 Cd2 115.7(3) . . ? C15 O3 Cd2 126.8(3) . . ? C21 O4 Cd2 127.2(3) . . ? C21 O4 Cd1 123.7(3) . . ? Cd2 O4 Cd1 103.56(12) . . ? C29 O5 Cd1 122.8(4) . . ? C32 O6 Cd1 132.2(4) . . ? H7A O7 H7B 117(2) . . ? H8A O8 H8B 116(2) . . ? C8 N1 C9 108.2(4) . . ? C8 N1 H1 125.9 . . ? C9 N1 H1 125.9 . . ? C8 N2 C14 106.6(4) . . ? C8 N2 Cd1 125.3(3) . . ? C14 N2 Cd1 127.5(3) . . ? C22 N3 C23 106.4(4) . . ? C22 N3 Cd1 125.3(3) . . ? C23 N3 Cd1 128.1(3) . . ? C22 N4 C28 108.6(4) . . ? C22 N4 H4 125.7 . . ? C28 N4 H4 125.7 . . ? C29 N5 C30 122.4(7) . . ? C29 N5 C31 121.0(6) . . ? C30 N5 C31 116.3(6) . . ? C32 N6 C33 120.3(7) . . ? C32 N6 C34 122.4(8) . . ? C33 N6 C34 117.2(7) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 123.9(5) . . ? C3 C2 C7 122.4(5) . . ? O1 C2 C7 113.7(4) . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 120.0(5) . . ? C5 C6 C8 118.0(4) . . ? C7 C6 C8 122.0(4) . . ? O2 C7 C6 125.0(4) . . ? O2 C7 C2 118.3(4) . . ? C6 C7 C2 116.7(5) . . ? N2 C8 N1 110.5(4) . . ? N2 C8 C6 128.1(4) . . ? N1 C8 C6 121.4(4) . . ? N1 C9 C14 105.4(4) . . ? N1 C9 C10 132.8(5) . . ? C14 C9 C10 121.8(5) . . ? C11 C10 C9 116.6(5) . . ? C11 C10 H10 121.7 . . ? C9 C10 H10 121.7 . . ? C10 C11 C12 122.6(6) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 120.6(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 117.8(5) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C9 C14 C13 120.7(5) . . ? C9 C14 N2 109.3(4) . . ? C13 C14 N2 130.0(5) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 C17 124.1(5) . . ? O3 C16 C21 113.7(4) . . ? C17 C16 C21 122.2(5) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 121.7(5) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 119.5(5) . . ? C19 C20 C22 118.6(5) . . ? C21 C20 C22 121.8(4) . . ? O4 C21 C16 118.1(4) . . ? O4 C21 C20 125.6(4) . . ? C16 C21 C20 116.2(4) . . ? N3 C22 N4 110.4(4) . . ? N3 C22 C20 128.2(4) . . ? N4 C22 C20 121.4(4) . . ? C24 C23 C28 121.0(5) . . ? C24 C23 N3 130.0(5) . . ? C28 C23 N3 108.9(5) . . ? C25 C24 C23 117.7(5) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 120.1(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 123.0(6) . . ? C27 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C26 C27 C28 116.7(5) . . ? C26 C27 H27 121.7 . . ? C28 C27 H27 121.7 . . ? N4 C28 C27 132.8(5) . . ? N4 C28 C23 105.7(4) . . ? C27 C28 C23 121.4(5) . . ? O5 C29 N5 125.8(7) . . ? O5 C29 H29 117.1 . . ? N5 C29 H29 117.1 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 N6 124.9(7) . . ? O6 C32 H32 117.5 . . ? N6 C32 H32 117.5 . . ? N6 C33 H33A 109.5 . . ? N6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 H34A 109.5 . . ? N6 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N6 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cd2 O1 C2 -34.7(4) . . . . ? O2 Cd2 O1 C2 -1.4(3) . . . . ? Cl1 Cd2 O1 C2 107.1(4) . . . . ? Cl2 Cd2 O1 C2 -135.1(4) . . . . ? O3 Cd2 O1 C2 148.1(4) . . . . ? O4 Cd2 O1 C1 156.7(4) . . . . ? O2 Cd2 O1 C1 -170.1(5) . . . . ? Cl1 Cd2 O1 C1 -61.5(4) . . . . ? Cl2 Cd2 O1 C1 56.2(4) . . . . ? O3 Cd2 O1 C1 -20.6(6) . . . . ? N3 Cd1 O2 C7 -131.8(4) . . . . ? N2 Cd1 O2 C7 36.1(4) . . . . ? O4 Cd1 O2 C7 -157.7(4) . . . . ? O5 Cd1 O2 C7 -56.9(4) . . . . ? O6 Cd1 O2 C7 119.3(4) . . . . ? N3 Cd1 O2 Cd2 22.2(4) . . . . ? N2 Cd1 O2 Cd2 -169.96(16) . . . . ? O4 Cd1 O2 Cd2 -3.81(12) . . . . ? O5 Cd1 O2 Cd2 96.99(15) . . . . ? O6 Cd1 O2 Cd2 -86.76(15) . . . . ? O4 Cd2 O2 C7 156.7(4) . . . . ? Cl1 Cd2 O2 C7 -74.0(4) . . . . ? Cl2 Cd2 O2 C7 60.4(4) . . . . ? O3 Cd2 O2 C7 -166.1(3) . . . . ? O1 Cd2 O2 C7 0.3(3) . . . . ? O4 Cd2 O2 Cd1 3.85(13) . . . . ? Cl1 Cd2 O2 Cd1 133.15(11) . . . . ? Cl2 Cd2 O2 Cd1 -92.41(13) . . . . ? O3 Cd2 O2 Cd1 41.0(2) . . . . ? O1 Cd2 O2 Cd1 -152.58(18) . . . . ? O4 Cd2 O3 C16 -0.9(3) . . . . ? O2 Cd2 O3 C16 -41.2(4) . . . . ? Cl1 Cd2 O3 C16 -142.2(3) . . . . ? Cl2 Cd2 O3 C16 101.9(3) . . . . ? O1 Cd2 O3 C16 177.0(3) . . . . ? O4 Cd2 O3 C15 175.3(5) . . . . ? O2 Cd2 O3 C15 134.9(4) . . . . ? Cl1 Cd2 O3 C15 34.0(4) . . . . ? Cl2 Cd2 O3 C15 -82.0(4) . . . . ? O1 Cd2 O3 C15 -6.9(7) . . . . ? O2 Cd2 O4 C21 150.4(4) . . . . ? Cl1 Cd2 O4 C21 54.8(4) . . . . ? Cl2 Cd2 O4 C21 -87.0(4) . . . . ? O3 Cd2 O4 C21 -0.1(4) . . . . ? O1 Cd2 O4 C21 -179.1(3) . . . . ? O2 Cd2 O4 Cd1 -3.83(12) . . . . ? Cl1 Cd2 O4 Cd1 -99.41(14) . . . . ? Cl2 Cd2 O4 Cd1 118.83(11) . . . . ? O3 Cd2 O4 Cd1 -154.30(18) . . . . ? O1 Cd2 O4 Cd1 26.8(2) . . . . ? N3 Cd1 O4 C21 39.2(4) . . . . ? N2 Cd1 O4 C21 -117.4(4) . . . . ? O2 Cd1 O4 C21 -151.5(4) . . . . ? O5 Cd1 O4 C21 124.8(4) . . . . ? O6 Cd1 O4 C21 -48.1(4) . . . . ? N3 Cd1 O4 Cd2 -165.46(17) . . . . ? N2 Cd1 O4 Cd2 37.9(4) . . . . ? O2 Cd1 O4 Cd2 3.87(13) . . . . ? O5 Cd1 O4 Cd2 -79.80(15) . . . . ? O6 Cd1 O4 Cd2 107.26(15) . . . . ? N3 Cd1 O5 C29 115.4(5) . . . . ? N2 Cd1 O5 C29 -123.1(5) . . . . ? O2 Cd1 O5 C29 -40.8(5) . . . . ? O4 Cd1 O5 C29 34.8(5) . . . . ? O6 Cd1 O5 C29 163.3(8) . . . . ? N3 Cd1 O6 C32 -149.2(6) . . . . ? N2 Cd1 O6 C32 88.7(5) . . . . ? O2 Cd1 O6 C32 7.4(6) . . . . ? O4 Cd1 O6 C32 -67.9(5) . . . . ? O5 Cd1 O6 C32 162.8(8) . . . . ? N3 Cd1 N2 C8 158.4(4) . . . . ? O2 Cd1 N2 C8 -15.7(4) . . . . ? O4 Cd1 N2 C8 -49.0(6) . . . . ? O5 Cd1 N2 C8 70.1(4) . . . . ? O6 Cd1 N2 C8 -118.6(4) . . . . ? N3 Cd1 N2 C14 -31.7(5) . . . . ? O2 Cd1 N2 C14 154.2(4) . . . . ? O4 Cd1 N2 C14 120.9(4) . . . . ? O5 Cd1 N2 C14 -120.0(4) . . . . ? O6 Cd1 N2 C14 51.3(4) . . . . ? N2 Cd1 N3 C22 140.7(4) . . . . ? O2 Cd1 N3 C22 -53.5(6) . . . . ? O4 Cd1 N3 C22 -27.9(4) . . . . ? O5 Cd1 N3 C22 -128.1(4) . . . . ? O6 Cd1 N3 C22 58.6(4) . . . . ? N2 Cd1 N3 C23 -34.5(5) . . . . ? O2 Cd1 N3 C23 131.3(4) . . . . ? O4 Cd1 N3 C23 156.9(4) . . . . ? O5 Cd1 N3 C23 56.7(4) . . . . ? O6 Cd1 N3 C23 -116.6(4) . . . . ? C1 O1 C2 C3 -9.9(8) . . . . ? Cd2 O1 C2 C3 -179.2(4) . . . . ? C1 O1 C2 C7 171.6(5) . . . . ? Cd2 O1 C2 C7 2.4(6) . . . . ? O1 C2 C3 C4 -178.1(5) . . . . ? C7 C2 C3 C4 0.3(8) . . . . ? C2 C3 C4 C5 -0.9(8) . . . . ? C3 C4 C5 C6 -0.2(8) . . . . ? C4 C5 C6 C7 2.0(8) . . . . ? C4 C5 C6 C8 -176.7(5) . . . . ? Cd1 O2 C7 C6 -33.8(6) . . . . ? Cd2 O2 C7 C6 178.6(3) . . . . ? Cd1 O2 C7 C2 148.5(4) . . . . ? Cd2 O2 C7 C2 0.9(6) . . . . ? C5 C6 C7 O2 179.8(4) . . . . ? C8 C6 C7 O2 -1.6(7) . . . . ? C5 C6 C7 C2 -2.5(7) . . . . ? C8 C6 C7 C2 176.1(4) . . . . ? C3 C2 C7 O2 179.3(5) . . . . ? O1 C2 C7 O2 -2.2(7) . . . . ? C3 C2 C7 C6 1.4(8) . . . . ? O1 C2 C7 C6 179.9(4) . . . . ? C14 N2 C8 N1 1.0(6) . . . . ? Cd1 N2 C8 N1 172.6(3) . . . . ? C14 N2 C8 C6 179.6(5) . . . . ? Cd1 N2 C8 C6 -8.7(7) . . . . ? C9 N1 C8 N2 -0.9(6) . . . . ? C9 N1 C8 C6 -179.7(4) . . . . ? C5 C6 C8 N2 -155.5(5) . . . . ? C7 C6 C8 N2 25.9(8) . . . . ? C5 C6 C8 N1 23.0(7) . . . . ? C7 C6 C8 N1 -155.6(5) . . . . ? C8 N1 C9 C14 0.4(6) . . . . ? C8 N1 C9 C10 -177.8(6) . . . . ? N1 C9 C10 C11 178.4(6) . . . . ? C14 C9 C10 C11 0.4(8) . . . . ? C9 C10 C11 C12 -0.3(10) . . . . ? C10 C11 C12 C13 1.1(11) . . . . ? C11 C12 C13 C14 -1.9(10) . . . . ? N1 C9 C14 C13 -179.7(5) . . . . ? C10 C9 C14 C13 -1.2(8) . . . . ? N1 C9 C14 N2 0.1(6) . . . . ? C10 C9 C14 N2 178.6(5) . . . . ? C12 C13 C14 C9 1.9(9) . . . . ? C12 C13 C14 N2 -177.9(6) . . . . ? C8 N2 C14 C9 -0.7(6) . . . . ? Cd1 N2 C14 C9 -172.1(3) . . . . ? C8 N2 C14 C13 179.1(6) . . . . ? Cd1 N2 C14 C13 7.7(8) . . . . ? C15 O3 C16 C17 5.0(8) . . . . ? Cd2 O3 C16 C17 -178.5(4) . . . . ? C15 O3 C16 C21 -174.9(5) . . . . ? Cd2 O3 C16 C21 1.6(5) . . . . ? O3 C16 C17 C18 -178.8(5) . . . . ? C21 C16 C17 C18 1.1(8) . . . . ? C16 C17 C18 C19 -0.6(8) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 2.4(8) . . . . ? C18 C19 C20 C22 -174.4(5) . . . . ? Cd2 O4 C21 C16 1.0(6) . . . . ? Cd1 O4 C21 C16 150.5(3) . . . . ? Cd2 O4 C21 C20 179.1(3) . . . . ? Cd1 O4 C21 C20 -31.5(6) . . . . ? O3 C16 C21 O4 -1.7(6) . . . . ? C17 C16 C21 O4 178.4(5) . . . . ? O3 C16 C21 C20 -180.0(4) . . . . ? C17 C16 C21 C20 0.1(7) . . . . ? C19 C20 C21 O4 -179.9(5) . . . . ? C22 C20 C21 O4 -3.2(7) . . . . ? C19 C20 C21 C16 -1.8(7) . . . . ? C22 C20 C21 C16 174.9(4) . . . . ? C23 N3 C22 N4 1.2(5) . . . . ? Cd1 N3 C22 N4 -174.9(3) . . . . ? C23 N3 C22 C20 -175.0(5) . . . . ? Cd1 N3 C22 C20 8.9(7) . . . . ? C28 N4 C22 N3 -0.7(6) . . . . ? C28 N4 C22 C20 175.8(4) . . . . ? C19 C20 C22 N3 -166.9(5) . . . . ? C21 C20 C22 N3 16.4(8) . . . . ? C19 C20 C22 N4 17.3(7) . . . . ? C21 C20 C22 N4 -159.4(5) . . . . ? C22 N3 C23 C24 176.4(5) . . . . ? Cd1 N3 C23 C24 -7.7(8) . . . . ? C22 N3 C23 C28 -1.3(6) . . . . ? Cd1 N3 C23 C28 174.7(3) . . . . ? C28 C23 C24 C25 0.6(8) . . . . ? N3 C23 C24 C25 -176.8(5) . . . . ? C23 C24 C25 C26 -1.0(9) . . . . ? C24 C25 C26 C27 0.5(10) . . . . ? C25 C26 C27 C28 0.4(9) . . . . ? C22 N4 C28 C27 -177.0(6) . . . . ? C22 N4 C28 C23 -0.1(5) . . . . ? C26 C27 C28 N4 175.7(6) . . . . ? C26 C27 C28 C23 -0.8(8) . . . . ? C24 C23 C28 N4 -177.0(5) . . . . ? N3 C23 C28 N4 0.8(6) . . . . ? C24 C23 C28 C27 0.3(8) . . . . ? N3 C23 C28 C27 178.1(5) . . . . ? Cd1 O5 C29 N5 -157.7(5) . . . . ? C30 N5 C29 O5 4.8(10) . . . . ? C31 N5 C29 O5 178.5(6) . . . . ? Cd1 O6 C32 N6 -145.8(5) . . . . ? C33 N6 C32 O6 3.5(10) . . . . ? C34 N6 C32 O6 178.8(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O8 0.838(10) 1.93(3) 2.744(7) 164(9) . O7 H7B Cl1 0.842(10) 2.41(3) 3.212(6) 160(9) 2_545 O8 H8A Cl2 0.843(10) 2.447(15) 3.287(6) 174(10) 2 O8 H8B Cl1 0.845(10) 2.62(7) 3.334(7) 143(10) 4_665 N1 H1 O7 0.86 1.98 2.822(6) 166.3 1_455 N4 H4 Cl2 0.86 2.81 3.652(4) 166.3 2 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.85 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.007 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.090 #################### END ###################