Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Scorpion-shaped Carboxylate Ligand Tailored Molecular Square, Bilayer, Self-threading and (3, 6)-Connected Nets ; _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_email YYG@FJIRSM.AC.CN loop_ _publ_author_name 'Yuan-Gen Yao' 'Xin-Yi Cao' 'Jian-Kai Cheng' 'Zhao-Ji Li' 'Jian Zhang' # Attachment 'complex_1.CIF' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 641175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H34 N4 O17 Zn2' _chemical_formula_weight 1021.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 13.0204(10) _cell_length_b 20.3203(14) _cell_length_c 15.8814(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4201.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.05 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .6921 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9693 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3669 _reflns_number_gt 2669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.1797P)^2^+6.7601P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3669 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1108 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2753 _refine_ls_wR_factor_gt 0.2378 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.21591(5) -0.07216(3) 0.52218(4) 0.0430(4) Uani 1 1 d . . . O1W O 0.0000 -0.1732(3) 0.2500 0.0557(15) Uani 1 2 d S . . O2 O -0.0737(3) -0.1984(2) 0.5765(4) 0.0680(14) Uani 1 1 d . . . O2W O -0.2452(3) -0.1747(2) 0.4943(3) 0.0578(12) Uani 1 1 d . . . H1 H -0.1993 -0.1975 0.5142 0.069 Uiso 1 1 d R . . H2 H -0.2719 -0.1713 0.4583 0.069 Uiso 1 1 d R . . O3 O -0.0907(3) -0.0894(2) 0.5873(3) 0.0494(10) Uani 1 1 d . . . O4 O 0.2532(4) -0.3002(2) 0.6888(4) 0.0671(13) Uani 1 1 d . . . O5 O 0.3564(3) -0.2360(2) 0.7626(3) 0.0686(14) Uani 1 1 d . . . H5OA H 0.412(7) -0.278(4) 0.759(7) 0.12(3) Uiso 1 1 d . . . O6 O 0.0739(3) 0.0986(2) 0.6278(3) 0.0548(11) Uani 1 1 d . . . O7 O 0.2197(3) 0.0478(2) 0.5975(3) 0.0517(11) Uani 1 1 d . . . O9 O 0.2205(3) -0.01370(19) 0.7510(3) 0.0442(10) Uani 1 1 d . . . N1 N -0.2190(3) 0.0318(3) 0.5539(3) 0.0464(12) Uani 1 1 d . . . N2 N -0.3624(4) -0.0618(3) 0.5718(3) 0.0480(12) Uani 1 1 d . . . C1 C -0.1471(5) 0.0771(3) 0.5438(5) 0.0547(16) Uani 1 1 d . . . H1A H -0.0824 0.0637 0.5259 0.066 Uiso 1 1 calc R . . C2 C -0.1633(6) 0.1441(3) 0.5586(5) 0.0626(18) Uani 1 1 d . . . H2A H -0.1108 0.1745 0.5502 0.075 Uiso 1 1 calc R . . C3 C -0.2589(6) 0.1643(4) 0.5860(5) 0.0670(19) Uani 1 1 d . . . H3A H -0.2714 0.2085 0.5969 0.080 Uiso 1 1 calc R . . C4 C -0.3376(5) 0.1173(3) 0.5975(4) 0.0545(16) Uani 1 1 d . . . C5 C -0.4387(6) 0.1333(4) 0.6260(5) 0.074(2) Uani 1 1 d . . . H5A H -0.4549 0.1769 0.6379 0.089 Uiso 1 1 calc R . . C6 C -0.5102(5) 0.0871(4) 0.6356(5) 0.0663(19) Uani 1 1 d . . . H6A H -0.5758 0.0993 0.6529 0.080 Uiso 1 1 calc R . . C7 C -0.4887(5) 0.0192(4) 0.6202(4) 0.0584(17) Uani 1 1 d . . . C8 C -0.5597(6) -0.0321(4) 0.6285(5) 0.069(2) Uani 1 1 d . . . H8A H -0.6260 -0.0228 0.6468 0.083 Uiso 1 1 calc R . . C9 C -0.5332(5) -0.0950(4) 0.6104(5) 0.072(2) Uani 1 1 d . . . H9A H -0.5807 -0.1289 0.6160 0.086 Uiso 1 1 calc R . . C10 C -0.4336(5) -0.1080(4) 0.5833(4) 0.0585(16) Uani 1 1 d . . . H10A H -0.4157 -0.1515 0.5726 0.070 Uiso 1 1 calc R . . C11 C -0.3129(5) 0.0514(3) 0.5804(4) 0.0461(13) Uani 1 1 d . . . C12 C -0.3900(4) 0.0011(3) 0.5907(4) 0.0463(14) Uani 1 1 d . . . C13 C 0.0557(4) -0.1380(3) 0.6476(4) 0.0439(13) Uani 1 1 d . . . C14 C 0.1159(5) -0.1937(3) 0.6613(4) 0.0480(14) Uani 1 1 d . . . H14A H 0.0948 -0.2345 0.6413 0.058 Uiso 1 1 calc R . . C15 C 0.2080(4) -0.1877(3) 0.7052(4) 0.0449(13) Uani 1 1 d . . . C16 C 0.2382(4) -0.1272(3) 0.7346(4) 0.0419(13) Uani 1 1 d . . . H16A H 0.2990 -0.1237 0.7650 0.050 Uiso 1 1 calc R . . C17 C 0.1803(5) -0.0714(3) 0.7200(4) 0.0421(13) Uani 1 1 d . . . C18 C 0.0881(4) -0.0768(3) 0.6766(4) 0.0416(13) Uani 1 1 d . . . H18A H 0.0481 -0.0397 0.6670 0.050 Uiso 1 1 calc R . . C19 C -0.0441(4) -0.1431(3) 0.5997(4) 0.0494(14) Uani 1 1 d . . . C20 C 0.2725(5) -0.2472(3) 0.7184(4) 0.0496(15) Uani 1 1 d . . . C21 C 0.1606(5) 0.0439(3) 0.7395(4) 0.0465(13) Uani 1 1 d . . . H21A H 0.1918 0.0796 0.7711 0.056 Uiso 1 1 calc R . . H21B H 0.0927 0.0363 0.7628 0.056 Uiso 1 1 calc R . . C22 C 0.1490(4) 0.0655(3) 0.6477(4) 0.0425(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 Zn1 0.0394(5) 0.0452(6) 0.0443(6) 0.0023(3) 0.0002(3) 0.0027(3) O1W 0.044(3) 0.045(3) 0.078(4) 0.000 0.010(3) 0.000 O2 0.065(3) 0.038(2) 0.101(4) -0.002(2) -0.036(3) -0.001(2) O2W 0.056(3) 0.051(3) 0.067(3) 0.003(2) -0.015(2) -0.001(2) O3 0.052(2) 0.045(2) 0.052(2) -0.003(2) -0.0106(19) 0.0064(19) O4 0.071(3) 0.048(3) 0.083(4) -0.007(3) -0.013(3) 0.009(2) O5 0.061(3) 0.054(3) 0.091(4) -0.007(3) -0.023(3) 0.012(2) O6 0.043(2) 0.069(3) 0.053(2) 0.000(2) 0.0011(19) 0.008(2) O7 0.044(2) 0.060(3) 0.051(3) -0.008(2) 0.0060(18) 0.0068(18) O9 0.050(2) 0.037(2) 0.046(2) -0.0040(19) -0.0084(17) 0.0012(16) N1 0.044(3) 0.048(3) 0.047(3) 0.001(2) 0.000(2) 0.002(2) N2 0.042(2) 0.053(3) 0.049(3) 0.004(2) 0.003(2) 0.001(2) C1 0.051(4) 0.056(4) 0.056(4) 0.000(3) -0.005(3) -0.003(3) C2 0.074(4) 0.050(4) 0.064(4) 0.005(3) -0.005(4) -0.008(3) C3 0.088(5) 0.057(4) 0.056(4) 0.003(4) -0.013(4) 0.010(4) C4 0.058(4) 0.056(4) 0.050(4) -0.004(3) -0.006(3) 0.012(3) C5 0.076(5) 0.062(5) 0.084(5) -0.014(4) -0.010(4) 0.034(4) C6 0.048(4) 0.081(5) 0.070(5) -0.009(4) 0.004(3) 0.020(4) C7 0.050(3) 0.074(4) 0.051(4) -0.001(3) 0.003(3) 0.013(3) C8 0.050(4) 0.082(5) 0.076(5) 0.005(4) 0.004(3) 0.003(3) C9 0.052(4) 0.083(6) 0.080(5) 0.010(4) 0.009(4) -0.008(4) C10 0.058(4) 0.058(4) 0.059(4) 0.013(3) 0.003(3) -0.008(3) C11 0.054(3) 0.044(3) 0.040(3) 0.001(3) -0.007(3) 0.009(3) C12 0.039(3) 0.057(4) 0.043(3) 0.000(3) -0.007(2) 0.001(3) C13 0.040(3) 0.042(3) 0.050(3) 0.000(3) -0.001(2) 0.003(2) C14 0.055(3) 0.037(3) 0.052(4) 0.000(3) -0.008(3) 0.006(3) C15 0.046(3) 0.038(3) 0.050(3) -0.001(3) 0.001(2) 0.005(2) C16 0.041(3) 0.041(3) 0.043(3) 0.001(2) -0.005(2) 0.006(2) C17 0.050(3) 0.042(3) 0.034(3) -0.002(2) 0.001(2) -0.004(2) C18 0.046(3) 0.035(3) 0.044(3) 0.004(2) 0.002(3) 0.006(2) C19 0.043(3) 0.053(4) 0.051(3) -0.003(3) -0.002(3) -0.005(3) C20 0.064(4) 0.038(4) 0.047(3) 0.000(3) -0.002(3) 0.005(3) C21 0.049(3) 0.042(3) 0.048(3) -0.002(3) 0.000(3) 0.002(3) C22 0.044(3) 0.038(3) 0.045(3) -0.002(2) -0.001(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.962(4) . ? Zn1 O7 1.966(5) 5_556 ? Zn1 N2 2.075(5) . ? Zn1 O2W 2.163(4) . ? Zn1 N1 2.172(5) . ? O2 C19 1.244(7) . ? O2W H1 0.8201 . ? O2W H2 0.6727 . ? O3 C19 1.264(7) . ? O4 C20 1.202(7) . ? O5 C20 1.318(7) . ? O5 H5OA 1.12(9) . ? O6 C22 1.228(7) . ? O7 C22 1.269(7) . ? O7 Zn1 1.966(5) 5_556 ? O9 C17 1.375(7) . ? O9 C21 1.419(7) . ? N1 C1 1.324(8) . ? N1 C11 1.354(8) . ? N2 C10 1.332(8) . ? N2 C12 1.360(8) . ? C1 C2 1.397(9) . ? C1 H1A 0.9300 . ? C2 C3 1.381(11) . ? C2 H2A 0.9300 . ? C3 C4 1.412(10) . ? C3 H3A 0.9300 . ? C4 C11 1.403(9) . ? C4 C5 1.429(10) . ? C5 C6 1.332(11) . ? C5 H5A 0.9300 . ? C6 C7 1.428(10) . ? C6 H6A 0.9300 . ? C7 C8 1.399(10) . ? C7 C12 1.417(9) . ? C8 C9 1.355(11) . ? C8 H8A 0.9300 . ? C9 C10 1.391(10) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.442(9) . ? C13 C18 1.391(7) . ? C13 C14 1.394(8) . ? C13 C19 1.509(8) . ? C14 C15 1.392(8) . ? C14 H14A 0.9300 . ? C15 C16 1.372(8) . ? C15 C20 1.488(8) . ? C16 C17 1.380(8) . ? C16 H16A 0.9300 . ? C17 C18 1.389(8) . ? C18 H18A 0.9300 . ? C21 C22 1.531(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? 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 O3 Zn1 O7 125.12(17) . 5_556 ? O3 Zn1 N2 125.6(2) . . ? O7 Zn1 N2 108.61(18) 5_556 . ? O3 Zn1 O2W 94.71(17) . . ? O7 Zn1 O2W 92.3(2) 5_556 . ? N2 Zn1 O2W 90.8(2) . . ? O3 Zn1 N1 93.82(18) . . ? O7 Zn1 N1 88.8(2) 5_556 . ? N2 Zn1 N1 78.25(19) . . ? O2W Zn1 N1 168.71(17) . . ? Zn1 O2W H1 109.7 . . ? Zn1 O2W H2 99.7 . . ? H1 O2W H2 139.5 . . ? C19 O3 Zn1 129.4(4) . . ? C20 O5 H5OA 112(5) . . ? C22 O7 Zn1 121.2(4) . 5_556 ? C17 O9 C21 116.7(4) . . ? C1 N1 C11 118.2(6) . . ? C1 N1 Zn1 129.5(4) . . ? C11 N1 Zn1 112.0(4) . . ? C10 N2 C12 116.7(5) . . ? C10 N2 Zn1 128.3(5) . . ? C12 N2 Zn1 114.9(4) . . ? N1 C1 C2 123.4(6) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.6(7) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.6(7) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C11 C4 C3 117.0(6) . . ? C11 C4 C5 119.3(7) . . ? C3 C4 C5 123.7(7) . . ? C6 C5 C4 121.3(7) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 121.6(6) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C8 C7 C12 115.9(7) . . ? C8 C7 C6 125.0(6) . . ? C12 C7 C6 119.1(7) . . ? C9 C8 C7 121.0(7) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 118.8(7) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? N2 C10 C9 123.8(7) . . ? N2 C10 H10A 118.1 . . ? C9 C10 H10A 118.1 . . ? N1 C11 C4 123.3(6) . . ? N1 C11 C12 117.0(5) . . ? C4 C11 C12 119.7(6) . . ? N2 C12 C7 123.8(6) . . ? N2 C12 C11 117.3(5) . . ? C7 C12 C11 118.9(6) . . ? C18 C13 C14 120.2(5) . . ? C18 C13 C19 119.3(5) . . ? C14 C13 C19 120.5(5) . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 C14 119.7(5) . . ? C16 C15 C20 121.2(5) . . ? C14 C15 C20 119.0(5) . . ? C15 C16 C17 121.4(5) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? O9 C17 C16 115.6(5) . . ? O9 C17 C18 125.0(5) . . ? C16 C17 C18 119.4(5) . . ? C17 C18 C13 119.9(5) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? O2 C19 O3 125.8(5) . . ? O2 C19 C13 118.6(5) . . ? O3 C19 C13 115.6(5) . . ? O4 C20 O5 122.4(6) . . ? O4 C20 C15 123.7(6) . . ? O5 C20 C15 113.8(5) . . ? O9 C21 C22 114.4(5) . . ? O9 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? O9 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? O6 C22 O7 124.9(6) . . ? O6 C22 C21 118.7(5) . . ? O7 C22 C21 116.4(5) . . ? 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 O2W H2 O4 0.67 2.43 2.953(8) 136.5 3_446 O5 H5OA O1W 1.12(9) 1.52(9) 2.635(6) 171(8) 2_545 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.574 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.147 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment 'complex_2.CIF' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 641176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18.66 N2 O10.33 Zn2' _chemical_formula_weight 583.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 13.017(2) _cell_length_b 12.4950(14) _cell_length_c 14.208(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.619(7) _cell_angle_gamma 90.00 _cell_volume 2190.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5067 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1181 _exptl_absorpt_coefficient_mu 2.253 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7818 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16725 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5025 _reflns_number_gt 4252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0751P)^2^+2.5099P] 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 5025 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0635 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.12364(3) 0.78243(3) 0.17292(3) 0.03223(14) Uani 1 1 d . . . Zn2 Zn 0.32475(4) 0.92249(3) 0.32436(4) 0.03627(15) Uani 1 1 d . . . O1 O 0.4188(2) 0.7948(2) 0.3512(2) 0.0428(7) Uani 1 1 d . . . O1W O 0.3337(3) 0.9290(3) 0.4795(3) 0.0476(8) Uani 1 1 d . . . H1WA H 0.3784 0.9742 0.5083 0.071 Uiso 1 1 calc R . . H1WB H 0.284(3) 0.931(3) 0.476(3) 0.008(10) Uiso 1 1 d . . . O2 O 0.5297(2) 0.9315(2) 0.3959(2) 0.0405(7) Uani 1 1 d . . . O2W O 0.1739(2) 0.8757(2) 0.2842(2) 0.0382(6) Uani 1 1 d . . . H8OA H 0.143(5) 0.865(4) 0.326(4) 0.057 Uiso 1 1 d . . . O3W O 0.1145(3) 0.9388(4) 0.4666(3) 0.0642(10) Uani 1 1 d . . . H2WB H 0.105(6) 0.857(6) 0.462(5) 0.096 Uiso 1 1 d . . . H2WA H 0.088(6) 1.001(6) 0.473(5) 0.096 Uiso 1 1 d . . . O3 O 0.9695(2) 0.6919(3) 0.6149(2) 0.0467(7) Uani 1 1 d . . . O4 O 0.9350(2) 0.8377(2) 0.5216(2) 0.0483(7) Uani 1 1 d . . . O4W O -0.0083(12) 1.0667(15) 0.0822(12) 0.121(7) Uani 0.33 1 d P . . O5 O 0.8166(3) 0.3134(3) 0.4337(3) 0.0591(9) Uani 1 1 d . . . O6 O 0.6780(3) 0.4064(3) 0.3351(2) 0.0605(9) Uani 1 1 d . . . O7 O 0.6227(2) 0.4729(2) 0.4918(2) 0.0434(7) Uani 1 1 d . . . N1 N 0.1729(3) 1.6291(2) 0.2096(2) 0.0352(7) Uani 1 1 d . . . N2 N 0.3136(3) 1.0841(2) 0.2992(2) 0.0348(7) Uani 1 1 d . . . C1 C 0.6028(3) 0.7547(3) 0.4326(3) 0.0291(7) Uani 1 1 d . . . C2 C 0.7102(3) 0.7886(3) 0.4673(2) 0.0267(7) Uani 1 1 d . . . H2A H 0.7272 0.8602 0.4623 0.032 Uiso 1 1 calc R . . C3 C 0.7917(3) 0.7154(3) 0.5094(3) 0.0268(7) Uani 1 1 d . . . C4 C 0.7662(3) 0.6076(3) 0.5162(3) 0.0323(8) Uani 1 1 d . . . H4A H 0.8211 0.5581 0.5433 0.039 Uiso 1 1 calc R . . C5 C 0.6584(3) 0.5748(3) 0.4823(3) 0.0323(8) Uani 1 1 d . . . C6 C 0.5776(3) 0.6483(3) 0.4391(3) 0.0321(8) Uani 1 1 d . . . H6A H 0.5059 0.6258 0.4144 0.039 Uiso 1 1 calc R . . C7 C 0.5127(3) 0.8328(3) 0.3904(3) 0.0309(8) Uani 1 1 d . . . C8 C 0.9069(3) 0.7530(3) 0.5503(3) 0.0326(8) Uani 1 1 d . . . C9 C 0.6978(3) 0.3885(3) 0.5075(3) 0.0387(9) Uani 1 1 d . . . H9A H 0.6654 0.3236 0.5228 0.046 Uiso 1 1 calc R . . H9B H 0.7609 0.4052 0.5640 0.046 Uiso 1 1 calc R . . C10 C 0.7334(4) 0.3694(3) 0.4159(3) 0.0420(9) Uani 1 1 d . . . C11 C 0.1034(3) 1.5548(3) 0.2183(3) 0.0394(9) Uani 1 1 d . . . H11A H 0.0327 1.5752 0.2116 0.047 Uiso 1 1 calc R . . C12 C 0.1320(4) 1.4482(3) 0.2371(3) 0.0411(9) Uani 1 1 d . . . H12A H 0.0814 1.3985 0.2435 0.049 Uiso 1 1 calc R . . C13 C 0.2361(3) 1.4166(3) 0.2463(3) 0.0329(8) Uani 1 1 d . . . C14 C 0.3096(3) 1.4946(3) 0.2399(3) 0.0377(9) Uani 1 1 d . . . H14A H 0.3812 1.4765 0.2481 0.045 Uiso 1 1 calc R . . C15 C 0.2754(3) 1.5986(3) 0.2213(3) 0.0371(8) Uani 1 1 d . . . H15A H 0.3251 1.6501 0.2167 0.045 Uiso 1 1 calc R . . C16 C 0.2662(3) 1.3016(3) 0.2645(3) 0.0334(8) Uani 1 1 d . . . C17 C 0.1874(4) 1.2239(3) 0.2277(3) 0.0420(10) Uani 1 1 d . . . H17A H 0.1172 1.2437 0.1910 0.050 Uiso 1 1 calc R . . C18 C 0.2138(4) 1.1171(3) 0.2459(3) 0.0438(10) Uani 1 1 d . . . H18A H 0.1602 1.0660 0.2202 0.053 Uiso 1 1 calc R . . C19 C 0.3903(3) 1.1584(3) 0.3326(3) 0.0370(9) Uani 1 1 d . . . H19A H 0.4601 1.1366 0.3686 0.044 Uiso 1 1 calc R . . C20 C 0.3700(3) 1.2674(3) 0.3156(3) 0.0369(9) Uani 1 1 d . . . H20A H 0.4259 1.3167 0.3384 0.044 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 Zn1 0.0261(2) 0.0245(2) 0.0424(3) -0.00137(17) 0.00567(18) 0.00003(16) Zn2 0.0285(2) 0.0239(2) 0.0492(3) 0.00086(17) 0.0022(2) 0.00263(16) O1 0.0246(13) 0.0410(16) 0.0538(17) -0.0086(13) -0.0004(12) 0.0057(11) O1W 0.0337(18) 0.053(2) 0.053(2) -0.0063(14) 0.0103(16) -0.0029(16) O2 0.0344(15) 0.0312(14) 0.0508(16) 0.0055(12) 0.0066(13) 0.0061(11) O2W 0.0274(14) 0.0442(16) 0.0393(15) -0.0079(12) 0.0052(12) -0.0038(12) O3W 0.053(2) 0.068(2) 0.078(2) 0.012(2) 0.030(2) 0.0074(19) O3 0.0237(13) 0.0518(18) 0.0544(17) 0.0177(14) -0.0021(12) -0.0015(12) O4 0.0326(15) 0.0426(16) 0.0634(19) 0.0120(14) 0.0065(14) -0.0028(13) O4W 0.069(9) 0.156(15) 0.098(10) 0.069(10) -0.027(8) -0.043(9) O5 0.063(2) 0.055(2) 0.067(2) 0.0050(17) 0.0311(18) 0.0191(18) O6 0.062(2) 0.074(2) 0.0453(18) 0.0021(16) 0.0157(17) 0.0082(19) O7 0.0376(15) 0.0323(14) 0.0618(19) 0.0041(13) 0.0181(14) -0.0016(12) N1 0.0389(18) 0.0267(15) 0.0367(16) 0.0025(13) 0.0076(14) 0.0055(13) N2 0.0402(18) 0.0248(15) 0.0362(16) 0.0020(12) 0.0077(14) 0.0047(13) C1 0.0255(17) 0.0332(18) 0.0271(17) -0.0006(14) 0.0062(14) 0.0053(14) C2 0.0260(17) 0.0258(16) 0.0277(16) 0.0006(13) 0.0076(14) 0.0012(13) C3 0.0226(16) 0.0295(17) 0.0283(16) -0.0003(13) 0.0081(13) 0.0015(13) C4 0.0285(18) 0.0304(18) 0.0363(19) 0.0037(14) 0.0079(15) 0.0064(15) C5 0.0320(19) 0.0274(18) 0.0383(19) 0.0000(14) 0.0124(16) -0.0031(14) C6 0.0244(17) 0.0351(19) 0.0350(18) -0.0019(15) 0.0067(15) -0.0009(15) C7 0.0242(17) 0.041(2) 0.0273(17) 0.0009(15) 0.0076(14) 0.0056(15) C8 0.0264(18) 0.0342(19) 0.0366(19) 0.0016(15) 0.0093(15) 0.0019(15) C9 0.041(2) 0.0300(19) 0.049(2) 0.0005(16) 0.0194(19) 0.0011(16) C10 0.045(2) 0.0279(19) 0.050(2) -0.0054(17) 0.011(2) -0.0055(17) C11 0.034(2) 0.034(2) 0.051(2) 0.0057(17) 0.0156(18) 0.0036(17) C12 0.042(2) 0.0302(19) 0.053(2) 0.0082(17) 0.0182(19) 0.0012(17) C13 0.044(2) 0.0258(18) 0.0283(17) 0.0018(13) 0.0111(16) 0.0037(15) C14 0.036(2) 0.0322(19) 0.045(2) 0.0003(16) 0.0134(18) 0.0034(16) C15 0.035(2) 0.0301(19) 0.047(2) -0.0001(16) 0.0134(18) 0.0001(16) C16 0.042(2) 0.0278(18) 0.0325(18) 0.0032(14) 0.0143(16) 0.0040(15) C17 0.040(2) 0.0289(19) 0.048(2) 0.0042(16) 0.0019(18) 0.0092(17) C18 0.043(2) 0.0276(19) 0.051(2) 0.0024(17) 0.0010(19) 0.0037(17) C19 0.036(2) 0.0315(19) 0.040(2) 0.0035(16) 0.0071(17) 0.0049(16) C20 0.044(2) 0.0288(19) 0.038(2) -0.0005(15) 0.0136(18) 0.0014(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2W 1.904(3) . ? Zn1 O3 1.937(3) 4_475 ? Zn1 O5 1.950(3) 2_655 ? Zn1 N1 2.034(3) 1_545 ? Zn2 O2W 1.952(3) . ? Zn2 O1 1.972(3) . ? Zn2 N2 2.048(3) . ? Zn2 O1W 2.171(4) . ? Zn2 O6 2.264(3) 2_655 ? Zn2 C7 2.580(4) . ? O1 C7 1.264(5) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.63(4) . ? O2 C7 1.251(5) . ? O2W H8OA 0.83(5) . ? O3W H2WB 1.03(7) . ? O3W H2WA 0.86(7) . ? O3 C8 1.270(5) . ? O3 Zn1 1.937(3) 4_676 ? O4 C8 1.230(5) . ? O5 C10 1.245(5) . ? O5 Zn1 1.950(3) 2_645 ? O6 C10 1.234(5) . ? O6 Zn2 2.264(3) 2_645 ? O7 C5 1.377(4) . ? O7 C9 1.408(5) . ? N1 C11 1.330(5) . ? N1 C15 1.346(5) . ? N1 Zn1 2.034(3) 1_565 ? N2 C19 1.335(5) . ? N2 C18 1.342(5) . ? C1 C6 1.380(5) . ? C1 C2 1.391(5) . ? C1 C7 1.496(5) . ? C2 C3 1.383(5) . ? C2 H2A 0.9300 . ? C3 C4 1.397(5) . ? C3 C8 1.501(5) . ? C4 C5 1.392(5) . ? C4 H4A 0.9300 . ? C5 C6 1.384(5) . ? C6 H6A 0.9300 . ? C9 C10 1.533(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.386(6) . ? C11 H11A 0.9300 . ? C12 C13 1.377(6) . ? C12 H12A 0.9300 . ? C13 C14 1.390(6) . ? C13 C16 1.490(5) . ? C14 C15 1.371(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C20 1.382(6) . ? C16 C17 1.386(6) . ? C17 C18 1.381(5) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.393(5) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Zn1 O3 106.63(12) . 4_475 ? O2W Zn1 O5 114.02(14) . 2_655 ? O3 Zn1 O5 104.66(15) 4_475 2_655 ? O2W Zn1 N1 111.54(13) . 1_545 ? O3 Zn1 N1 117.65(14) 4_475 1_545 ? O5 Zn1 N1 102.36(15) 2_655 1_545 ? O2W Zn2 O1 108.57(12) . . ? O2W Zn2 N2 103.63(13) . . ? O1 Zn2 N2 146.77(13) . . ? O2W Zn2 O1W 91.80(13) . . ? O1 Zn2 O1W 90.31(13) . . ? N2 Zn2 O1W 96.78(13) . . ? O2W Zn2 O6 89.30(13) . 2_655 ? O1 Zn2 O6 86.11(14) . 2_655 ? N2 Zn2 O6 86.27(13) . 2_655 ? O1W Zn2 O6 176.42(14) . 2_655 ? O2W Zn2 C7 136.47(13) . . ? O1 Zn2 C7 28.43(12) . . ? N2 Zn2 C7 119.87(13) . . ? O1W Zn2 C7 84.82(13) . . ? O6 Zn2 C7 92.04(13) 2_655 . ? C7 O1 Zn2 103.6(2) . . ? Zn2 O1W H1WA 109.5 . . ? Zn2 O1W H1WB 102(4) . . ? H1WA O1W H1WB 123.3 . . ? Zn1 O2W Zn2 118.24(15) . . ? Zn1 O2W H8OA 112(4) . . ? Zn2 O2W H8OA 120(4) . . ? H2WB O3W H2WA 148(7) . . ? C8 O3 Zn1 123.1(3) . 4_676 ? C10 O5 Zn1 119.4(3) . 2_645 ? C10 O6 Zn2 141.4(3) . 2_645 ? C5 O7 C9 118.0(3) . . ? C11 N1 C15 117.9(3) . . ? C11 N1 Zn1 120.9(3) . 1_565 ? C15 N1 Zn1 121.2(3) . 1_565 ? C19 N2 C18 117.8(3) . . ? C19 N2 Zn2 128.3(3) . . ? C18 N2 Zn2 113.8(3) . . ? C6 C1 C2 120.2(3) . . ? C6 C1 C7 118.8(3) . . ? C2 C1 C7 121.0(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 C8 119.6(3) . . ? C4 C3 C8 120.3(3) . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? O7 C5 C6 115.1(3) . . ? O7 C5 C4 125.0(3) . . ? C6 C5 C4 119.8(3) . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? O2 C7 O1 121.7(3) . . ? O2 C7 C1 121.2(3) . . ? O1 C7 C1 117.2(3) . . ? O2 C7 Zn2 73.9(2) . . ? O1 C7 Zn2 47.99(18) . . ? C1 C7 Zn2 163.8(3) . . ? O4 C8 O3 124.5(4) . . ? O4 C8 C3 120.5(3) . . ? O3 C8 C3 115.0(3) . . ? O7 C9 C10 111.4(3) . . ? O7 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? O7 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O6 C10 O5 127.7(4) . . ? O6 C10 C9 119.1(4) . . ? O5 C10 C9 113.2(4) . . ? N1 C11 C12 122.7(4) . . ? N1 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 118.0(3) . . ? C12 C13 C16 119.3(4) . . ? C14 C13 C16 122.7(4) . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N1 C15 C14 122.7(4) . . ? N1 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C20 C16 C17 117.6(3) . . ? C20 C16 C13 123.2(4) . . ? C17 C16 C13 119.2(4) . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? N2 C18 C17 122.7(4) . . ? N2 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? N2 C19 C20 122.6(4) . . ? N2 C19 H19A 118.7 . . ? C20 C19 H19A 118.7 . . ? C16 C20 C19 119.6(4) . . ? C16 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? 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 O1W H1WA O2 0.82 1.91 2.706(5) 165.0 3_676 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.558 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.085 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment 'complex_3.CIF' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 641177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 Cd3 N8 O20' _chemical_formula_weight 1544.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3945(7) _cell_length_b 10.2207(9) _cell_length_c 18.3523(17) _cell_angle_alpha 104.241(2) _cell_angle_beta 101.498(2) _cell_angle_gamma 92.684(2) _cell_volume 1487.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2819 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 25.06 _exptl_crystal_description Prism _exptl_crystal_colour white _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .6411 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7797 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5210 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0000P)^2^+48.4902P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5210 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1467 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2315 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.38363(13) 0.36256(10) 0.10956(6) 0.0305(3) Uani 1 1 d . . . Cd2 Cd 0.5000 1.0000 0.5000 0.0437(5) Uani 1 2 d S . . O1 O 0.5333(14) 0.5552(9) 0.1997(6) 0.050(3) Uani 1 1 d . . . O1W O 0.5898(13) 0.3338(9) 0.0398(6) 0.046(3) Uani 1 1 d . . . H1 H 0.5813 0.3538 -0.0010 0.055 Uiso 1 1 d R . . H1# H 0.6205 0.2801 0.0471 0.055 Uiso 1 1 d R . . O2 O 0.3941(13) 0.5961(9) 0.0937(6) 0.041(3) Uani 1 1 d . . . O2W O 0.5302(16) 0.7785(12) 0.5087(8) 0.074(4) Uani 1 1 d . . . H3 H 0.4813 0.7045 0.4845 0.088 Uiso 1 1 d R . . H4 H 0.6050 0.7889 0.4873 0.088 Uiso 1 1 d R . . O3 O 0.3500(13) 1.0915(9) 0.0953(6) 0.043(3) Uani 1 1 d . . . O4 O 0.5403(12) 1.2433(9) 0.1803(6) 0.037(2) Uani 1 1 d . . . O5 O 0.8838(13) 0.9999(10) 0.3400(6) 0.046(3) Uani 1 1 d . . . O6 O 0.7219(14) 0.9924(12) 0.4523(7) 0.058(3) Uani 1 1 d . . . O7 O 0.7963(17) 0.7889(15) 0.4547(10) 0.087(5) Uani 1 1 d . . . N1 N -0.291(2) 0.3977(17) 0.4696(9) 0.068(4) Uani 1 1 d . . . N2 N 0.1976(14) 0.3700(12) 0.1922(6) 0.037(3) Uani 1 1 d . . . N3 N -0.3456(15) 0.0770(14) -0.3704(7) 0.047(3) Uani 1 1 d . . . N4 N 0.1824(15) 0.3004(12) -0.0011(7) 0.040(3) Uani 1 1 d . . . C1 C -0.328(3) 0.4530(18) 0.4111(11) 0.067(5) Uani 1 1 d . . . H1B H -0.4248 0.4943 0.4068 0.081 Uiso 1 1 calc R . . C2 C -0.239(2) 0.4555(16) 0.3562(10) 0.052(4) Uani 1 1 d . . . H2A H -0.2740 0.4977 0.3172 0.063 Uiso 1 1 calc R . . C3 C -0.052(2) 0.3343(16) 0.4224(10) 0.053(4) Uani 1 1 d . . . H3B H 0.0456 0.2943 0.4293 0.063 Uiso 1 1 calc R . . C4 C -0.150(3) 0.336(2) 0.4718(12) 0.075(6) Uani 1 1 d . . . H4A H -0.1206 0.2915 0.5103 0.089 Uiso 1 1 calc R . . C5 C -0.093(2) 0.3919(14) 0.3610(9) 0.045(4) Uani 1 1 d . . . C6 C 0.007(2) 0.3864(15) 0.3025(9) 0.046(4) Uani 1 1 d . . . C7 C 0.176(2) 0.3915(17) 0.3222(10) 0.053(4) Uani 1 1 d . . . H7A H 0.2286 0.4022 0.3732 0.063 Uiso 1 1 calc R . . C8 C 0.264(2) 0.3807(18) 0.2660(10) 0.058(5) Uani 1 1 d . . . H8A H 0.3770 0.3809 0.2802 0.069 Uiso 1 1 calc R . . C9 C -0.066(2) 0.3697(16) 0.2259(10) 0.050(4) Uani 1 1 d . . . H9A H -0.1789 0.3640 0.2097 0.059 Uiso 1 1 calc R . . C10 C 0.035(2) 0.3616(15) 0.1735(9) 0.048(4) Uani 1 1 d . . . H10A H -0.0144 0.3494 0.1219 0.058 Uiso 1 1 calc R . . C11 C -0.300(2) 0.2064(17) -0.3372(8) 0.049(4) Uani 1 1 d . . . H11A H -0.3377 0.2690 -0.3642 0.059 Uiso 1 1 calc R . . C12 C -0.2020(19) 0.2547(15) -0.2654(9) 0.044(4) Uani 1 1 d . . . H12A H -0.1752 0.3475 -0.2446 0.053 Uiso 1 1 calc R . . C13 C -0.291(2) -0.0072(17) -0.3306(10) 0.053(4) Uani 1 1 d . . . H13A H -0.3245 -0.0990 -0.3525 0.063 Uiso 1 1 calc R . . C14 C -0.1882(19) 0.0277(15) -0.2594(8) 0.044(4) Uani 1 1 d . . . H14A H -0.1502 -0.0387 -0.2356 0.053 Uiso 1 1 calc R . . C15 C -0.1421(18) 0.1634(16) -0.2237(8) 0.040(4) Uani 1 1 d . . . C16 C -0.0294(17) 0.2094(13) -0.1464(8) 0.031(3) Uani 1 1 d . . . C17 C -0.0299(18) 0.1441(14) -0.0903(8) 0.039(4) Uani 1 1 d . . . H17A H -0.1021 0.0670 -0.0998 0.047 Uiso 1 1 calc R . . C18 C 0.077(2) 0.1915(15) -0.0185(9) 0.048(4) Uani 1 1 d . . . H18A H 0.0736 0.1445 0.0187 0.058 Uiso 1 1 calc R . . C19 C 0.079(2) 0.3248(16) -0.1275(9) 0.051(4) Uani 1 1 d . . . H19A H 0.0827 0.3734 -0.1639 0.061 Uiso 1 1 calc R . . C20 C 0.182(2) 0.3693(15) -0.0556(9) 0.047(4) Uani 1 1 d . . . H20A H 0.2521 0.4481 -0.0442 0.056 Uiso 1 1 calc R . . C21 C 0.5569(18) 0.7849(11) 0.1895(8) 0.032(3) Uani 1 1 d . . . C22 C 0.4906(16) 0.8775(11) 0.1535(8) 0.028(3) Uani 1 1 d . . . H22A H 0.4053 0.8509 0.1103 0.034 Uiso 1 1 calc R . . C23 C 0.5537(16) 1.0138(13) 0.1830(8) 0.030(3) Uani 1 1 d . . . C24 C 0.6831(17) 1.0482(13) 0.2459(7) 0.032(3) Uani 1 1 d . . . H24A H 0.7264 1.1384 0.2653 0.038 Uiso 1 1 calc R . . C25 C 0.7497(17) 0.9532(14) 0.2806(7) 0.034(3) Uani 1 1 d . . . C26 C 0.6841(17) 0.8214(13) 0.2537(8) 0.035(3) Uani 1 1 d . . . H26A H 0.7246 0.7566 0.2783 0.042 Uiso 1 1 calc R . . C27 C 0.4892(16) 0.6360(14) 0.1585(8) 0.035(3) Uani 1 1 d . . . C28 C 0.4753(19) 1.1246(13) 0.1497(9) 0.038(4) Uani 1 1 d . . . C29 C 0.9284(18) 0.9140(16) 0.3894(9) 0.042(4) Uani 1 1 d . . . H29A H 1.0319 0.9515 0.4244 0.050 Uiso 1 1 calc R . . H29B H 0.9436 0.8255 0.3585 0.050 Uiso 1 1 calc R . . C30 C 0.7982(19) 0.8962(17) 0.4373(8) 0.044(4) Uani 1 1 d . . . O3W O 0.7404(16) 0.0951(12) 0.0414(7) 0.067(4) 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 0.0381(6) 0.0193(5) 0.0305(5) 0.0055(4) 0.0010(4) -0.0014(4) Cd2 0.0382(9) 0.0522(10) 0.0345(9) 0.0023(7) 0.0061(7) -0.0031(8) O1 0.064(8) 0.022(5) 0.053(7) 0.009(5) -0.008(6) -0.005(5) O1W 0.065(7) 0.031(5) 0.047(6) 0.015(5) 0.016(6) 0.006(5) O2 0.051(6) 0.021(5) 0.041(6) 0.005(4) -0.007(5) -0.005(4) O2W 0.073(9) 0.054(8) 0.094(10) 0.012(7) 0.031(8) -0.008(7) O3 0.053(7) 0.023(5) 0.044(6) 0.007(4) -0.012(5) 0.003(5) O4 0.044(6) 0.021(5) 0.045(6) 0.010(4) 0.005(5) -0.006(4) O5 0.046(6) 0.047(6) 0.035(6) 0.006(5) -0.002(5) -0.011(5) O6 0.053(7) 0.063(8) 0.064(8) 0.017(6) 0.025(6) 0.014(6) O7 0.080(10) 0.088(10) 0.133(14) 0.074(10) 0.051(10) 0.041(8) N1 0.085(12) 0.070(11) 0.051(9) 0.011(8) 0.029(9) -0.010(9) N2 0.037(7) 0.042(7) 0.030(7) 0.012(5) -0.001(5) 0.002(6) N3 0.034(7) 0.065(9) 0.035(7) 0.006(7) 0.001(6) 0.003(7) N4 0.043(7) 0.035(7) 0.038(7) 0.011(6) -0.001(6) -0.008(6) C1 0.089(15) 0.049(11) 0.065(13) 0.004(9) 0.032(11) 0.001(10) C2 0.063(12) 0.039(9) 0.050(10) 0.011(8) 0.004(9) -0.004(8) C3 0.067(12) 0.037(9) 0.058(11) 0.021(8) 0.012(9) 0.011(8) C4 0.094(17) 0.076(14) 0.070(14) 0.027(11) 0.042(13) 0.016(12) C5 0.056(10) 0.028(8) 0.042(9) 0.000(7) 0.006(8) -0.016(7) C6 0.060(11) 0.030(8) 0.038(9) 0.000(6) 0.000(8) 0.000(7) C7 0.044(10) 0.065(11) 0.043(9) 0.015(8) -0.005(8) 0.001(8) C8 0.042(10) 0.071(12) 0.059(11) 0.009(9) 0.019(9) 0.008(9) C9 0.043(9) 0.049(10) 0.054(10) 0.006(8) 0.014(8) -0.001(8) C10 0.056(11) 0.041(9) 0.045(9) 0.016(7) 0.000(8) 0.004(8) C11 0.053(10) 0.054(10) 0.031(8) 0.008(7) -0.009(7) 0.007(8) C12 0.044(9) 0.037(8) 0.040(9) -0.002(7) -0.001(7) 0.001(7) C13 0.050(10) 0.044(9) 0.055(11) 0.005(8) 0.004(9) -0.008(8) C14 0.053(10) 0.036(8) 0.035(8) 0.009(7) -0.006(7) -0.007(7) C15 0.034(8) 0.055(10) 0.034(8) 0.012(7) 0.011(7) 0.007(7) C16 0.036(8) 0.024(7) 0.033(8) 0.007(6) 0.009(6) 0.001(6) C17 0.042(9) 0.029(7) 0.040(8) 0.012(6) -0.006(7) -0.015(6) C18 0.051(10) 0.035(8) 0.055(10) 0.018(7) 0.000(8) -0.004(7) C19 0.063(11) 0.042(9) 0.043(9) 0.014(7) 0.000(8) -0.003(8) C20 0.055(10) 0.027(8) 0.056(10) 0.015(7) 0.004(8) -0.007(7) C21 0.047(8) 0.009(6) 0.038(8) 0.000(5) 0.011(7) 0.002(6) C22 0.031(7) 0.010(6) 0.040(8) 0.001(5) 0.006(6) 0.003(5) C23 0.032(8) 0.028(7) 0.035(8) 0.012(6) 0.015(6) 0.009(6) C24 0.039(8) 0.028(7) 0.026(7) 0.006(6) 0.004(6) -0.005(6) C25 0.040(8) 0.034(8) 0.023(7) 0.004(6) 0.005(6) -0.005(6) C26 0.041(8) 0.020(7) 0.041(8) 0.010(6) 0.001(7) 0.003(6) C27 0.023(7) 0.032(8) 0.044(9) 0.005(7) 0.002(6) 0.001(6) C28 0.056(10) 0.024(7) 0.046(9) 0.016(6) 0.028(8) 0.005(7) C29 0.035(8) 0.046(9) 0.042(9) 0.008(7) 0.008(7) 0.008(7) C30 0.041(9) 0.055(10) 0.030(8) 0.015(7) -0.013(7) 0.007(8) O3W 0.084(9) 0.061(8) 0.062(8) 0.014(6) 0.025(7) 0.034(7) _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 O4 2.269(9) 1_545 ? Cd1 N4 2.298(12) . ? Cd1 O1W 2.338(10) . ? Cd1 O1 2.352(10) . ? Cd1 N2 2.376(12) . ? Cd1 O2 2.474(9) . ? Cd1 O3 2.714(9) 1_545 ? Cd1 C27 2.760(14) . ? Cd1 C28 2.807(13) 1_545 ? Cd2 O6 2.207(11) . ? Cd2 O6 2.207(11) 2_676 ? Cd2 O2W 2.330(12) 2_676 ? Cd2 O2W 2.330(12) . ? Cd2 N3 2.389(12) 2_565 ? Cd2 N3 2.389(12) 1_666 ? Cd2 H4 2.3449 . ? O1 C27 1.271(17) . ? O1W H1 0.8153 . ? O1W H1# 0.6488 . ? O2 C27 1.253(16) . ? O2W H3 0.8190 . ? O2W H4 0.8203 . ? O3 C28 1.264(18) . ? O3 Cd1 2.714(9) 1_565 ? O4 C28 1.252(16) . ? O4 Cd1 2.269(9) 1_565 ? O5 C25 1.375(16) . ? O5 C29 1.421(17) . ? O6 C30 1.203(18) . ? O7 C30 1.215(19) . ? N1 C1 1.32(2) . ? N1 C4 1.36(3) . ? N2 C10 1.332(19) . ? N2 C8 1.33(2) . ? N3 C13 1.30(2) . ? N3 C11 1.32(2) . ? N3 Cd2 2.389(12) 1_444 ? N4 C18 1.321(18) . ? N4 C20 1.355(18) . ? C1 C2 1.37(2) . ? C1 H1B 0.9300 . ? C2 C5 1.41(2) . ? C2 H2A 0.9300 . ? C3 C4 1.34(2) . ? C3 C5 1.39(2) . ? C3 H3B 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.48(2) . ? C6 C9 1.38(2) . ? C6 C7 1.39(2) . ? C7 C8 1.37(2) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.39(2) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.37(2) . ? C11 H11A 0.9300 . ? C12 C15 1.40(2) . ? C12 H12A 0.9300 . ? C13 C14 1.37(2) . ? C13 H13A 0.9300 . ? C14 C15 1.38(2) . ? C14 H14A 0.9300 . ? C15 C16 1.490(19) . ? C16 C17 1.359(18) . ? C16 C19 1.38(2) . ? C17 C18 1.40(2) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.38(2) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.361(18) . ? C21 C26 1.383(19) . ? C21 C27 1.525(17) . ? C22 C23 1.400(17) . ? C22 H22A 0.9300 . ? C23 C24 1.379(18) . ? C23 C28 1.529(18) . ? C24 C25 1.369(19) . ? C24 H24A 0.9300 . ? C25 C26 1.362(18) . ? C26 H26A 0.9300 . ? C28 Cd1 2.807(14) 1_565 ? C29 C30 1.56(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 N4 133.3(4) 1_545 . ? O4 Cd1 O1W 82.6(4) 1_545 . ? N4 Cd1 O1W 92.0(4) . . ? O4 Cd1 O1 85.1(3) 1_545 . ? N4 Cd1 O1 141.6(4) . . ? O1W Cd1 O1 91.8(4) . . ? O4 Cd1 N2 88.2(4) 1_545 . ? N4 Cd1 N2 94.0(4) . . ? O1W Cd1 N2 170.8(4) . . ? O1 Cd1 N2 87.9(4) . . ? O4 Cd1 O2 137.0(3) 1_545 . ? N4 Cd1 O2 88.0(4) . . ? O1W Cd1 O2 85.2(3) . . ? O1 Cd1 O2 54.3(3) . . ? N2 Cd1 O2 102.0(4) . . ? O4 Cd1 O3 52.3(3) 1_545 1_545 ? N4 Cd1 O3 81.6(4) . 1_545 ? O1W Cd1 O3 89.9(3) . 1_545 ? O1 Cd1 O3 136.6(3) . 1_545 ? N2 Cd1 O3 84.0(4) . 1_545 ? O2 Cd1 O3 168.3(3) . 1_545 ? O4 Cd1 C27 111.4(4) 1_545 . ? N4 Cd1 C27 114.7(4) . . ? O1W Cd1 C27 88.2(4) . . ? O1 Cd1 C27 27.3(4) . . ? N2 Cd1 C27 95.7(4) . . ? O2 Cd1 C27 27.0(4) . . ? O3 Cd1 C27 163.6(4) 1_545 . ? O4 Cd1 C28 25.9(4) 1_545 1_545 ? N4 Cd1 C28 107.7(4) . 1_545 ? O1W Cd1 C28 85.3(4) . 1_545 ? O1 Cd1 C28 110.7(4) . 1_545 ? N2 Cd1 C28 86.2(4) . 1_545 ? O2 Cd1 C28 161.9(4) . 1_545 ? O3 Cd1 C28 26.4(4) 1_545 1_545 ? C27 Cd1 C28 137.2(4) . 1_545 ? O6 Cd2 O6 180.000(2) . 2_676 ? O6 Cd2 O2W 92.3(5) . 2_676 ? O6 Cd2 O2W 87.7(5) 2_676 2_676 ? O6 Cd2 O2W 87.7(5) . . ? O6 Cd2 O2W 92.3(5) 2_676 . ? O2W Cd2 O2W 180.000(3) 2_676 . ? O6 Cd2 N3 87.5(4) . 2_565 ? O6 Cd2 N3 92.5(4) 2_676 2_565 ? O2W Cd2 N3 88.1(5) 2_676 2_565 ? O2W Cd2 N3 91.9(5) . 2_565 ? O6 Cd2 N3 92.5(4) . 1_666 ? O6 Cd2 N3 87.5(4) 2_676 1_666 ? O2W Cd2 N3 91.9(5) 2_676 1_666 ? O2W Cd2 N3 88.1(5) . 1_666 ? N3 Cd2 N3 180.000(3) 2_565 1_666 ? O6 Cd2 H4 67.5 . . ? O6 Cd2 H4 112.5 2_676 . ? O2W Cd2 H4 159.8 2_676 . ? O2W Cd2 H4 20.2 . . ? N3 Cd2 H4 89.4 2_565 . ? N3 Cd2 H4 90.6 1_666 . ? C27 O1 Cd1 94.5(8) . . ? Cd1 O1W H1 122.0 . . ? Cd1 O1W H1# 103.0 . . ? H1 O1W H1# 124.9 . . ? C27 O2 Cd1 89.3(8) . . ? Cd2 O2W H3 133.8 . . ? Cd2 O2W H4 80.9 . . ? H3 O2W H4 105.3 . . ? C28 O3 Cd1 80.9(7) . 1_565 ? C28 O4 Cd1 101.9(9) . 1_565 ? C25 O5 C29 116.6(11) . . ? C30 O6 Cd2 126.9(12) . . ? C1 N1 C4 114.0(17) . . ? C10 N2 C8 116.2(14) . . ? C10 N2 Cd1 127.9(10) . . ? C8 N2 Cd1 115.8(10) . . ? C13 N3 C11 116.0(13) . . ? C13 N3 Cd2 121.9(11) . 1_444 ? C11 N3 Cd2 121.9(11) . 1_444 ? C18 N4 C20 117.5(13) . . ? C18 N4 Cd1 123.2(10) . . ? C20 N4 Cd1 118.8(9) . . ? N1 C1 C2 127(2) . . ? N1 C1 H1B 116.7 . . ? C2 C1 H1B 116.7 . . ? C1 C2 C5 117.8(17) . . ? C1 C2 H2A 121.1 . . ? C5 C2 H2A 121.1 . . ? C4 C3 C5 120.7(18) . . ? C4 C3 H3B 119.7 . . ? C5 C3 H3B 119.7 . . ? C3 C4 N1 124.6(19) . . ? C3 C4 H4A 117.7 . . ? N1 C4 H4A 117.7 . . ? C3 C5 C2 116.3(16) . . ? C3 C5 C6 122.8(16) . . ? C2 C5 C6 121.0(15) . . ? C9 C6 C7 117.8(16) . . ? C9 C6 C5 121.0(15) . . ? C7 C6 C5 121.1(15) . . ? C8 C7 C6 119.7(16) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? N2 C8 C7 123.6(16) . . ? N2 C8 H8A 118.2 . . ? C7 C8 H8A 118.2 . . ? C6 C9 C10 118.1(16) . . ? C6 C9 H9A 121.0 . . ? C10 C9 H9A 121.0 . . ? N2 C10 C9 124.5(15) . . ? N2 C10 H10A 117.7 . . ? C9 C10 H10A 117.7 . . ? N3 C11 C12 124.1(15) . . ? N3 C11 H11A 118.0 . . ? C12 C11 H11A 118.0 . . ? C11 C12 C15 119.5(15) . . ? C11 C12 H12A 120.3 . . ? C15 C12 H12A 120.3 . . ? N3 C13 C14 125.6(15) . . ? N3 C13 H13A 117.2 . . ? C14 C13 H13A 117.2 . . ? C13 C14 C15 118.7(15) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? C14 C15 C12 116.1(13) . . ? C14 C15 C16 121.9(13) . . ? C12 C15 C16 122.0(13) . . ? C17 C16 C19 116.3(13) . . ? C17 C16 C15 122.7(12) . . ? C19 C16 C15 121.0(13) . . ? C16 C17 C18 120.7(13) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? N4 C18 C17 122.7(14) . . ? N4 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C20 C19 C16 121.3(15) . . ? C20 C19 H19A 119.4 . . ? C16 C19 H19A 119.4 . . ? N4 C20 C19 121.4(14) . . ? N4 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C22 C21 C26 122.0(11) . . ? C22 C21 C27 119.3(12) . . ? C26 C21 C27 118.6(12) . . ? C21 C22 C23 118.6(12) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? C22 C23 C24 118.7(12) . . ? C22 C23 C28 121.2(12) . . ? C24 C23 C28 120.0(12) . . ? C25 C24 C23 121.8(12) . . ? C25 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? C24 C25 C26 119.4(13) . . ? C24 C25 O5 115.8(12) . . ? C26 C25 O5 124.7(13) . . ? C25 C26 C21 119.4(12) . . ? C25 C26 H26A 120.3 . . ? C21 C26 H26A 120.3 . . ? O2 C27 O1 121.8(12) . . ? O2 C27 C21 120.0(13) . . ? O1 C27 C21 118.2(12) . . ? O2 C27 Cd1 63.7(7) . . ? O1 C27 Cd1 58.1(7) . . ? C21 C27 Cd1 176.2(10) . . ? O4 C28 O3 124.9(13) . . ? O4 C28 C23 116.2(14) . . ? O3 C28 C23 118.8(12) . . ? O4 C28 Cd1 52.3(7) . 1_565 ? O3 C28 Cd1 72.7(7) . 1_565 ? C23 C28 Cd1 168.5(11) . 1_565 ? O5 C29 C30 113.0(12) . . ? O5 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? O5 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O6 C30 O7 131.7(18) . . ? O6 C30 C29 114.5(14) . . ? O7 C30 C29 113.7(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.869 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.182 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment 'complex_4.CIF' data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 641178' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22.67 Cd2 N4 O8.34' _chemical_formula_weight 845.41 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5513(4) _cell_length_b 12.2888(4) _cell_length_c 13.3152(5) _cell_angle_alpha 64.5410(10) _cell_angle_beta 72.4970(10) _cell_angle_gamma 62.5390(10) _cell_volume 1501.83(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5062 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.03 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3300 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 835 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .8656 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7884 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5276 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.1000P)^2^+8.9174P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5276 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0592 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.60836(4) -0.12816(4) 0.95602(4) 0.02421(17) Uani 1 1 d . . . Cd2 Cd -0.33330(4) 0.15316(5) 0.74372(4) 0.02639(17) Uani 1 1 d . . . O1 O 0.3110(6) -0.1404(6) 0.9543(4) 0.0474(14) Uani 1 1 d . . . O1W O 0.5818(4) 0.0772(4) 0.9206(4) 0.0262(10) Uani 1 1 d . . . H1 H 0.6101 0.0887 0.9473 0.031 Uiso 1 1 d R . . O2 O 0.4789(5) -0.0971(6) 0.8364(4) 0.0405(13) Uani 1 1 d . . . O2W O -0.013(2) 0.098(2) 0.417(2) 0.071(6) Uani 0.33 1 d P . . O3 O -0.1276(5) 0.0900(6) 0.8116(5) 0.0488(15) Uani 1 1 d . . . O4 O -0.1277(5) 0.1326(6) 0.6347(5) 0.0464(14) Uani 1 1 d . . . O5 O 0.3401(5) 0.1044(5) 0.4580(4) 0.0336(11) Uani 1 1 d . . . O6 O 0.2480(5) 0.1177(5) 0.2179(4) 0.0354(12) Uani 1 1 d . . . O7 O 0.3438(5) -0.0524(5) 0.3615(4) 0.0384(12) Uani 1 1 d . . . N1 N 0.6583(6) -0.3535(6) 1.0452(5) 0.0368(15) Uani 1 1 d . . . N2 N 0.8105(6) -0.2307(6) 1.0350(5) 0.0311(13) Uani 1 1 d . . . N3 N -0.5498(6) 0.2903(6) 0.6940(5) 0.0318(13) Uani 1 1 d . . . N4 N -0.3732(7) 0.3779(6) 0.6945(6) 0.0416(16) Uani 1 1 d . . . C1 C 0.5800(8) -0.4104(8) 1.0535(6) 0.0410(18) Uani 1 1 d . . . H1A H 0.4987 -0.3586 1.0271 0.049 Uiso 1 1 calc R . . C2 C 0.6169(10) -0.5467(9) 1.1011(8) 0.053(2) Uani 1 1 d . . . H2A H 0.5609 -0.5843 1.1054 0.064 Uiso 1 1 calc R . . C3 C 0.7358(11) -0.6234(9) 1.1409(7) 0.054(2) Uani 1 1 d . . . H3A H 0.7615 -0.7136 1.1718 0.065 Uiso 1 1 calc R . . C4 C 0.8192(8) -0.5651(7) 1.1348(6) 0.0408(19) Uani 1 1 d . . . C5 C 0.9460(9) -0.6384(8) 1.1721(7) 0.055(3) Uani 1 1 d . . . H5A H 0.9763 -0.7290 1.2024 0.066 Uiso 1 1 calc R . . C6 C 1.0222(9) -0.5783(9) 1.1641(7) 0.052(2) Uani 1 1 d . . . H6A H 1.1048 -0.6285 1.1881 0.062 Uiso 1 1 calc R . . C7 C 0.9792(8) -0.4383(8) 1.1193(6) 0.043(2) Uani 1 1 d . . . C8 C 1.0543(8) -0.3716(10) 1.1107(7) 0.051(2) Uani 1 1 d . . . H8A H 1.1372 -0.4186 1.1344 0.062 Uiso 1 1 calc R . . C9 C 1.0080(8) -0.2394(10) 1.0682(7) 0.051(2) Uani 1 1 d . . . H9A H 1.0564 -0.1946 1.0649 0.061 Uiso 1 1 calc R . . C10 C 0.8847(8) -0.1723(9) 1.0294(7) 0.0436(19) Uani 1 1 d . . . H10A H 0.8536 -0.0817 0.9981 0.052 Uiso 1 1 calc R . . C11 C 0.8552(7) -0.3634(7) 1.0801(6) 0.0339(16) Uani 1 1 d . . . C12 C 0.7751(7) -0.4278(7) 1.0862(6) 0.0346(17) Uani 1 1 d . . . C13 C -0.2863(11) 0.4200(11) 0.6940(9) 0.064(3) Uani 1 1 d . . . H13A H -0.2066 0.3593 0.7205 0.076 Uiso 1 1 calc R . . C14 C -0.3106(15) 0.5528(13) 0.6549(11) 0.084(4) Uani 1 1 d . . . H14A H -0.2479 0.5792 0.6566 0.101 Uiso 1 1 calc R . . C15 C -0.4240(15) 0.6426(11) 0.6148(10) 0.079(4) Uani 1 1 d . . . H15A H -0.4391 0.7308 0.5881 0.095 Uiso 1 1 calc R . . C16 C -0.5212(11) 0.6033(8) 0.6130(7) 0.055(3) Uani 1 1 d . . . C17 C -0.6427(13) 0.6911(9) 0.5739(7) 0.067(3) Uani 1 1 d . . . H17A H -0.6627 0.7804 0.5478 0.081 Uiso 1 1 calc R . . C18 C -0.7323(12) 0.6479(9) 0.5733(8) 0.066(3) Uani 1 1 d . . . H18A H -0.8114 0.7081 0.5455 0.080 Uiso 1 1 calc R . . C19 C -0.7055(10) 0.5098(9) 0.6155(7) 0.055(3) Uani 1 1 d . . . C20 C -0.7927(9) 0.4568(11) 0.6207(8) 0.060(3) Uani 1 1 d . . . H20A H -0.8751 0.5122 0.5973 0.072 Uiso 1 1 calc R . . C21 C -0.7584(9) 0.3264(10) 0.6594(8) 0.053(2) Uani 1 1 d . . . H21A H -0.8156 0.2914 0.6612 0.064 Uiso 1 1 calc R . . C22 C -0.6354(8) 0.2449(8) 0.6968(6) 0.0385(17) Uani 1 1 d . . . H22A H -0.6126 0.1550 0.7247 0.046 Uiso 1 1 calc R . . C23 C -0.5834(8) 0.4209(7) 0.6539(6) 0.0379(18) Uani 1 1 d . . . C24 C -0.4882(10) 0.4668(8) 0.6554(6) 0.045(2) Uani 1 1 d . . . C25 C 0.2863(6) -0.0328(7) 0.7620(6) 0.0274(14) Uani 1 1 d . . . C26 C 0.1517(7) -0.0035(7) 0.7828(6) 0.0289(15) Uani 1 1 d . . . H26A H 0.1111 -0.0263 0.8563 0.035 Uiso 1 1 calc R . . C27 C 0.0766(7) 0.0608(7) 0.6928(6) 0.0327(16) Uani 1 1 d . . . C28 C 0.1384(7) 0.0934(7) 0.5828(6) 0.0336(16) Uani 1 1 d . . . H28A H 0.0900 0.1326 0.5232 0.040 Uiso 1 1 calc R . . C29 C 0.2709(6) 0.0675(6) 0.5626(5) 0.0235(13) Uani 1 1 d . . . C30 C 0.3456(6) 0.0032(6) 0.6521(5) 0.0253(14) Uani 1 1 d . . . H30A H 0.4354 -0.0154 0.6377 0.030 Uiso 1 1 calc R . . C31 C 0.3641(6) -0.0966(7) 0.8587(5) 0.0272(14) Uani 1 1 d . . . C32 C -0.0688(7) 0.0958(7) 0.7169(6) 0.0323(16) Uani 1 1 d . . . C33 C 0.2796(7) 0.1634(7) 0.3588(5) 0.0287(15) Uani 1 1 d . . . H33A H 0.3187 0.2237 0.3028 0.034 Uiso 1 1 calc R . . H33B H 0.1870 0.2136 0.3754 0.034 Uiso 1 1 calc R . . C34 C 0.2926(6) 0.0664(7) 0.3100(5) 0.0265(14) 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 0.0245(3) 0.0225(3) 0.0211(3) -0.0040(2) -0.00702(19) -0.0061(2) Cd2 0.0242(3) 0.0293(3) 0.0252(3) -0.0061(2) -0.00402(19) -0.0124(2) O1 0.045(3) 0.068(4) 0.029(3) -0.002(3) -0.010(2) -0.032(3) O1W 0.027(2) 0.029(2) 0.022(2) -0.0058(19) -0.0048(18) -0.012(2) O2 0.029(3) 0.066(4) 0.026(3) -0.011(3) -0.008(2) -0.020(3) O2W 0.065(14) 0.078(15) 0.081(15) -0.034(13) 0.005(11) -0.040(12) O3 0.029(3) 0.075(4) 0.035(3) -0.011(3) -0.002(2) -0.022(3) O4 0.025(3) 0.063(4) 0.044(3) -0.010(3) -0.013(2) -0.014(3) O5 0.032(3) 0.052(3) 0.020(2) -0.012(2) -0.002(2) -0.020(2) O6 0.026(3) 0.048(3) 0.032(3) -0.016(2) -0.004(2) -0.012(2) O7 0.043(3) 0.026(3) 0.041(3) -0.006(2) -0.009(2) -0.012(2) N1 0.036(3) 0.029(3) 0.033(3) -0.008(3) -0.008(3) -0.003(3) N2 0.028(3) 0.033(3) 0.022(3) -0.005(2) -0.004(2) -0.008(3) N3 0.035(3) 0.024(3) 0.030(3) -0.007(2) -0.006(3) -0.007(3) N4 0.053(4) 0.036(4) 0.043(4) -0.013(3) -0.003(3) -0.025(3) C1 0.047(5) 0.041(4) 0.033(4) -0.003(3) -0.013(3) -0.020(4) C2 0.070(6) 0.045(5) 0.048(5) -0.012(4) -0.008(5) -0.029(5) C3 0.088(7) 0.034(4) 0.037(5) -0.006(4) -0.011(5) -0.024(5) C4 0.053(5) 0.026(4) 0.027(4) -0.007(3) -0.003(3) -0.006(4) C5 0.054(6) 0.026(4) 0.040(5) -0.002(4) -0.002(4) 0.010(4) C6 0.036(4) 0.050(5) 0.041(5) -0.014(4) -0.014(4) 0.012(4) C7 0.037(4) 0.046(5) 0.026(4) -0.008(3) -0.008(3) -0.001(4) C8 0.036(4) 0.064(6) 0.040(5) -0.017(4) -0.020(4) 0.000(4) C9 0.039(5) 0.067(6) 0.047(5) -0.018(5) -0.011(4) -0.019(4) C10 0.038(4) 0.046(5) 0.041(4) -0.012(4) -0.013(4) -0.009(4) C11 0.040(4) 0.027(4) 0.025(3) -0.008(3) -0.009(3) -0.003(3) C12 0.035(4) 0.027(4) 0.023(3) -0.006(3) -0.007(3) 0.003(3) C13 0.074(7) 0.064(6) 0.073(7) -0.031(5) 0.008(5) -0.046(6) C14 0.119(11) 0.067(8) 0.090(9) -0.042(7) 0.014(8) -0.057(8) C15 0.135(12) 0.039(6) 0.069(7) -0.028(5) 0.026(7) -0.053(7) C16 0.096(7) 0.024(4) 0.030(4) -0.012(3) 0.004(4) -0.017(5) C17 0.113(9) 0.022(4) 0.031(5) -0.003(3) -0.003(5) -0.007(5) C18 0.080(8) 0.035(5) 0.034(5) -0.004(4) -0.012(5) 0.013(5) C19 0.059(6) 0.037(5) 0.030(4) -0.006(4) -0.010(4) 0.009(4) C20 0.043(5) 0.074(7) 0.047(5) -0.032(5) -0.021(4) 0.009(5) C21 0.040(5) 0.067(6) 0.057(6) -0.030(5) -0.012(4) -0.013(4) C22 0.036(4) 0.038(4) 0.038(4) -0.011(3) -0.011(3) -0.010(3) C23 0.045(4) 0.026(4) 0.028(4) -0.008(3) -0.009(3) -0.001(3) C24 0.073(6) 0.037(4) 0.021(4) -0.010(3) 0.004(4) -0.023(4) C25 0.020(3) 0.033(4) 0.026(3) -0.007(3) -0.007(3) -0.009(3) C26 0.030(4) 0.040(4) 0.022(3) -0.008(3) -0.004(3) -0.020(3) C27 0.027(4) 0.039(4) 0.036(4) -0.013(3) -0.005(3) -0.015(3) C28 0.032(4) 0.040(4) 0.026(4) -0.004(3) -0.012(3) -0.013(3) C29 0.027(3) 0.033(3) 0.015(3) -0.009(3) -0.003(2) -0.013(3) C30 0.022(3) 0.026(3) 0.030(4) -0.011(3) -0.003(3) -0.011(3) C31 0.021(3) 0.038(4) 0.021(3) -0.003(3) -0.007(3) -0.013(3) C32 0.025(4) 0.037(4) 0.033(4) -0.004(3) -0.007(3) -0.016(3) C33 0.035(4) 0.026(3) 0.020(3) -0.002(3) -0.009(3) -0.010(3) C34 0.024(3) 0.032(4) 0.023(3) -0.009(3) -0.003(3) -0.012(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 O1W 2.244(5) . ? Cd1 O2 2.303(5) . ? Cd1 O1W 2.316(4) 2_657 ? Cd1 N1 2.350(6) . ? Cd1 O6 2.401(5) 2_656 ? Cd1 N2 2.402(6) . ? Cd1 Cd1 3.4199(9) 2_657 ? Cd1 Cd2 3.6051(7) 1_655 ? Cd2 O1W 2.224(4) 1_455 ? Cd2 O7 2.290(5) 2_556 ? Cd2 O4 2.345(5) . ? Cd2 N3 2.384(6) . ? Cd2 N4 2.392(6) . ? Cd2 O3 2.460(5) . ? Cd2 C32 2.744(7) . ? Cd2 O6 2.851(5) 2_556 ? Cd2 Cd1 3.6051(7) 1_455 ? O1 C31 1.238(8) . ? O1W Cd2 2.224(4) 1_655 ? O1W Cd1 2.316(4) 2_657 ? O1W H1 0.6398 . ? O2 C31 1.266(8) . ? O3 C32 1.228(9) . ? O4 C32 1.267(9) . ? O5 C29 1.381(8) . ? O5 C33 1.422(8) . ? O6 C34 1.258(8) . ? O6 Cd1 2.401(5) 2_656 ? O6 Cd2 2.851(5) 2_556 ? O7 C34 1.240(8) . ? O7 Cd2 2.290(5) 2_556 ? N1 C1 1.334(10) . ? N1 C12 1.352(9) . ? N2 C10 1.318(11) . ? N2 C11 1.362(9) . ? N3 C22 1.327(10) . ? N3 C23 1.351(9) . ? N4 C13 1.321(12) . ? N4 C24 1.349(12) . ? C1 C2 1.407(12) . ? C1 H1A 0.9300 . ? C2 C3 1.367(14) . ? C2 H2A 0.9300 . ? C3 C4 1.409(13) . ? C3 H3A 0.9300 . ? C4 C12 1.411(10) . ? C4 C5 1.428(13) . ? C5 C6 1.345(15) . ? C5 H5A 0.9300 . ? C6 C7 1.438(13) . ? C6 H6A 0.9300 . ? C7 C8 1.397(14) . ? C7 C11 1.412(11) . ? C8 C9 1.355(13) . ? C8 H8A 0.9300 . ? C9 C10 1.403(11) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.438(12) . ? C13 C14 1.396(15) . ? C13 H13A 0.9300 . ? C14 C15 1.341(19) . ? C14 H14A 0.9300 . ? C15 C16 1.421(17) . ? C15 H15A 0.9300 . ? C16 C24 1.415(11) . ? C16 C17 1.403(16) . ? C17 C18 1.366(17) . ? C17 H17A 0.9300 . ? C18 C19 1.447(14) . ? C18 H18A 0.9300 . ? C19 C20 1.404(16) . ? C19 C23 1.406(12) . ? C20 C21 1.347(15) . ? C20 H20A 0.9300 . ? C21 C22 1.398(12) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.457(13) . ? C25 C30 1.388(9) . ? C25 C26 1.390(9) . ? C25 C31 1.503(9) . ? C26 C27 1.411(10) . ? C26 H26A 0.9300 . ? C27 C28 1.395(10) . ? C27 C32 1.497(9) . ? C28 C29 1.376(10) . ? C28 H28A 0.9300 . ? C29 C30 1.403(9) . ? C30 H30A 0.9300 . ? C33 C34 1.519(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? 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 O1W Cd1 O2 101.93(19) . . ? O1W Cd1 O1W 82.81(17) . 2_657 ? O2 Cd1 O1W 87.37(17) . 2_657 ? O1W Cd1 N1 161.6(2) . . ? O2 Cd1 N1 95.5(2) . . ? O1W Cd1 N1 92.26(19) 2_657 . ? O1W Cd1 O6 87.24(17) . 2_656 ? O2 Cd1 O6 77.06(17) . 2_656 ? O1W Cd1 O6 159.39(17) 2_657 2_656 ? N1 Cd1 O6 102.5(2) . 2_656 ? O1W Cd1 N2 95.62(19) . . ? O2 Cd1 N2 152.9(2) . . ? O1W Cd1 N2 115.44(18) 2_657 . ? N1 Cd1 N2 70.4(2) . . ? O6 Cd1 N2 83.39(18) 2_656 . ? O1W Cd1 Cd1 42.21(11) . 2_657 ? O2 Cd1 Cd1 96.00(15) . 2_657 ? O1W Cd1 Cd1 40.61(11) 2_657 2_657 ? N1 Cd1 Cd1 130.48(15) . 2_657 ? O6 Cd1 Cd1 127.03(13) 2_656 2_657 ? N2 Cd1 Cd1 110.80(15) . 2_657 ? O1W Cd1 Cd2 36.01(11) . 1_655 ? O2 Cd1 Cd2 85.39(14) . 1_655 ? O1W Cd1 Cd2 113.92(11) 2_657 1_655 ? N1 Cd1 Cd2 153.81(15) . 1_655 ? O6 Cd1 Cd2 52.11(13) 2_656 1_655 ? N2 Cd1 Cd2 97.31(14) . 1_655 ? Cd1 Cd1 Cd2 75.159(17) 2_657 1_655 ? O1W Cd2 O7 110.44(18) 1_455 2_556 ? O1W Cd2 O4 139.80(18) 1_455 . ? O7 Cd2 O4 82.5(2) 2_556 . ? O1W Cd2 N3 89.70(18) 1_455 . ? O7 Cd2 N3 80.6(2) 2_556 . ? O4 Cd2 N3 130.4(2) . . ? O1W Cd2 N4 109.7(2) 1_455 . ? O7 Cd2 N4 128.8(2) 2_556 . ? O4 Cd2 N4 86.8(2) . . ? N3 Cd2 N4 69.2(2) . . ? O1W Cd2 O3 88.75(17) 1_455 . ? O7 Cd2 O3 121.6(2) 2_556 . ? O4 Cd2 O3 53.97(19) . . ? N3 Cd2 O3 156.6(2) . . ? N4 Cd2 O3 89.4(2) . . ? O1W Cd2 C32 113.93(19) 1_455 . ? O7 Cd2 C32 102.5(2) 2_556 . ? O4 Cd2 C32 27.4(2) . . ? N3 Cd2 C32 152.5(2) . . ? N4 Cd2 C32 88.8(2) . . ? O3 Cd2 C32 26.6(2) . . ? O1W Cd2 O6 77.26(15) 1_455 2_556 ? O7 Cd2 O6 49.86(16) 2_556 2_556 ? O4 Cd2 O6 84.53(18) . 2_556 ? N3 Cd2 O6 116.87(18) . 2_556 ? N4 Cd2 O6 171.28(19) . 2_556 ? O3 Cd2 O6 85.45(19) . 2_556 ? C32 Cd2 O6 83.50(18) . 2_556 ? O1W Cd2 Cd1 36.38(12) 1_455 1_455 ? O7 Cd2 Cd1 77.86(13) 2_556 1_455 ? O4 Cd2 Cd1 121.15(15) . 1_455 ? N3 Cd2 Cd1 100.12(14) . 1_455 ? N4 Cd2 Cd1 145.92(16) . 1_455 ? O3 Cd2 Cd1 92.33(14) . 1_455 ? C32 Cd2 Cd1 107.28(15) . 1_455 ? O6 Cd2 Cd1 41.64(10) 2_556 1_455 ? Cd2 O1W Cd1 107.61(19) 1_655 . ? Cd2 O1W Cd1 141.6(2) 1_655 2_657 ? Cd1 O1W Cd1 97.19(17) . 2_657 ? Cd2 O1W H1 102.4 1_655 . ? Cd1 O1W H1 120.5 . . ? Cd1 O1W H1 88.9 2_657 . ? C31 O2 Cd1 128.6(4) . . ? C32 O3 Cd2 89.7(4) . . ? C32 O4 Cd2 94.1(4) . . ? C29 O5 C33 121.1(5) . . ? C34 O6 Cd1 121.3(4) . 2_656 ? C34 O6 Cd2 78.6(4) . 2_556 ? Cd1 O6 Cd2 86.25(15) 2_656 2_556 ? C34 O7 Cd2 105.5(4) . 2_556 ? C1 N1 C12 119.4(7) . . ? C1 N1 Cd1 123.3(5) . . ? C12 N1 Cd1 117.2(5) . . ? C10 N2 C11 118.8(7) . . ? C10 N2 Cd1 126.4(5) . . ? C11 N2 Cd1 114.6(5) . . ? C22 N3 C23 118.5(7) . . ? C22 N3 Cd2 123.3(5) . . ? C23 N3 Cd2 118.0(5) . . ? C13 N4 C24 118.5(8) . . ? C13 N4 Cd2 124.5(7) . . ? C24 N4 Cd2 116.8(5) . . ? N1 C1 C2 121.8(8) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 119.5(9) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C12 117.5(8) . . ? C3 C4 C5 123.2(8) . . ? C12 C4 C5 119.3(8) . . ? C6 C5 C4 121.0(8) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C7 121.7(8) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C8 C7 C11 117.7(8) . . ? C8 C7 C6 123.7(8) . . ? C11 C7 C6 118.6(8) . . ? C9 C8 C7 120.9(8) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 117.8(9) . . ? C8 C9 H9A 121.1 . . ? C10 C9 H9A 121.1 . . ? N2 C10 C9 123.6(8) . . ? N2 C10 H10A 118.2 . . ? C9 C10 H10A 118.2 . . ? N2 C11 C7 121.1(8) . . ? N2 C11 C12 119.1(6) . . ? C7 C11 C12 119.7(7) . . ? N1 C12 C4 122.1(8) . . ? N1 C12 C11 118.2(7) . . ? C4 C12 C11 119.7(7) . . ? N4 C13 C14 122.0(12) . . ? N4 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 120.4(12) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.2(9) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C24 115.3(10) . . ? C15 C16 C17 123.7(9) . . ? C24 C16 C17 121.0(10) . . ? C18 C17 C16 121.2(9) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 120.8(10) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C23 116.9(8) . . ? C20 C19 C18 124.8(9) . . ? C23 C19 C18 118.4(10) . . ? C21 C20 C19 120.7(8) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 118.8(9) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? N3 C22 C21 122.8(8) . . ? N3 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? N3 C23 C19 122.4(8) . . ? N3 C23 C24 116.8(7) . . ? C19 C23 C24 120.8(8) . . ? N4 C24 C16 123.7(9) . . ? N4 C24 C23 118.7(7) . . ? C16 C24 C23 117.6(9) . . ? C30 C25 C26 119.4(6) . . ? C30 C25 C31 120.9(6) . . ? C26 C25 C31 119.6(6) . . ? C25 C26 C27 120.2(6) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 119.6(6) . . ? C28 C27 C32 120.9(7) . . ? C26 C27 C32 119.5(6) . . ? C29 C28 C27 120.0(6) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 O5 124.9(6) . . ? C28 C29 C30 120.3(6) . . ? O5 C29 C30 114.7(6) . . ? C25 C30 C29 120.4(6) . . ? C25 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? O1 C31 O2 124.5(6) . . ? O1 C31 C25 118.5(6) . . ? O2 C31 C25 116.9(6) . . ? O3 C32 O4 122.0(7) . . ? O3 C32 C27 121.3(7) . . ? O4 C32 C27 116.6(7) . . ? O3 C32 Cd2 63.7(4) . . ? O4 C32 Cd2 58.5(4) . . ? C27 C32 Cd2 174.4(5) . . ? O5 C33 C34 113.9(6) . . ? O5 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? O5 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? O7 C34 O6 126.0(7) . . ? O7 C34 C33 119.6(6) . . ? O6 C34 C33 114.5(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.685 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.120 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment 'complex_5.CIF' data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 641179' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H60 N8 O34 Zn8' _chemical_formula_weight 2200.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 9.424(18) _cell_length_b 14.37(3) _cell_length_c 15.40(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.87(6) _cell_angle_gamma 90.00 _cell_volume 2015(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour white _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 2.436 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7681 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15378 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4620 _reflns_number_gt 3876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0755P)^2^+1.4073P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4620 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0607 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.57789(4) 0.13206(3) 0.15016(3) 0.03106(15) Uani 1 1 d . . . Zn2 Zn -0.40607(4) 0.13118(3) 0.00249(3) 0.03069(14) Uani 1 1 d . . . O1W O -0.4715(13) -0.0810(8) 0.3488(7) 0.123(4) Uani 0.50 1 d P . . O4 O -0.2516(3) 0.1039(2) -0.05345(18) 0.0401(6) Uani 1 1 d . . . O5 O -0.4053(3) 0.07963(18) 0.11690(16) 0.0338(6) Uani 1 1 d . . . O8 O -0.3679(3) 0.0216(2) -0.17420(17) 0.0383(6) Uani 1 1 d . . . N1 N -0.7549(3) 0.1708(2) 0.2045(2) 0.0334(7) Uani 1 1 d . . . N2 N -0.4770(4) 0.1435(2) 0.2894(2) 0.0366(7) Uani 1 1 d . . . C1 C -0.8936(5) 0.1821(3) 0.1579(3) 0.0469(10) Uani 1 1 d . . . H1A H -0.9160 0.1759 0.0958 0.056 Uiso 1 1 calc R . . C2 C -1.0062(5) 0.2025(4) 0.1974(4) 0.0654(14) Uani 1 1 d . . . H2A H -1.1022 0.2103 0.1630 0.078 Uiso 1 1 calc R . . C3 C -0.9707(6) 0.2108(4) 0.2894(4) 0.0692(16) Uani 1 1 d . . . H3A H -1.0432 0.2254 0.3183 0.083 Uiso 1 1 calc R . . C4 C -0.8283(6) 0.1974(4) 0.3387(3) 0.0585(13) Uani 1 1 d . . . H4A H -0.8042 0.2020 0.4010 0.070 Uiso 1 1 calc R . . C5 C -0.7219(5) 0.1772(3) 0.2948(2) 0.0383(9) Uani 1 1 d . . . C6 C -0.5657(5) 0.1629(3) 0.3422(3) 0.0405(9) Uani 1 1 d . . . C7 C -0.5111(6) 0.1678(4) 0.4345(3) 0.0604(13) Uani 1 1 d . . . H7A H -0.5732 0.1809 0.4712 0.072 Uiso 1 1 calc R . . C8 C -0.3627(7) 0.1529(4) 0.4715(3) 0.0678(16) Uani 1 1 d . . . H8A H -0.3244 0.1557 0.5334 0.081 Uiso 1 1 calc R . . C9 C -0.2733(6) 0.1341(3) 0.4175(4) 0.0653(16) Uani 1 1 d . . . H9A H -0.1734 0.1244 0.4416 0.078 Uiso 1 1 calc R . . C10 C -0.3339(5) 0.1296(3) 0.3258(3) 0.0523(12) Uani 1 1 d . . . H10A H -0.2732 0.1166 0.2883 0.063 Uiso 1 1 calc R . . C11 C -0.1194(4) 0.0677(2) -0.1588(2) 0.0283(7) Uani 1 1 d . . . C12 C 0.0116(4) 0.0885(2) -0.0970(2) 0.0279(7) Uani 1 1 d . . . H12A H 0.0131 0.0974 -0.0369 0.033 Uiso 1 1 calc R . . C13 C -0.1208(4) 0.0517(2) -0.2483(2) 0.0302(7) Uani 1 1 d . . . H13A H -0.2079 0.0357 -0.2899 0.036 Uiso 1 1 calc R . . C14 C -0.2587(4) 0.0630(3) -0.1282(2) 0.0309(7) Uani 1 1 d . . . C15 C 0.0084(4) 0.0596(2) -0.2749(2) 0.0297(7) Uani 1 1 d . . . C16 C 0.1394(4) 0.0820(2) -0.2143(2) 0.0304(7) Uani 1 1 d . . . H16A H 0.2254 0.0875 -0.2330 0.036 Uiso 1 1 calc R . . C17 C 0.1400(4) 0.0962(2) -0.1241(2) 0.0276(7) Uani 1 1 d . . . C20 C 0.2814(4) 0.1162(2) -0.0545(2) 0.0273(7) Uani 1 1 d . . . O2 O 0.2746(3) 0.12441(19) 0.02436(16) 0.0368(6) Uani 1 1 d . . . O3 O 0.3963(3) 0.12342(18) -0.08227(17) 0.0353(6) Uani 1 1 d . . . O1 O -0.0022(3) 0.04099(18) -0.36475(15) 0.0360(6) Uani 1 1 d . . . C18 C 0.0950(4) 0.0902(3) -0.4060(2) 0.0350(8) Uani 1 1 d . . . H18A H 0.0878 0.0637 -0.4649 0.042 Uiso 1 1 calc R . . H18B H 0.1950 0.0815 -0.3703 0.042 Uiso 1 1 calc R . . C19 C 0.0630(4) 0.1938(2) -0.4162(2) 0.0291(7) Uani 1 1 d . . . O6 O -0.0263(3) 0.22820(19) -0.37836(18) 0.0398(6) Uani 1 1 d . . . O7 O 0.1333(3) 0.23491(19) -0.46435(18) 0.0424(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0217(2) 0.0483(3) 0.0242(2) -0.00451(16) 0.00779(17) -0.00195(16) Zn2 0.0221(2) 0.0427(3) 0.0300(2) -0.00440(16) 0.01168(17) -0.00184(16) O1W 0.116(9) 0.116(8) 0.111(8) 0.032(7) -0.017(7) -0.023(7) O4 0.0229(13) 0.0601(17) 0.0411(14) -0.0132(13) 0.0152(11) -0.0053(12) O5 0.0242(13) 0.0455(15) 0.0340(12) 0.0007(11) 0.0115(10) 0.0032(10) O8 0.0228(13) 0.0517(16) 0.0399(13) -0.0044(12) 0.0073(11) -0.0085(11) N1 0.0307(16) 0.0424(17) 0.0290(14) -0.0055(13) 0.0112(13) -0.0007(13) N2 0.0343(18) 0.0430(18) 0.0295(15) -0.0055(13) 0.0026(14) -0.0036(13) C1 0.032(2) 0.068(3) 0.042(2) -0.011(2) 0.0108(18) 0.0047(19) C2 0.035(2) 0.098(4) 0.065(3) -0.021(3) 0.015(2) 0.011(2) C3 0.054(3) 0.103(4) 0.065(3) -0.028(3) 0.042(3) -0.004(3) C4 0.062(3) 0.078(3) 0.045(2) -0.015(2) 0.031(2) -0.008(3) C5 0.048(2) 0.041(2) 0.0291(17) -0.0080(15) 0.0165(17) -0.0063(17) C6 0.050(2) 0.041(2) 0.0305(18) -0.0058(16) 0.0104(18) -0.0059(18) C7 0.078(4) 0.070(3) 0.031(2) -0.008(2) 0.009(2) -0.002(3) C8 0.077(4) 0.077(3) 0.034(2) -0.011(2) -0.014(3) 0.006(3) C9 0.059(3) 0.066(3) 0.054(3) -0.012(2) -0.018(3) 0.007(2) C10 0.034(2) 0.072(3) 0.045(2) -0.008(2) -0.002(2) 0.003(2) C11 0.0228(17) 0.0339(18) 0.0292(16) -0.0002(13) 0.0084(14) -0.0008(13) C12 0.0231(17) 0.0387(19) 0.0230(14) -0.0022(13) 0.0079(13) 0.0014(14) C13 0.0249(18) 0.0352(19) 0.0283(16) -0.0023(14) 0.0026(14) -0.0032(14) C14 0.0256(18) 0.0384(19) 0.0296(16) 0.0003(14) 0.0085(14) 0.0008(14) C15 0.0286(18) 0.0328(18) 0.0280(16) -0.0006(13) 0.0078(14) -0.0002(14) C16 0.0272(18) 0.040(2) 0.0271(15) 0.0016(14) 0.0118(14) -0.0018(14) C17 0.0217(17) 0.0377(18) 0.0236(15) -0.0007(13) 0.0059(13) 0.0023(14) C20 0.0202(16) 0.0355(18) 0.0268(15) -0.0003(13) 0.0073(13) 0.0018(13) O2 0.0217(13) 0.0640(18) 0.0243(12) -0.0052(11) 0.0050(10) -0.0008(11) O3 0.0202(12) 0.0562(17) 0.0307(12) -0.0026(11) 0.0084(10) -0.0023(11) O1 0.0420(15) 0.0429(15) 0.0251(11) -0.0058(10) 0.0121(11) -0.0093(12) C18 0.038(2) 0.043(2) 0.0291(16) -0.0022(15) 0.0172(16) 0.0002(16) C19 0.0248(17) 0.0401(19) 0.0213(14) -0.0003(13) 0.0039(13) 0.0011(14) O6 0.0408(15) 0.0393(14) 0.0442(14) 0.0009(12) 0.0201(13) 0.0063(12) O7 0.0510(17) 0.0455(15) 0.0387(14) 0.0057(12) 0.0259(13) 0.0049(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.975(4) . ? Zn1 O2 2.078(4) 1_455 ? Zn1 N2 2.118(5) . ? Zn1 N1 2.123(4) . ? Zn1 O6 2.138(5) 4_566 ? Zn1 O8 2.317(5) 3_455 ? Zn1 Zn2 3.112(5) . ? Zn2 O5 1.910(4) . ? Zn2 O4 1.913(4) . ? Zn2 O3 1.984(4) 1_455 ? Zn2 O7 2.001(5) 4_566 ? O4 C14 1.279(5) . ? O8 C14 1.241(5) . ? O8 Zn1 2.317(5) 3_455 ? N1 C1 1.330(6) . ? N1 C5 1.348(5) . ? N2 C6 1.336(6) . ? N2 C10 1.336(6) . ? C1 C2 1.383(6) . ? C2 C3 1.375(8) . ? C3 C4 1.375(8) . ? C4 C5 1.377(6) . ? C5 C6 1.480(7) . ? C6 C7 1.385(6) . ? C7 C8 1.385(8) . ? C8 C9 1.354(9) . ? C9 C10 1.383(7) . ? C11 C12 1.384(5) . ? C11 C13 1.395(5) . ? C11 C14 1.505(5) . ? C12 C17 1.382(5) . ? C13 C15 1.386(5) . ? C15 C16 1.381(5) . ? C15 O1 1.388(5) . ? C16 C17 1.404(5) . ? C17 C20 1.508(5) . ? C20 O2 1.238(5) . ? C20 O3 1.267(5) . ? O2 Zn1 2.078(4) 1_655 ? O3 Zn2 1.984(4) 1_655 ? O1 C18 1.429(5) . ? C18 C19 1.518(6) . ? C19 O6 1.242(5) . ? C19 O7 1.261(5) . ? O6 Zn1 2.138(5) 4_665 ? O7 Zn2 2.001(5) 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 O5 Zn1 O2 97.85(16) . 1_455 ? O5 Zn1 N2 96.13(16) . . ? O2 Zn1 N2 165.39(12) 1_455 . ? O5 Zn1 N1 169.87(12) . . ? O2 Zn1 N1 88.62(18) 1_455 . ? N2 Zn1 N1 76.96(17) . . ? O5 Zn1 O6 93.37(14) . 4_566 ? O2 Zn1 O6 89.49(12) 1_455 4_566 ? N2 Zn1 O6 93.94(13) . 4_566 ? N1 Zn1 O6 94.48(14) . 4_566 ? O5 Zn1 O8 84.73(14) . 3_455 ? O2 Zn1 O8 88.65(11) 1_455 3_455 ? N2 Zn1 O8 88.40(12) . 3_455 ? N1 Zn1 O8 87.65(14) . 3_455 ? O6 Zn1 O8 177.15(10) 4_566 3_455 ? O5 Zn1 Zn2 36.06(8) . . ? O2 Zn1 Zn2 70.58(17) 1_455 . ? N2 Zn1 Zn2 123.92(16) . . ? N1 Zn1 Zn2 153.86(9) . . ? O6 Zn1 Zn2 70.43(9) 4_566 . ? O8 Zn1 Zn2 106.88(8) 3_455 . ? O5 Zn2 O4 120.87(14) . . ? O5 Zn2 O3 111.47(15) . 1_455 ? O4 Zn2 O3 112.74(19) . 1_455 ? O5 Zn2 O7 100.42(15) . 4_566 ? O4 Zn2 O7 101.47(13) . 4_566 ? O3 Zn2 O7 107.66(12) 1_455 4_566 ? O5 Zn2 Zn1 37.51(10) . . ? O4 Zn2 Zn1 158.26(9) . . ? O3 Zn2 Zn1 84.52(17) 1_455 . ? O7 Zn2 Zn1 84.66(9) 4_566 . ? C14 O4 Zn2 129.0(2) . . ? Zn2 O5 Zn1 106.44(14) . . ? C14 O8 Zn1 123.4(2) . 3_455 ? C1 N1 C5 118.8(3) . . ? C1 N1 Zn1 125.6(3) . . ? C5 N1 Zn1 115.4(3) . . ? C6 N2 C10 119.9(4) . . ? C6 N2 Zn1 116.3(3) . . ? C10 N2 Zn1 123.7(3) . . ? N1 C1 C2 123.2(4) . . ? C3 C2 C1 117.4(5) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 119.3(4) . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 115.8(3) . . ? C4 C5 C6 123.0(4) . . ? N2 C6 C7 120.6(4) . . ? N2 C6 C5 115.3(4) . . ? C7 C6 C5 124.0(4) . . ? C6 C7 C8 118.9(5) . . ? C9 C8 C7 120.0(5) . . ? C8 C9 C10 118.6(5) . . ? N2 C10 C9 121.9(5) . . ? C12 C11 C13 119.7(3) . . ? C12 C11 C14 119.3(3) . . ? C13 C11 C14 120.9(3) . . ? C17 C12 C11 120.3(3) . . ? C15 C13 C11 119.5(3) . . ? O8 C14 O4 125.4(3) . . ? O8 C14 C11 120.3(3) . . ? O4 C14 C11 114.3(3) . . ? C16 C15 C13 121.4(3) . . ? C16 C15 O1 122.8(3) . . ? C13 C15 O1 115.8(3) . . ? C15 C16 C17 118.6(3) . . ? C12 C17 C16 120.4(3) . . ? C12 C17 C20 118.9(3) . . ? C16 C17 C20 120.6(3) . . ? O2 C20 O3 126.0(3) . . ? O2 C20 C17 117.2(3) . . ? O3 C20 C17 116.9(3) . . ? C20 O2 Zn1 136.8(3) . 1_655 ? C20 O3 Zn2 121.5(3) . 1_655 ? C15 O1 C18 117.2(3) . . ? O1 C18 C19 113.5(3) . . ? O6 C19 O7 127.7(4) . . ? O6 C19 C18 118.8(3) . . ? O7 C19 C18 113.5(3) . . ? C19 O6 Zn1 133.4(3) . 4_665 ? C19 O7 Zn2 120.6(3) . 4_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.887 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.154 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ;