# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'O. Reinaud' _publ_contact_author_address # Name and address of author for correspondence ; Pr O. Reinaud Laboratoire de Chimie et Biochimie Pharmacologiques et Toxicologiques, UMR CNRS 8601 Universite Rene Descartes, 45 rue des Saints Peres 75270 Paris Cedex 06 France ; _publ_contact_author_phone '(33) 1 42 86 21 83' _publ_contact_author_fax '(33) 1 42 86 83 87' _publ_contact_author_email Olivia.Reinaud@univ-paris5.fr # 3. title and author list _publ_section_title ; Encapsulation of a (H~3~O~2~)^-^ Unit in the Aromatic Core of a Calix[6]arene Closed by Two Zn(II) Ions at the Small and Large Rims ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address D.Coquiere ; Laboratoire de Chimie et Biochimie Pharmacologiques et Toxicologiques, UMR CNRS 8601 Universite Rene Descartes, 45 rue des Saints P\`eres 75270 Paris Cedex 06 France ; J.Marrot ; Institut Lavoisier de Versailles, UMR CNRS 8180 Universite de Versailles 45 Avenue des Etats Unis 78035 Versailles Cedex France ; O.Reinaud ; Laboratoire de Chimie et Biochimie Pharmacologiques et Toxicologiques, UMR CNRS 8601 Universite Rene Descartes, 45 rue des Saints P\`eres 75270 Paris Cedex 06 France ; #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of Gottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #==================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 610232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H87 Cl3 N9 O21 Zn2' _chemical_formula_weight 1651.60 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 18.9573(7) _cell_length_b 18.9573(7) _cell_length_c 12.5640(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3910.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4089 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.62 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1722 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9249 _exptl_absorpt_correction_T_max 0.9690 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(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 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61565 _diffrn_reflns_av_R_equivalents 0.1492 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 22.47 _reflns_number_total 3394 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1966P)^2^+9.4044P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(6) _refine_ls_number_reflns 3394 _refine_ls_number_parameters 336 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.3044 _refine_ls_wR_factor_gt 0.2737 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.6667 0.3333 -0.1677(2) 0.0914(11) Uani 1 3 d S . . Zn2 Zn 0.6667 0.3333 0.2944(2) 0.0869(11) Uani 1 3 d S . . N1 N 0.5724(10) 0.3474(9) -0.2119(10) 0.079(3) Uani 1 1 d . . . C2 C 0.572(2) 0.4096(10) -0.2785(12) 0.126(10) Uani 1 1 d . . . H2 H 0.6171 0.4512 -0.3161 0.152 Uiso 1 1 calc R . . C3 C 0.4933(16) 0.3969(15) -0.2769(16) 0.118(8) Uani 1 1 d . . . H3 H 0.4744 0.4289 -0.3113 0.142 Uiso 1 1 calc R . . N4 N 0.4523(10) 0.3346(8) -0.2209(9) 0.080(4) Uani 1 1 d . . . C5 C 0.4982(14) 0.3042(10) -0.1855(11) 0.085(5) Uani 1 1 d . . . C6 C 0.4674(9) 0.2334(8) -0.1082(10) 0.065(3) Uani 1 1 d . . . H6A H 0.4104 0.1926 -0.1259 0.078 Uiso 1 1 calc R . . H6B H 0.5008 0.2069 -0.1146 0.078 Uiso 1 1 calc R . . O7 O 0.4713(5) 0.2610(5) -0.0022(7) 0.0550(19) Uani 1 1 d . . . C8 C 0.4002(6) 0.2397(6) 0.0579(11) 0.048(3) Uani 1 1 d . . . C9 C 0.3821(6) 0.2999(7) 0.0790(9) 0.048(3) Uani 1 1 d . . . C10 C 0.3142(7) 0.2778(8) 0.1420(9) 0.057(3) Uani 1 1 d . . . H10 H 0.3026 0.3192 0.1626 0.068 Uiso 1 1 calc R . . C11 C 0.2640(7) 0.2018(7) 0.1756(10) 0.055(3) Uani 1 1 d . . . C12 C 0.2833(7) 0.1428(8) 0.1511(10) 0.053(3) Uani 1 1 d . . . H12 H 0.2490 0.0889 0.1764 0.064 Uiso 1 1 calc R . . C13 C 0.3525(7) 0.1596(7) 0.0894(9) 0.055(3) Uani 1 1 d . . . C14 C 0.7224(6) 0.6281(7) 0.0679(11) 0.050(2) Uani 1 1 d . . . H14A H 0.7153 0.6282 -0.0102 0.060 Uiso 1 1 calc R . . H14B H 0.7152 0.6723 0.0979 0.060 Uiso 1 1 calc R . . C15 C 0.6551(6) 0.5475(6) 0.1115(10) 0.049(3) Uani 1 1 d . . . C16 C 0.5825(7) 0.5012(6) 0.0608(11) 0.049(3) Uani 1 1 d . . . C17 C 0.5210(7) 0.4308(8) 0.1001(10) 0.055(3) Uani 1 1 d . . . C18 C 0.5318(7) 0.4019(7) 0.1952(9) 0.052(3) Uani 1 1 d . . . H18 H 0.4894 0.3529 0.2250 0.062 Uiso 1 1 calc R . . C19 C 0.6073(7) 0.4467(8) 0.2478(10) 0.058(3) Uani 1 1 d . . . C20 C 0.6662(7) 0.5164(8) 0.2088(10) 0.060(3) Uani 1 1 d . . . H20 H 0.7162 0.5457 0.2462 0.072 Uiso 1 1 calc R . . C21 C 0.4369(6) 0.3844(6) 0.0447(11) 0.055(3) Uani 1 1 d . . . H21A H 0.4085 0.4157 0.0559 0.066 Uiso 1 1 calc R . . H21B H 0.4462 0.3840 -0.0327 0.066 Uiso 1 1 calc R . . N22 N 0.6225(7) 0.4095(7) 0.3421(8) 0.074(3) Uani 1 1 d . . . H22A H 0.5749 0.3800 0.3798 0.089 Uiso 1 1 calc R . . H22B H 0.6598 0.4498 0.3859 0.089 Uiso 1 1 calc R . . O23 O 0.5754(5) 0.5228(5) -0.0467(6) 0.055(2) Uani 1 1 d . . . C24 C 0.5464(11) 0.5785(10) -0.0512(11) 0.084(4) Uani 1 1 d . . . H24A H 0.4878 0.5497 -0.0367 0.126 Uiso 1 1 calc R . . H24B H 0.5567 0.6031 -0.1222 0.126 Uiso 1 1 calc R . . H24C H 0.5747 0.6213 0.0022 0.126 Uiso 1 1 calc R . . C25 C 0.3645(13) 0.3018(10) -0.2168(14) 0.095(6) Uani 1 1 d . . . H25A H 0.3392 0.2683 -0.2800 0.143 Uiso 1 1 calc R . . H25B H 0.3530 0.3467 -0.2149 0.143 Uiso 1 1 calc R . . H25C H 0.3424 0.2683 -0.1528 0.143 Uiso 1 1 calc R . . C26 C 0.1869(8) 0.1824(10) 0.2450(12) 0.078(4) Uani 1 1 d . . . C27 C 0.1552(15) 0.1031(13) 0.303(2) 0.151(11) Uani 1 1 d . . . H27A H 0.1174 0.0993 0.3586 0.227 Uiso 1 1 calc R . . H27B H 0.2008 0.1002 0.3348 0.227 Uiso 1 1 calc R . . H27C H 0.1267 0.0580 0.2524 0.227 Uiso 1 1 calc R . . C28 C 0.2122(17) 0.2439(13) 0.333(3) 0.207(19) Uani 1 1 d . . . H28A H 0.1808 0.2174 0.3974 0.311 Uiso 1 1 calc R . . H28B H 0.2020 0.2877 0.3116 0.311 Uiso 1 1 calc R . . H28C H 0.2704 0.2667 0.3477 0.311 Uiso 1 1 calc R . . C29 C 0.1269(11) 0.1910(15) 0.168(3) 0.152(10) Uani 1 1 d . . . H29A H 0.0985 0.1420 0.1240 0.227 Uiso 1 1 calc R . . H29B H 0.1575 0.2387 0.1224 0.227 Uiso 1 1 calc R . . H29C H 0.0870 0.1978 0.2099 0.227 Uiso 1 1 calc R . . O30 O 0.705(2) 0.370(2) -0.019(4) 0.129(17) Uani 0.33 1 d P . . O31 O 0.6667 0.3333 0.1469(19) 0.22(2) Uani 1 3 d S . . Cl1 Cl 0.7781(3) 0.5762(3) 0.5100(3) 0.0820(11) Uani 1 1 d . . . O1 O 0.8558(11) 0.6403(10) 0.5351(13) 0.146(6) Uani 1 1 d . . . O2 O 0.7721(10) 0.5008(12) 0.5065(16) 0.074(4) Uani 0.50 1 d P . . O3 O 0.745(2) 0.611(2) 0.4625(18) 0.29(2) Uani 1 1 d . . . O4 O 0.7431(17) 0.5604(15) 0.6220(19) 0.207(10) Uani 1 1 d . . . O5 O 0.7983(11) 0.5367(13) 0.4201(16) 0.074(4) Uani 0.50 1 d P . . O1W O 0.6667 0.3333 0.519(3) 0.179(13) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.1168(17) 0.1168(17) 0.0407(17) 0.000 0.000 0.0584(9) Zn2 0.1062(16) 0.1062(16) 0.0481(19) 0.000 0.000 0.0531(8) N1 0.105(10) 0.095(9) 0.040(6) 0.022(6) 0.003(6) 0.052(8) C2 0.23(3) 0.064(10) 0.030(9) 0.014(7) 0.002(12) 0.030(13) C3 0.131(17) 0.149(19) 0.079(14) 0.013(13) -0.053(13) 0.074(16) N4 0.134(12) 0.075(8) 0.037(7) 0.011(6) 0.009(7) 0.056(8) C5 0.160(18) 0.072(9) 0.034(8) 0.017(7) -0.011(9) 0.067(11) C6 0.099(10) 0.063(8) 0.039(8) 0.003(6) 0.008(7) 0.045(8) O7 0.075(5) 0.067(5) 0.040(4) 0.008(4) 0.005(4) 0.048(4) C8 0.045(6) 0.054(6) 0.061(7) -0.006(6) -0.010(6) 0.036(5) C9 0.042(6) 0.065(7) 0.043(7) -0.012(5) -0.016(5) 0.031(5) C10 0.061(8) 0.069(8) 0.047(7) -0.029(6) -0.024(6) 0.038(7) C11 0.055(7) 0.051(7) 0.047(8) -0.001(5) 0.001(6) 0.017(6) C12 0.042(6) 0.055(7) 0.060(7) -0.016(6) -0.002(6) 0.022(5) C13 0.064(7) 0.049(7) 0.043(8) -0.014(5) -0.019(5) 0.022(6) C14 0.050(6) 0.077(7) 0.033(5) 0.011(6) 0.011(6) 0.038(5) C15 0.050(6) 0.045(6) 0.062(8) 0.009(5) 0.011(6) 0.030(5) C16 0.063(7) 0.051(6) 0.046(6) -0.001(6) -0.004(6) 0.039(6) C17 0.057(7) 0.065(8) 0.054(8) -0.009(6) -0.012(6) 0.039(7) C18 0.043(6) 0.069(7) 0.034(6) 0.022(5) 0.019(5) 0.021(6) C19 0.055(7) 0.065(8) 0.058(8) 0.019(6) 0.010(6) 0.033(7) C20 0.046(7) 0.086(9) 0.047(7) 0.009(7) -0.003(6) 0.032(7) C21 0.056(6) 0.057(7) 0.064(9) 0.003(6) 0.002(6) 0.036(6) N22 0.078(7) 0.096(8) 0.036(6) 0.029(6) -0.001(5) 0.034(7) O23 0.076(5) 0.065(5) 0.036(4) 0.013(4) 0.000(4) 0.045(4) C24 0.126(13) 0.111(12) 0.032(7) -0.010(7) -0.005(7) 0.071(11) C25 0.154(17) 0.088(11) 0.064(10) -0.014(8) -0.048(11) 0.075(12) C26 0.048(7) 0.094(11) 0.066(9) -0.022(8) 0.002(6) 0.016(7) C27 0.19(2) 0.117(15) 0.17(2) 0.048(15) 0.13(2) 0.092(16) C28 0.17(2) 0.086(13) 0.25(3) -0.075(18) 0.14(2) -0.022(14) C29 0.066(11) 0.148(19) 0.22(3) 0.050(19) 0.025(15) 0.035(12) O30 0.13(4) 0.08(2) 0.20(5) -0.10(3) -0.04(3) 0.068(19) O31 0.32(3) 0.32(3) 0.017(12) 0.000 0.000 0.160(16) Cl1 0.095(3) 0.097(3) 0.069(2) -0.006(2) -0.003(2) 0.060(2) O1 0.177(14) 0.138(11) 0.099(12) -0.023(9) 0.011(10) 0.061(11) O2 0.068(8) 0.108(11) 0.059(8) -0.040(8) -0.009(7) 0.052(8) O3 0.41(4) 0.59(6) 0.152(19) -0.18(3) -0.12(2) 0.45(5) O4 0.25(3) 0.187(19) 0.17(2) 0.074(15) -0.002(17) 0.106(19) O5 0.068(8) 0.108(11) 0.059(8) -0.040(8) -0.009(7) 0.052(8) O1W 0.23(2) 0.23(2) 0.09(2) 0.000 0.000 0.113(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O30 2.00(5) . ? Zn1 O30 2.00(5) 3_665 ? Zn1 O30 2.00(5) 2_655 ? Zn1 N1 2.012(14) 2_655 ? Zn1 N1 2.012(14) . ? Zn1 N1 2.012(14) 3_665 ? Zn2 O31 1.85(2) . ? Zn2 N22 2.088(13) 2_655 ? Zn2 N22 2.088(13) 3_665 ? Zn2 N22 2.088(13) . ? N1 C5 1.27(2) . ? N1 C2 1.45(2) . ? C2 C3 1.39(3) . ? C2 H2 0.9500 . ? C3 N4 1.26(2) . ? C3 H3 0.9500 . ? N4 C5 1.34(2) . ? N4 C25 1.46(2) . ? C5 C6 1.52(2) . ? C6 O7 1.418(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.417(14) . ? C8 C9 1.373(15) . ? C8 C13 1.381(16) . ? C9 C10 1.385(17) . ? C9 C21 1.472(15) . ? C10 C11 1.338(17) . ? C10 H10 0.9500 . ? C11 C12 1.373(16) . ? C11 C26 1.580(18) . ? C12 C13 1.416(17) . ? C12 H12 0.9500 . ? C13 C14 1.481(16) 2_655 ? C14 C13 1.481(16) 3_665 ? C14 C15 1.521(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.365(16) . ? C15 C20 1.417(17) . ? C16 C17 1.352(17) . ? C16 O23 1.437(15) . ? C17 C18 1.372(16) . ? C17 C21 1.547(17) . ? C18 C19 1.411(18) . ? C18 H18 0.9500 . ? C19 C20 1.326(18) . ? C19 N22 1.479(16) . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N22 H22A 0.9200 . ? N22 H22B 0.9200 . ? O23 C24 1.416(16) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.50(3) . ? C26 C28 1.50(3) . ? C26 C29 1.56(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O30 O30 1.22(6) 2_655 ? O30 O30 1.22(6) 3_665 ? Cl1 O3 1.27(2) . ? Cl1 O2 1.38(2) . ? Cl1 O1 1.398(16) . ? Cl1 O5 1.505(17) . ? Cl1 O4 1.52(2) . ? O2 O5 1.25(3) . ? 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 O30 Zn1 O30 36(2) . 3_665 ? O30 Zn1 O30 36(2) . 2_655 ? O30 Zn1 O30 36(2) 3_665 2_655 ? O30 Zn1 N1 117.1(12) . 2_655 ? O30 Zn1 N1 85.4(13) 3_665 2_655 ? O30 Zn1 N1 113.6(12) 2_655 2_655 ? O30 Zn1 N1 113.6(12) . . ? O30 Zn1 N1 117.1(12) 3_665 . ? O30 Zn1 N1 85.4(13) 2_655 . ? N1 Zn1 N1 112.7(3) 2_655 . ? O30 Zn1 N1 85.4(13) . 3_665 ? O30 Zn1 N1 113.6(12) 3_665 3_665 ? O30 Zn1 N1 117.1(12) 2_655 3_665 ? N1 Zn1 N1 112.7(3) 2_655 3_665 ? N1 Zn1 N1 112.7(3) . 3_665 ? O31 Zn2 N22 106.7(3) . 2_655 ? O31 Zn2 N22 106.7(3) . 3_665 ? N22 Zn2 N22 112.1(2) 2_655 3_665 ? O31 Zn2 N22 106.7(3) . . ? N22 Zn2 N22 112.1(2) 2_655 . ? N22 Zn2 N22 112.1(2) 3_665 . ? C5 N1 C2 102.8(17) . . ? C5 N1 Zn1 127.9(10) . . ? C2 N1 Zn1 129.3(17) . . ? C3 C2 N1 107.1(18) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? N4 C3 C2 106.2(17) . . ? N4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? C3 N4 C5 111.1(18) . . ? C3 N4 C25 117.4(16) . . ? C5 N4 C25 130.9(14) . . ? N1 C5 N4 112.7(13) . . ? N1 C5 C6 123.5(15) . . ? N4 C5 C6 123.2(18) . . ? O7 C6 C5 110.5(10) . . ? O7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 O7 C6 121.9(10) . . ? C9 C8 C13 124.1(11) . . ? C9 C8 O7 117.6(10) . . ? C13 C8 O7 118.3(9) . . ? C8 C9 C10 116.1(11) . . ? C8 C9 C21 121.0(10) . . ? C10 C9 C21 122.7(10) . . ? C11 C10 C9 123.9(11) . . ? C11 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C10 C11 C12 118.2(11) . . ? C10 C11 C26 120.1(12) . . ? C12 C11 C26 121.7(11) . . ? C11 C12 C13 122.2(11) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C8 C13 C12 115.4(10) . . ? C8 C13 C14 124.5(11) . 2_655 ? C12 C13 C14 120.1(10) . 2_655 ? C13 C14 C15 116.4(9) 3_665 . ? C13 C14 H14A 108.2 3_665 . ? C15 C14 H14A 108.2 . . ? C13 C14 H14B 108.2 3_665 . ? C15 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? C16 C15 C20 116.5(10) . . ? C16 C15 C14 123.2(11) . . ? C20 C15 C14 120.3(11) . . ? C17 C16 C15 124.1(12) . . ? C17 C16 O23 117.8(10) . . ? C15 C16 O23 117.5(10) . . ? C16 C17 C18 119.0(11) . . ? C16 C17 C21 122.1(11) . . ? C18 C17 C21 118.8(11) . . ? C17 C18 C19 118.4(10) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C20 C19 C18 121.5(11) . . ? C20 C19 N22 120.2(11) . . ? C18 C19 N22 117.9(11) . . ? C19 C20 C15 120.5(11) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C9 C21 C17 116.9(10) . . ? C9 C21 H21A 108.1 . . ? C17 C21 H21A 108.1 . . ? C9 C21 H21B 108.1 . . ? C17 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C19 N22 Zn2 109.9(8) . . ? C19 N22 H22A 109.7 . . ? Zn2 N22 H22A 109.7 . . ? C19 N22 H22B 109.7 . . ? Zn2 N22 H22B 109.7 . . ? H22A N22 H22B 108.2 . . ? C24 O23 C16 112.1(8) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 H25A 109.5 . . ? N4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 103.6(19) . . ? C27 C26 C29 117.2(17) . . ? C28 C26 C29 110(2) . . ? C27 C26 C11 111.2(13) . . ? C28 C26 C11 109.1(12) . . ? C29 C26 C11 105.8(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O30 O30 O30 60.005(5) 2_655 3_665 ? O30 O30 Zn1 72.1(11) 2_655 . ? O30 O30 Zn1 72.1(11) 3_665 . ? O3 Cl1 O2 136.2(16) . . ? O3 Cl1 O1 103.7(19) . . ? O2 Cl1 O1 114.5(10) . . ? O3 Cl1 O5 103.0(12) . . ? O2 Cl1 O5 51.0(11) . . ? O1 Cl1 O5 100.5(10) . . ? O3 Cl1 O4 104.6(15) . . ? O2 Cl1 O4 91.4(14) . . ? O1 Cl1 O4 97.4(13) . . ? O5 Cl1 O4 142.3(14) . . ? O5 O2 Cl1 69.9(15) . . ? O2 O5 Cl1 59.1(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.792 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.217 #===END