# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Harald Krautscheid' _publ_contact_author_address ; Universit\"at Leipzig Fakult\"at f\"ur Chemie und Mineralogie Institut f\"ur Anorganische Chemie Johannisallee 29 D-04103 Leipzig Germany ; _publ_contact_author_email Krautscheid@rz.uni-leipzig.de _publ_contact_author_phone 00493419736172 _publ_contact_author_fax 00493419736199 loop_ _publ_author_name _publ_author_address 'J\"org Lincke' ;Universit\"at Leipzig Fakult\"at f\"ur Chemie und Mineralogie Institut f\"ur Anorganische Chemie Johannisallee 29 D-04103 Leipzig Germany ; D.Lassig ;Universit\"at Leipzig Fakult\"at f\"ur Chemie und Mineralogie Institut f\"ur Anorganische Chemie Johannisallee 29 D-04103 Leipzig Germany ; 'Karolin Stein' ;Universit\"at Leipzig Fakult\"at f\"ur Chemie und Mineralogie Institut f\"ur Anorganische Chemie Johannisallee 29 D-04103 Leipzig Germany ; J.Mollmer ;Institut f\"ur Nichtklassische Chemie e.V. Permoser Strasse 15 D-4318 Leipzig Germany ; 'Anusree Viswanath Kuttatheyil' ;Universit\"at Leipzig Fakult\"at f\"ur Physik und Geowissenschaften Linnestrasse 5 D-04103 Leipzig Germany ; ; C.Reichenbach ; ;Universit\"at Leipzig Fakult\"at f\"ur Physik und Geowissenschaften Linnestrasse 5 D-04103 Leipzig Germany ; A.Moller ;Institut f\"ur Nichtklassische Chemie e.V. Permoser Strasse 15 D-4318 Leipzig Germany ; 'Reiner Staudt' ;Hochschule Offenburg Fakult\"at Maschinenbau und Verfahrenstechnik Badstrasse 24 D-77652 Offenburg Germany ; 'Grit Kalies' ;Universit\"at Leipzig Fakult\"at f\"ur Physik und Geowissenschaften Linnestrasse 5 D-04103 Leipzig Germany ; 'Marko Bertmer' ;Universit\"at Leipzig Fakult\"at f\"ur Physik und Geowissenschaften Linnestrasse 5 D-04103 Leipzig Germany ; 'Harald Krautscheid' ;Universit\"at Leipzig Fakult\"at f\"ur Chemie und Mineralogie Institut f\"ur Anorganische Chemie Johannisallee 29 D-04103 Leipzig Germany ; data_1-8DMF _database_code_depnum_ccdc_archive 'CCDC 836622' #TrackingRef 'J. Lincke Dalton Trans.cif' #TrackingRef 'J. Lincke Dalton Trans.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn4O{(Metrz-pba)2mPh}3]-8DMF' _chemical_melting_point ? _chemical_formula_moiety 'C78 H54 N18 O13 Zn4, 8(C3 H7 N O)' _chemical_formula_sum 'C102 H110 N26 O21 Zn4' _chemical_formula_weight 2297.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P31c _symmetry_space_group_name_Hall P3-2c _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, z+1/2' '-x+y, -x, z' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 18.9863(11) _cell_length_b 18.9863(11) _cell_length_c 18.0965(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5649.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 15207 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.80 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'STOE IPDS-I' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14932 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.87 _reflns_number_total 5986 _reflns_number_gt 4844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 Sheldrick, G. M. (2008) Acta Cryst.' _computing_structure_refinement 'SHELXL-97 Sheldrick, G. M. (2008) Acta Cryst.' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; There are 8 DMF molecules per formula unit present which could not be localized during single crystal structure refinement. Nevertheless, evidence is given by TG-MS analysis as well as solid state 13C NMR as presented in the paper. Furthermore, application of the PLATON/SQUEEZE routine leads to similar residual R values as obtained for the desolvated compound. 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^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(18) _refine_ls_number_reflns 5986 _refine_ls_number_parameters 342 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.5320(3) 0.3638(4) 0.6051(4) 0.0416(13) Uani 1 1 d . . . C2 C 0.5028(3) 0.4112(3) 0.6496(4) 0.0428(13) Uani 1 1 d . . . C3 C 0.5371(4) 0.4399(5) 0.7192(5) 0.072(2) Uani 1 1 d . . . H3 H 0.5778 0.4300 0.7373 0.087 Uiso 1 1 calc R . . C4 C 0.5104(5) 0.4833(6) 0.7615(6) 0.081(3) Uani 1 1 d . . . H4 H 0.5329 0.5033 0.8084 0.097 Uiso 1 1 calc R . . C5 C 0.4495(4) 0.4967(4) 0.7331(4) 0.0522(16) Uani 1 1 d . . . C6 C 0.4166(4) 0.4694(4) 0.6660(4) 0.0542(17) Uani 1 1 d . . . H6 H 0.3760 0.4796 0.6482 0.065 Uiso 1 1 calc R . . C7 C 0.4425(4) 0.4260(4) 0.6232(4) 0.0505(15) Uani 1 1 d . . . H7 H 0.4195 0.4067 0.5764 0.061 Uiso 1 1 calc R . . C8 C 0.3350(5) 0.4136(4) 0.8631(6) 0.074(3) Uani 1 1 d . . . H8A H 0.2880 0.3974 0.8946 0.111 Uiso 1 1 calc R . . H8B H 0.3754 0.4064 0.8896 0.111 Uiso 1 1 calc R . . H8C H 0.3187 0.3803 0.8189 0.111 Uiso 1 1 calc R . . C9 C 0.3702(3) 0.5002(3) 0.8423(4) 0.0464(14) Uani 1 1 d . . . C10 C 0.4410(3) 0.6174(3) 0.7854(4) 0.0425(13) Uani 1 1 d . . . C11 C 0.7112(4) 0.5711(4) 0.4597(4) 0.0508(15) Uani 1 1 d . . . C12 C 0.6586(3) 0.6119(3) 0.4608(4) 0.0448(14) Uani 1 1 d . . . C13 C 0.6875(4) 0.6884(4) 0.4340(5) 0.065(2) Uani 1 1 d . . . H13 H 0.7400 0.7166 0.4136 0.078 Uiso 1 1 calc R . . C14 C 0.6410(4) 0.7250(4) 0.4362(5) 0.065(2) Uani 1 1 d . . . H14 H 0.6617 0.7776 0.4169 0.078 Uiso 1 1 calc R . . C15 C 0.5641(3) 0.6850(4) 0.4666(4) 0.0447(13) Uani 1 1 d . . . C16 C 0.5328(4) 0.6075(4) 0.4913(4) 0.0525(17) Uani 1 1 d . . . H16 H 0.4794 0.5791 0.5098 0.063 Uiso 1 1 calc R . . C17 C 0.5794(4) 0.5704(4) 0.4893(4) 0.0515(16) Uani 1 1 d . . . H17 H 0.5579 0.5170 0.5071 0.062 Uiso 1 1 calc R . . C18 C 0.4852(6) 0.7290(6) 0.3369(5) 0.076(2) Uani 1 1 d . . . H18A H 0.4522 0.7452 0.3086 0.115 Uiso 1 1 calc R . . H18B H 0.4643 0.6712 0.3304 0.115 Uiso 1 1 calc R . . H18C H 0.5410 0.7590 0.3197 0.115 Uiso 1 1 calc R . . C19 C 0.4820(4) 0.7467(4) 0.4165(4) 0.0552(17) Uani 1 1 d . . . C20 C 0.4965(4) 0.7500(4) 0.5359(4) 0.0508(15) Uani 1 1 d . . . C21 C 0.5239(4) 0.7428(4) 0.6111(4) 0.0493(15) Uani 1 1 d . . . C22 C 0.6038(5) 0.7948(6) 0.6321(5) 0.087(3) Uani 1 1 d . . . H22 H 0.6410 0.8322 0.5980 0.104 Uiso 1 1 calc R . . C23 C 0.6286(5) 0.7916(8) 0.7031(7) 0.118(5) Uani 1 1 d . . . H23 H 0.6823 0.8281 0.7178 0.142 Uiso 1 1 calc R . . C24 C 0.5752(5) 0.7355(6) 0.7522(5) 0.086(3) Uani 1 1 d . . . H24 H 0.5927 0.7349 0.8007 0.103 Uiso 1 1 calc R . . C25 C 0.4972(3) 0.6803(4) 0.7326(4) 0.0454(14) Uani 1 1 d . . . C26 C 0.4716(4) 0.6848(4) 0.6610(4) 0.0477(15) Uani 1 1 d . . . H26 H 0.4179 0.6479 0.6465 0.057 Uiso 1 1 calc R . . N1 N 0.3609(3) 0.5552(3) 0.8772(3) 0.0391(10) Uani 1 1 d . . . N2 N 0.4062(3) 0.6294(3) 0.8422(3) 0.0425(11) Uani 1 1 d . . . N3 N 0.4191(3) 0.5364(3) 0.7824(3) 0.0495(13) Uani 1 1 d . . . N4 N 0.4436(4) 0.7821(4) 0.4438(4) 0.0689(18) Uani 1 1 d . . . N5 N 0.4534(4) 0.7847(4) 0.5213(4) 0.0671(16) Uani 1 1 d . . . N6 N 0.5170(3) 0.7256(3) 0.4716(3) 0.0457(12) Uani 1 1 d . . . O1 O 0.6667 0.3333 0.4921(4) 0.0306(12) Uani 1 3 d S . . O2 O 0.5809(3) 0.3480(3) 0.6401(3) 0.0568(12) Uani 1 1 d . . . O3 O 0.5076(2) 0.3438(2) 0.5412(3) 0.0444(9) Uani 1 1 d . . . O4 O 0.6795(2) 0.5008(2) 0.4883(3) 0.0519(11) Uani 1 1 d . . . O5 O 0.7795(3) 0.6073(3) 0.4311(3) 0.0703(15) Uani 1 1 d . . . Zn1 Zn 0.6667 0.3333 0.59782(6) 0.0328(2) Uani 1 3 d S . . Zn2 Zn 0.74289(3) 0.44777(3) 0.46496(4) 0.03408(16) 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 C1 0.038(3) 0.048(3) 0.041(4) -0.001(3) 0.004(3) 0.023(2) C2 0.040(3) 0.050(3) 0.039(4) -0.006(3) 0.003(2) 0.023(2) C3 0.063(4) 0.111(6) 0.065(6) -0.039(5) -0.016(4) 0.060(4) C4 0.070(4) 0.113(6) 0.077(7) -0.055(5) -0.021(4) 0.058(4) C5 0.048(3) 0.054(3) 0.056(5) -0.008(3) 0.013(3) 0.027(3) C6 0.060(4) 0.070(4) 0.051(5) -0.005(3) 0.005(3) 0.047(3) C7 0.058(3) 0.056(3) 0.045(4) -0.009(3) -0.006(3) 0.034(3) C8 0.079(5) 0.046(3) 0.105(8) 0.007(4) 0.038(5) 0.037(3) C9 0.048(3) 0.045(3) 0.049(4) -0.007(3) 0.009(3) 0.025(2) C10 0.047(3) 0.047(3) 0.036(4) -0.005(2) 0.001(3) 0.026(3) C11 0.063(4) 0.062(4) 0.042(4) -0.007(3) -0.007(3) 0.042(3) C12 0.044(3) 0.048(3) 0.047(4) 0.000(3) 0.005(3) 0.027(3) C13 0.057(4) 0.059(4) 0.089(7) 0.021(4) 0.032(4) 0.036(3) C14 0.067(4) 0.052(3) 0.086(7) 0.022(4) 0.025(4) 0.036(3) C15 0.055(3) 0.046(3) 0.042(4) 0.003(3) 0.006(3) 0.031(3) C16 0.040(3) 0.053(3) 0.067(5) 0.008(3) 0.008(3) 0.025(3) C17 0.050(3) 0.045(3) 0.065(5) 0.004(3) 0.000(3) 0.028(3) C18 0.101(6) 0.097(6) 0.050(5) -0.003(4) -0.005(5) 0.064(5) C19 0.070(4) 0.059(4) 0.050(5) 0.006(3) 0.002(3) 0.042(3) C20 0.060(4) 0.059(3) 0.044(4) 0.006(3) 0.008(3) 0.039(3) C21 0.056(3) 0.058(3) 0.039(4) 0.003(3) 0.008(3) 0.033(3) C22 0.057(4) 0.110(7) 0.055(6) 0.027(5) 0.009(4) 0.013(4) C23 0.057(5) 0.150(9) 0.078(8) 0.044(7) -0.010(5) 0.000(5) C24 0.055(4) 0.115(7) 0.049(6) 0.022(5) 0.000(4) 0.014(4) C25 0.048(3) 0.053(3) 0.037(4) -0.001(3) 0.005(3) 0.026(3) C26 0.049(3) 0.050(3) 0.049(4) -0.003(3) 0.002(3) 0.029(3) N1 0.043(2) 0.042(2) 0.037(3) -0.002(2) 0.003(2) 0.025(2) N2 0.045(2) 0.044(2) 0.041(3) 0.004(2) 0.007(2) 0.024(2) N3 0.058(3) 0.049(3) 0.044(4) -0.005(2) 0.013(3) 0.029(2) N4 0.095(5) 0.082(4) 0.061(5) 0.003(3) -0.001(4) 0.068(4) N5 0.089(4) 0.088(4) 0.056(4) 0.002(3) 0.004(3) 0.069(4) N6 0.057(3) 0.054(3) 0.039(3) 0.003(2) 0.004(2) 0.038(2) O1 0.0349(17) 0.0349(17) 0.022(3) 0.000 0.000 0.0174(9) O2 0.066(3) 0.083(3) 0.041(3) 0.000(2) 0.008(2) 0.051(3) O3 0.045(2) 0.050(2) 0.042(3) -0.0086(19) 0.0030(18) 0.0268(18) O4 0.055(2) 0.048(2) 0.062(3) -0.009(2) -0.011(2) 0.0331(19) O5 0.066(3) 0.097(4) 0.068(4) 0.012(3) 0.018(3) 0.057(3) Zn1 0.0363(3) 0.0363(3) 0.0257(6) 0.000 0.000 0.01817(16) Zn2 0.0355(3) 0.0344(3) 0.0312(3) 0.0034(3) 0.0029(3) 0.0166(2) _geom_special_details ; All s.u. (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u. are taken into account individually in the estimation of s.u. in distances, angles and torsion angles; correlations between s.u. in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u. is used for estimating s.u. 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 C1 O3 1.234(8) . ? C1 O2 1.278(7) . ? C1 C2 1.504(8) . ? C2 C7 1.393(8) . ? C2 C3 1.397(10) . ? C3 C4 1.393(10) . ? C3 H3 0.9400 . ? C4 C5 1.400(10) . ? C4 H4 0.9400 . ? C5 C6 1.344(10) . ? C5 N3 1.460(8) . ? C6 C7 1.389(9) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.481(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 N1 1.305(7) . ? C9 N3 1.368(9) . ? C10 N2 1.301(8) . ? C10 N3 1.379(7) . ? C10 C25 1.485(9) . ? C11 O5 1.238(8) . ? C11 O4 1.267(8) . ? C11 C12 1.539(8) . ? C12 C13 1.360(9) . ? C12 C17 1.401(9) . ? C13 C14 1.369(9) . ? C13 H13 0.9400 . ? C14 C15 1.380(9) . ? C14 H14 0.9400 . ? C15 C16 1.359(8) . ? C15 N6 1.446(7) . ? C16 C17 1.380(8) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C19 1.488(12) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 N4 1.310(9) . ? C19 N6 1.365(9) . ? C20 N5 1.308(8) . ? C20 N6 1.377(9) . ? C20 C21 1.489(10) . ? C21 C26 1.385(9) . ? C21 C22 1.386(10) . ? C22 C23 1.381(14) . ? C22 H22 0.9400 . ? C23 C24 1.369(12) . ? C23 H23 0.9400 . ? C24 C25 1.365(10) . ? C24 H24 0.9400 . ? C25 C26 1.402(9) . ? C26 H26 0.9400 . ? N1 N2 1.384(7) . ? N1 Zn2 2.003(5) 6_565 ? N4 N5 1.413(9) . ? O1 Zn1 1.913(6) . ? O1 Zn2 1.9780(17) 4_665 ? O1 Zn2 1.9780(17) . ? O1 Zn2 1.9780(17) 2_655 ? O2 Zn1 1.941(4) . ? O3 Zn2 2.064(4) 2_655 ? O4 Zn2 1.962(4) . ? Zn1 O2 1.941(4) 2_655 ? Zn1 O2 1.941(4) 4_665 ? Zn1 Zn2 3.0743(11) 4_665 ? Zn1 Zn2 3.0743(11) 2_655 ? Zn1 Zn2 3.0743(11) . ? Zn2 N1 2.003(5) 6_664 ? Zn2 O3 2.064(4) 4_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 O2 126.7(5) . . ? O3 C1 C2 119.5(5) . . ? O2 C1 C2 113.8(6) . . ? C7 C2 C3 120.0(6) . . ? C7 C2 C1 121.5(6) . . ? C3 C2 C1 118.5(5) . . ? C4 C3 C2 119.3(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.9(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 121.9(6) . . ? C6 C5 N3 121.5(6) . . ? C4 C5 N3 116.4(7) . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 120.0(7) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 N3 108.2(5) . . ? N1 C9 C8 126.7(6) . . ? N3 C9 C8 125.1(5) . . ? N2 C10 N3 109.3(5) . . ? N2 C10 C25 126.2(5) . . ? N3 C10 C25 124.5(5) . . ? O5 C11 O4 124.7(6) . . ? O5 C11 C12 119.3(6) . . ? O4 C11 C12 116.0(6) . . ? C13 C12 C17 118.5(5) . . ? C13 C12 C11 121.1(5) . . ? C17 C12 C11 120.3(5) . . ? C12 C13 C14 120.9(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 120.5(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.7(5) . . ? C16 C15 N6 120.4(5) . . ? C14 C15 N6 119.9(5) . . ? C15 C16 C17 120.0(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 120.3(5) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 N6 110.6(7) . . ? N4 C19 C18 125.2(7) . . ? N6 C19 C18 124.1(6) . . ? N5 C20 N6 110.6(6) . . ? N5 C20 C21 124.5(6) . . ? N6 C20 C21 124.8(5) . . ? C26 C21 C22 118.9(7) . . ? C26 C21 C20 121.6(6) . . ? C22 C21 C20 119.6(6) . . ? C23 C22 C21 119.9(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.2(8) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 121.6(9) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 118.1(6) . . ? C24 C25 C10 121.1(7) . . ? C26 C25 C10 120.8(5) . . ? C21 C26 C25 121.1(6) . . ? C21 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C9 N1 N2 109.1(5) . . ? C9 N1 Zn2 133.9(4) . 6_565 ? N2 N1 Zn2 117.0(3) . 6_565 ? C10 N2 N1 107.2(5) . . ? C9 N3 C10 106.2(5) . . ? C9 N3 C5 124.7(5) . . ? C10 N3 C5 128.5(5) . . ? C19 N4 N5 107.1(6) . . ? C20 N5 N4 106.7(6) . . ? C19 N6 C20 104.9(5) . . ? C19 N6 C15 129.2(6) . . ? C20 N6 C15 125.9(6) . . ? Zn1 O1 Zn2 104.39(18) . 4_665 ? Zn1 O1 Zn2 104.39(18) . . ? Zn2 O1 Zn2 114.04(14) 4_665 . ? Zn1 O1 Zn2 104.39(18) . 2_655 ? Zn2 O1 Zn2 114.04(14) 4_665 2_655 ? Zn2 O1 Zn2 114.04(14) . 2_655 ? C1 O2 Zn1 126.8(4) . . ? C1 O3 Zn2 126.1(3) . 2_655 ? C11 O4 Zn2 111.3(4) . . ? O1 Zn1 O2 113.24(16) . 2_655 ? O1 Zn1 O2 113.24(16) . 4_665 ? O2 Zn1 O2 105.45(18) 2_655 4_665 ? O1 Zn1 O2 113.24(16) . . ? O2 Zn1 O2 105.45(18) 2_655 . ? O2 Zn1 O2 105.45(18) 4_665 . ? O1 Zn1 Zn2 38.553(17) . 4_665 ? O2 Zn1 Zn2 78.34(16) 2_655 4_665 ? O2 Zn1 Zn2 109.85(15) 4_665 4_665 ? O2 Zn1 Zn2 142.03(16) . 4_665 ? O1 Zn1 Zn2 38.553(17) . 2_655 ? O2 Zn1 Zn2 109.85(15) 2_655 2_655 ? O2 Zn1 Zn2 142.03(16) 4_665 2_655 ? O2 Zn1 Zn2 78.34(16) . 2_655 ? Zn2 Zn1 Zn2 65.33(3) 4_665 2_655 ? O1 Zn1 Zn2 38.553(17) . . ? O2 Zn1 Zn2 142.03(16) 2_655 . ? O2 Zn1 Zn2 78.34(16) 4_665 . ? O2 Zn1 Zn2 109.85(15) . . ? Zn2 Zn1 Zn2 65.33(3) 4_665 . ? Zn2 Zn1 Zn2 65.33(3) 2_655 . ? O4 Zn2 O1 102.17(14) . . ? O4 Zn2 N1 135.3(2) . 6_664 ? O1 Zn2 N1 106.57(19) . 6_664 ? O4 Zn2 O3 105.45(17) . 4_665 ? O1 Zn2 O3 106.95(18) . 4_665 ? N1 Zn2 O3 98.04(19) 6_664 4_665 ? O4 Zn2 Zn1 90.10(14) . . ? O1 Zn2 Zn1 37.06(18) . . ? N1 Zn2 Zn1 132.58(13) 6_664 . ? O3 Zn2 Zn1 76.82(12) 4_665 . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.785 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.151 data_1 _database_code_depnum_ccdc_archive 'CCDC 836623' #TrackingRef 'J. Lincke Dalton Trans.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn4O{(Metrz-pba)2mPh}3]' _chemical_melting_point ? _chemical_formula_moiety 'C78 H54 N18 O13 Zn4' _chemical_formula_sum 'C78 H54 N18 O13 Zn4' _chemical_formula_weight 1712.87 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 trigonal _symmetry_space_group_name_H-M P31c _symmetry_space_group_name_Hall P3-2c _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, z+1/2' '-x+y, -x, z' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 19.2401(8) _cell_length_b 19.2401(8) _cell_length_c 17.8208(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5713.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 29021 _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24961 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7490 _reflns_number_gt 6941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 Sheldrick, G. M. (2008) Acta Cryst.' _computing_structure_refinement 'SHELXL-97 Sheldrick, G. M. (2008) Acta Cryst.' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0083(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(9) _refine_ls_number_reflns 7490 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _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 C1 C 0.53193(17) 0.36212(17) 0.60689(15) 0.0372(6) Uani 1 1 d . . . C2 C 0.49924(17) 0.40690(18) 0.65005(15) 0.0402(6) Uani 1 1 d . . . C3 C 0.5322(3) 0.4389(3) 0.7196(3) 0.0892(18) Uani 1 1 d . . . H3 H 0.5745 0.4321 0.7388 0.107 Uiso 1 1 calc R . . C4 C 0.5043(3) 0.4802(4) 0.7611(3) 0.0956(18) Uani 1 1 d . . . H4 H 0.5266 0.5009 0.8090 0.115 Uiso 1 1 calc R . . C5 C 0.44335(18) 0.4916(2) 0.73239(18) 0.0477(7) Uani 1 1 d . . . C6 C 0.4099(2) 0.4608(2) 0.66335(18) 0.0492(7) Uani 1 1 d . . . H6 H 0.3682 0.4684 0.6439 0.059 Uiso 1 1 calc R . . C7 C 0.4384(2) 0.4180(2) 0.62212(18) 0.0462(7) Uani 1 1 d . . . H7 H 0.4156 0.3963 0.5745 0.055 Uiso 1 1 calc R . . C8 C 0.3272(2) 0.4109(2) 0.8626(3) 0.0651(10) Uani 1 1 d . . . H8A H 0.2913 0.4001 0.9055 0.098 Uiso 1 1 calc R . . H8B H 0.3699 0.3997 0.8766 0.098 Uiso 1 1 calc R . . H8C H 0.2965 0.3765 0.8204 0.098 Uiso 1 1 calc R . . C9 C 0.36327(17) 0.49660(17) 0.84022(16) 0.0405(6) Uani 1 1 d . . . C10 C 0.43525(16) 0.61196(17) 0.78147(15) 0.0361(6) Uani 1 1 d . . . C11 C 0.70296(18) 0.56446(19) 0.45654(17) 0.0430(6) Uani 1 1 d . . . C12 C 0.65129(17) 0.60370(17) 0.45707(16) 0.0391(6) Uani 1 1 d . . . C13 C 0.6817(2) 0.6808(2) 0.4277(2) 0.0537(8) Uani 1 1 d . . . H13 H 0.7341 0.7078 0.4068 0.064 Uiso 1 1 calc R . . C14 C 0.6356(2) 0.7186(2) 0.4289(2) 0.0539(8) Uani 1 1 d . . . H14 H 0.6570 0.7714 0.4095 0.065 Uiso 1 1 calc R . . C15 C 0.55894(17) 0.67889(17) 0.45849(16) 0.0383(6) Uani 1 1 d . . . C16 C 0.52587(18) 0.60065(18) 0.48567(17) 0.0411(6) Uani 1 1 d . . . H16 H 0.4725 0.5729 0.5045 0.049 Uiso 1 1 calc R . . C17 C 0.57288(18) 0.56396(17) 0.48465(17) 0.0415(6) Uani 1 1 d . . . H17 H 0.5509 0.5108 0.5032 0.050 Uiso 1 1 calc R . . C18 C 0.4829(3) 0.7238(3) 0.3255(2) 0.0654(10) Uani 1 1 d . . . H18A H 0.4470 0.7362 0.2968 0.098 Uiso 1 1 calc R . . H18B H 0.4658 0.6668 0.3198 0.098 Uiso 1 1 calc R . . H18C H 0.5379 0.7565 0.3069 0.098 Uiso 1 1 calc R . . C19 C 0.4798(2) 0.74197(19) 0.40624(18) 0.0450(7) Uani 1 1 d . . . C20 C 0.49313(18) 0.74494(18) 0.52835(17) 0.0416(6) Uani 1 1 d . . . C21 C 0.51951(19) 0.73580(19) 0.60423(17) 0.0441(6) Uani 1 1 d . . . C22 C 0.5982(2) 0.7861(3) 0.6257(2) 0.0856(15) Uani 1 1 d . . . H22 H 0.6354 0.8240 0.5911 0.103 Uiso 1 1 calc R . . C23 C 0.6230(3) 0.7813(4) 0.6972(3) 0.132(3) Uani 1 1 d . . . H23 H 0.6768 0.8172 0.7119 0.159 Uiso 1 1 calc R . . C24 C 0.5700(2) 0.7242(4) 0.7481(2) 0.0975(19) Uani 1 1 d . . . H24 H 0.5877 0.7209 0.7971 0.117 Uiso 1 1 calc R . . C25 C 0.49118(18) 0.67231(19) 0.72671(16) 0.0418(6) Uani 1 1 d . . . C26 C 0.46592(18) 0.67853(18) 0.65503(16) 0.0393(6) Uani 1 1 d . . . H26 H 0.4118 0.6436 0.6405 0.047 Uiso 1 1 calc R . . N1 N 0.35576(13) 0.55240(13) 0.87471(12) 0.0334(5) Uani 1 1 d . . . N2 N 0.40161(14) 0.62591(13) 0.83869(13) 0.0368(5) Uani 1 1 d . . . N3 N 0.41226(16) 0.53101(15) 0.77927(15) 0.0466(6) Uani 1 1 d . . . N4 N 0.4433(2) 0.77897(19) 0.43395(17) 0.0571(7) Uani 1 1 d . . . N5 N 0.45178(18) 0.78020(19) 0.51280(16) 0.0552(7) Uani 1 1 d . . . N6 N 0.51329(15) 0.71979(15) 0.46375(13) 0.0387(5) Uani 1 1 d . . . O1 O 0.6667 0.3333 0.49218(16) 0.0283(6) Uani 1 3 d S . . O2 O 0.58291(14) 0.35058(15) 0.64204(11) 0.0482(5) Uani 1 1 d . . . O3 O 0.50717(12) 0.33915(12) 0.54142(11) 0.0387(4) Uani 1 1 d . . . O4 O 0.67273(13) 0.49571(12) 0.48802(12) 0.0452(5) Uani 1 1 d . . . O5 O 0.76942(15) 0.59887(17) 0.42559(15) 0.0606(6) Uani 1 1 d . . . Zn1 Zn 0.6667 0.3333 0.60008(2) 0.02906(12) Uani 1 3 d S . . Zn2 Zn 0.739513(16) 0.447280(16) 0.465174(15) 0.02929(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0355(13) 0.0414(14) 0.0347(14) -0.0012(11) 0.0040(11) 0.0191(12) C2 0.0366(14) 0.0457(15) 0.0375(14) -0.0092(12) 0.0018(11) 0.0199(12) C3 0.075(3) 0.149(5) 0.079(3) -0.074(3) -0.038(2) 0.083(3) C4 0.073(3) 0.153(5) 0.089(3) -0.082(3) -0.037(2) 0.077(3) C5 0.0444(16) 0.0495(17) 0.0485(17) -0.0157(13) 0.0085(13) 0.0229(14) C6 0.0586(19) 0.0617(19) 0.0435(16) -0.0054(14) 0.0044(14) 0.0424(17) C7 0.0558(18) 0.0544(17) 0.0405(15) -0.0084(13) -0.0010(13) 0.0365(15) C8 0.064(2) 0.0427(17) 0.093(3) 0.0006(18) 0.026(2) 0.0292(17) C9 0.0409(14) 0.0383(14) 0.0450(15) -0.0046(11) 0.0086(12) 0.0219(12) C10 0.0353(13) 0.0457(15) 0.0298(12) -0.0038(11) 0.0022(10) 0.0222(12) C11 0.0438(16) 0.0502(16) 0.0411(15) -0.0045(13) -0.0055(13) 0.0280(14) C12 0.0394(14) 0.0420(14) 0.0419(14) -0.0023(12) -0.0002(11) 0.0250(12) C13 0.0447(17) 0.0514(18) 0.071(2) 0.0150(16) 0.0218(15) 0.0282(15) C14 0.0530(18) 0.0446(17) 0.072(2) 0.0191(15) 0.0206(16) 0.0307(15) C15 0.0451(15) 0.0430(14) 0.0358(13) 0.0003(11) 0.0018(11) 0.0287(13) C16 0.0372(14) 0.0414(15) 0.0493(16) 0.0080(12) 0.0054(12) 0.0229(12) C17 0.0395(14) 0.0360(14) 0.0521(16) 0.0062(12) 0.0023(12) 0.0213(12) C18 0.090(3) 0.088(3) 0.0404(18) -0.0036(17) -0.0090(18) 0.061(2) C19 0.0541(17) 0.0491(17) 0.0422(16) 0.0056(13) -0.0006(13) 0.0335(15) C20 0.0453(15) 0.0460(16) 0.0400(15) 0.0014(12) 0.0044(12) 0.0277(14) C21 0.0474(16) 0.0507(17) 0.0389(15) -0.0010(13) 0.0054(13) 0.0280(14) C22 0.053(2) 0.110(4) 0.051(2) 0.025(2) 0.0050(17) 0.008(2) C23 0.052(2) 0.177(6) 0.065(3) 0.043(3) -0.012(2) -0.019(3) C24 0.044(2) 0.143(5) 0.048(2) 0.027(2) -0.0049(16) 0.004(2) C25 0.0392(14) 0.0499(16) 0.0336(13) -0.0002(12) 0.0052(11) 0.0202(13) C26 0.0397(14) 0.0408(14) 0.0410(15) 0.0000(11) 0.0043(12) 0.0228(12) N1 0.0351(11) 0.0345(11) 0.0331(11) -0.0013(9) 0.0015(9) 0.0192(9) N2 0.0394(12) 0.0354(11) 0.0368(11) 0.0023(9) 0.0062(9) 0.0196(10) N3 0.0489(14) 0.0403(13) 0.0503(14) -0.0086(11) 0.0132(11) 0.0220(11) N4 0.073(2) 0.0657(18) 0.0547(17) 0.0021(14) -0.0036(14) 0.0514(17) N5 0.0692(19) 0.0676(18) 0.0517(15) -0.0044(14) -0.0010(13) 0.0513(16) N6 0.0478(13) 0.0419(12) 0.0360(12) 0.0024(9) 0.0019(10) 0.0297(11) O1 0.0285(9) 0.0285(9) 0.0278(14) 0.000 0.000 0.0142(4) O2 0.0534(12) 0.0712(15) 0.0319(10) -0.0035(10) 0.0032(9) 0.0401(12) O3 0.0389(10) 0.0417(10) 0.0383(10) -0.0073(8) -0.0001(8) 0.0223(8) O4 0.0505(12) 0.0398(11) 0.0512(12) -0.0055(9) -0.0093(9) 0.0272(10) O5 0.0541(14) 0.0800(17) 0.0644(15) 0.0081(13) 0.0120(12) 0.0460(13) Zn1 0.03220(16) 0.03220(16) 0.0228(2) 0.000 0.000 0.01610(8) Zn2 0.02986(15) 0.02923(15) 0.02766(14) 0.00214(11) 0.00131(11) 0.01394(12) _geom_special_details ; All s.u. (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u. are taken into account individually in the estimation of s.u. in distances, angles and torsion angles; correlations between s.u. in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u. is used for estimating s.u. 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 C1 O3 1.254(4) . ? C1 O2 1.274(4) . ? C1 C2 1.507(4) . ? C2 C7 1.384(4) . ? C2 C3 1.389(5) . ? C3 C4 1.376(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.378(5) . ? C5 N3 1.443(4) . ? C6 C7 1.403(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.487(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.307(3) . ? C9 N3 1.372(4) . ? C10 N2 1.306(4) . ? C10 N3 1.391(4) . ? C10 C25 1.486(4) . ? C11 O5 1.237(4) . ? C11 O4 1.278(4) . ? C11 C12 1.520(4) . ? C12 C13 1.395(4) . ? C12 C17 1.396(4) . ? C13 C14 1.401(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.396(4) . ? C15 N6 1.446(4) . ? C16 C17 1.398(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.488(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N4 1.322(4) . ? C19 N6 1.386(4) . ? C20 N5 1.308(4) . ? C20 N6 1.377(4) . ? C20 C21 1.485(4) . ? C21 C22 1.382(5) . ? C21 C26 1.400(4) . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.396(6) . ? C23 H23 0.9500 . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C25 C26 1.393(4) . ? C26 H26 0.9500 . ? N1 N2 1.394(3) . ? N1 Zn2 2.025(2) 6_565 ? N4 N5 1.414(4) . ? O1 Zn1 1.923(3) . ? O1 Zn2 1.9823(7) 4_665 ? O1 Zn2 1.9823(7) . ? O1 Zn2 1.9823(7) 2_655 ? O2 Zn1 1.950(2) . ? O3 Zn2 2.0542(18) 2_655 ? O4 Zn2 1.970(2) . ? Zn1 O2 1.950(2) 2_655 ? Zn1 O2 1.950(2) 4_665 ? Zn1 Zn2 3.0787(4) 4_665 ? Zn1 Zn2 3.0787(4) 2_655 ? Zn1 Zn2 3.0787(4) . ? Zn2 N1 2.025(2) 6_664 ? Zn2 O3 2.0542(18) 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 O3 C1 O2 125.9(3) . . ? O3 C1 C2 118.9(2) . . ? O2 C1 C2 115.3(2) . . ? C7 C2 C3 119.2(3) . . ? C7 C2 C1 122.1(3) . . ? C3 C2 C1 118.7(3) . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 N3 121.1(3) . . ? C4 C5 N3 118.2(3) . . ? C5 C6 C7 119.0(3) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C2 C7 C6 120.7(3) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 N3 107.9(2) . . ? N1 C9 C8 127.0(3) . . ? N3 C9 C8 125.1(3) . . ? N2 C10 N3 109.8(2) . . ? N2 C10 C25 126.3(3) . . ? N3 C10 C25 123.9(2) . . ? O5 C11 O4 124.3(3) . . ? O5 C11 C12 119.7(3) . . ? O4 C11 C12 116.1(3) . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C11 119.6(3) . . ? C17 C12 C11 121.8(3) . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.9(3) . . ? C14 C15 N6 119.7(3) . . ? C16 C15 N6 119.4(3) . . ? C15 C16 C17 118.6(3) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C12 C17 C16 121.5(3) . . ? C12 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 N6 110.1(3) . . ? N4 C19 C18 125.6(3) . . ? N6 C19 C18 124.3(3) . . ? N5 C20 N6 110.9(3) . . ? N5 C20 C21 125.9(3) . . ? N6 C20 C21 123.1(3) . . ? C22 C21 C26 119.3(3) . . ? C22 C21 C20 119.2(3) . . ? C26 C21 C20 121.4(3) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.8(4) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 C10 119.0(3) . . ? C26 C25 C10 121.4(3) . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C9 N1 N2 110.1(2) . . ? C9 N1 Zn2 133.8(2) . 6_565 ? N2 N1 Zn2 116.13(16) . 6_565 ? C10 N2 N1 106.2(2) . . ? C9 N3 C10 106.0(2) . . ? C9 N3 C5 124.8(3) . . ? C10 N3 C5 128.4(3) . . ? C19 N4 N5 107.0(3) . . ? C20 N5 N4 107.3(3) . . ? C20 N6 C19 104.7(2) . . ? C20 N6 C15 126.8(2) . . ? C19 N6 C15 128.4(2) . . ? Zn1 O1 Zn2 104.05(8) . 4_665 ? Zn1 O1 Zn2 104.05(8) . . ? Zn2 O1 Zn2 114.31(6) 4_665 . ? Zn1 O1 Zn2 104.05(8) . 2_655 ? Zn2 O1 Zn2 114.31(6) 4_665 2_655 ? Zn2 O1 Zn2 114.31(6) . 2_655 ? C1 O2 Zn1 127.97(18) . . ? C1 O3 Zn2 126.86(18) . 2_655 ? C11 O4 Zn2 109.38(19) . . ? O1 Zn1 O2 112.55(6) . 2_655 ? O1 Zn1 O2 112.55(6) . 4_665 ? O2 Zn1 O2 106.22(7) 2_655 4_665 ? O1 Zn1 O2 112.55(6) . . ? O2 Zn1 O2 106.22(7) 2_655 . ? O2 Zn1 O2 106.22(7) 4_665 . ? O1 Zn1 Zn2 38.655(7) . 4_665 ? O2 Zn1 Zn2 78.47(6) 2_655 4_665 ? O2 Zn1 Zn2 107.40(7) 4_665 4_665 ? O2 Zn1 Zn2 143.07(7) . 4_665 ? O1 Zn1 Zn2 38.655(7) . 2_655 ? O2 Zn1 Zn2 107.40(7) 2_655 2_655 ? O2 Zn1 Zn2 143.07(7) 4_665 2_655 ? O2 Zn1 Zn2 78.47(6) . 2_655 ? Zn2 Zn1 Zn2 65.496(12) 4_665 2_655 ? O1 Zn1 Zn2 38.655(7) . . ? O2 Zn1 Zn2 143.07(7) 2_655 . ? O2 Zn1 Zn2 78.47(6) 4_665 . ? O2 Zn1 Zn2 107.40(7) . . ? Zn2 Zn1 Zn2 65.496(12) 4_665 . ? Zn2 Zn1 Zn2 65.496(12) 2_655 . ? O4 Zn2 O1 101.84(7) . . ? O4 Zn2 N1 134.52(9) . 6_664 ? O1 Zn2 N1 106.80(9) . 6_664 ? O4 Zn2 O3 106.98(8) . 4_665 ? O1 Zn2 O3 107.09(8) . 4_665 ? N1 Zn2 O3 97.51(9) 6_664 4_665 ? O4 Zn2 Zn1 90.17(6) . . ? O1 Zn2 Zn1 37.30(8) . . ? N1 Zn2 Zn1 133.11(6) 6_664 . ? O3 Zn2 Zn1 77.06(6) 4_665 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.374 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.074