# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1391 data_aquaZnTCPP _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '(C48 H28 N4 O8 Zn).(H2 O).4(C6 H5 N O2)' _chemical_formula_sum 'C72 H50 N8 O17 Zn' _chemical_formula_weight 1364.57 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' 'Zn' 'Zn' 0.2839 1.4301 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.6220(10) _cell_length_b 29.6490(10) _cell_length_c 7.5130(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 99.239(10) _cell_angle_gamma 90.000(10) _cell_volume 4314.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 115 _cell_measurement_reflns_used 2300 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.7 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 115 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.5 degree Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6103 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.91 _reflns_number_total 3629 _reflns_number_gt 2096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'DENZO' _computing_data_reduction 'DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep & InsightII' _computing_publication_material ? #==================================================================== # Refinement results after the SQUEEZE/BYPASS procedure #==================================================================== _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. This refinement is based on diffraction data from which the contribution of the heavily disordered nitrobenzene solvent was substracted by the SQUEEZE procedure (Spek, 1990). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3629 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1982 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.009 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.5644(2) 0.0000 0.7409(4) 0.0617(10) Uani 1 d S . . N2 N 0.5000 0.06915(11) 0.5000 0.0587(10) Uani 1 d S . . C3 C 0.53584(17) 0.09716(10) 0.6296(4) 0.0594(8) Uani 1 d . . . C4 C 0.57945(18) 0.08239(10) 0.7856(4) 0.0601(8) Uani 1 d . . . C5 C 0.59335(18) 0.03714(10) 0.8316(4) 0.0622(9) Uani 1 d . . . C6 C 0.64493(19) 0.02298(11) 0.9820(4) 0.0783(11) Uani 1 d . . . H6 H 0.6726 0.0417 1.0628 0.082(10) Uiso 1 calc R . . C7 C 0.52117(18) 0.14399(10) 0.5800(4) 0.0624(9) Uani 1 d . . . H7 H 0.5379 0.1693 0.6464 0.075 Uiso 1 calc R . . C8 C 0.61229(18) 0.11706(11) 0.9185(4) 0.0615(9) Uani 1 d . . . C9 C 0.59740(19) 0.11607(11) 1.0940(4) 0.0693(10) Uani 1 d . . . H9 H 0.5661 0.0950 1.1250 0.069(10) Uiso 1 calc R . . C10 C 0.6288(2) 0.14616(12) 1.2220(4) 0.0772(11) Uani 1 d . . . H10 H 0.6197 0.1447 1.3395 0.086(11) Uiso 1 calc R . . C11 C 0.6738(2) 0.17843(12) 1.1765(4) 0.0793(11) Uani 1 d . . . C12 C 0.6882(2) 0.18011(13) 1.0007(4) 0.0828(12) Uani 1 d . . . H12 H 0.7186 0.2016 0.9693 0.069(10) Uiso 1 calc R . . C13 C 0.65710(19) 0.14961(11) 0.8729(4) 0.0733(10) Uani 1 d . . . H13 H 0.6664 0.1510 0.7555 0.073(10) Uiso 1 calc R . . C14 C 0.7074(2) 0.21033(13) 1.3150(5) 0.0906(13) Uani 1 d . . . O15 O 0.69513(16) 0.20576(9) 1.4754(3) 0.1057(10) Uani 1 d . . . O16 O 0.74710(18) 0.24027(10) 1.2697(3) 0.1149(12) Uani 1 d . . . H16 H 0.7710 0.2643 1.3553 0.100 Uiso 1 d . . . Zn17 Zn 0.5000 0.0000 0.5000 0.0739(4) Uani 1 d S . . O18 O 0.6049(5) 0.0000 0.3610(9) 0.104(3) Uani 0.50 d SP . . H18A H 0.6553 0.0000 0.4213 0.100 Uiso 0.50 d SP . . H18B H 0.6055 0.0000 0.2316 0.100 Uiso 0.50 d SP . . 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 N1 0.083(3) 0.056(2) 0.041(2) 0.000 -0.0070(17) 0.000 N2 0.078(3) 0.058(2) 0.038(2) 0.000 0.0015(16) 0.000 C3 0.081(2) 0.0568(19) 0.0385(17) -0.0055(13) 0.0037(14) -0.0100(17) C4 0.083(2) 0.0584(19) 0.0369(17) -0.0022(13) 0.0025(14) -0.0104(18) C5 0.084(2) 0.059(2) 0.0373(19) -0.0046(13) -0.0109(14) -0.0094(17) C6 0.098(3) 0.077(2) 0.049(2) -0.0033(15) -0.0235(17) -0.0048(19) C7 0.093(3) 0.0501(17) 0.0433(18) -0.0030(12) 0.0085(15) -0.0092(17) C8 0.078(2) 0.0559(19) 0.048(2) -0.0066(13) 0.0017(15) -0.0179(17) C9 0.095(3) 0.067(2) 0.043(2) -0.0054(14) 0.0010(16) -0.028(2) C10 0.112(3) 0.084(2) 0.035(2) -0.0107(15) 0.0091(17) -0.032(2) C11 0.115(3) 0.076(2) 0.046(2) -0.0100(16) 0.0103(18) -0.037(2) C12 0.120(3) 0.084(2) 0.046(2) -0.0118(16) 0.0182(19) -0.044(2) C13 0.104(3) 0.078(2) 0.037(2) -0.0116(15) 0.0104(16) -0.026(2) C14 0.140(4) 0.085(3) 0.046(2) -0.0195(17) 0.011(2) -0.060(3) O15 0.164(3) 0.110(2) 0.0458(16) -0.0245(13) 0.0240(15) -0.0757(19) O16 0.182(3) 0.111(2) 0.0528(15) -0.0263(13) 0.0223(15) -0.098(2) Zn17 0.1167(8) 0.0507(5) 0.0410(5) 0.000 -0.0278(4) 0.000 O18 0.144(7) 0.117(6) 0.054(4) 0.000 0.025(4) 0.000 _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 N1 C5 1.370(3) 6 ? N1 C5 1.370(3) . ? N1 Zn17 2.034(3) . ? N2 C3 1.383(3) 2_656 ? N2 C3 1.383(3) . ? N2 Zn17 2.050(3) . ? C3 C4 1.406(4) . ? C3 C7 1.454(4) . ? C4 C5 1.401(4) . ? C4 C8 1.504(4) . ? C5 C6 1.453(4) . ? C6 C6 1.363(7) 6 ? C6 H6 0.9300 . ? C7 C7 1.347(6) 2_656 ? C7 H7 0.9300 . ? C8 C13 1.385(4) . ? C8 C9 1.396(4) . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 C12 1.395(4) . ? C11 C14 1.481(5) . ? C12 C13 1.387(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O15 1.273(4) . ? C14 O16 1.263(4) . ? O16 H16 1.0217 . ? Zn17 N1 2.034(3) 5_656 ? Zn17 N2 2.050(3) 5_656 ? Zn17 O18 2.453(8) 5_656 ? Zn17 O18 2.453(8) . ? O18 H18A 1.0198 . ? O18 H18B 0.9744 . ? 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 C5 N1 C5 107.0(3) 6 . ? C5 N1 Zn17 126.29(17) 6 . ? C5 N1 Zn17 126.29(17) . . ? C3 N2 C3 106.2(3) 2_656 . ? C3 N2 Zn17 126.91(17) 2_656 . ? C3 N2 Zn17 126.90(17) . . ? N2 C3 C4 124.9(3) . . ? N2 C3 C7 109.6(3) . . ? C4 C3 C7 125.5(3) . . ? C5 C4 C3 124.9(3) . . ? C5 C4 C8 116.4(3) . . ? C3 C4 C8 118.6(3) . . ? N1 C5 C4 126.7(3) . . ? N1 C5 C6 109.7(3) . . ? C4 C5 C6 123.5(3) . . ? C6 C6 C5 106.80(18) 6 . ? C6 C6 H6 126.6 6 . ? C5 C6 H6 126.6 . . ? C7 C7 C3 107.29(17) 2_656 . ? C7 C7 H7 126.4 2_656 . ? C3 C7 H7 126.4 . . ? C13 C8 C9 119.1(3) . . ? C13 C8 C4 122.2(3) . . ? C9 C8 C4 118.7(3) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 C14 119.9(3) . . ? C12 C11 C14 120.5(3) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C8 C13 C12 120.6(3) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? O15 C14 O16 123.2(3) . . ? O15 C14 C11 117.8(3) . . ? O16 C14 C11 118.9(3) . . ? C14 O16 H16 124.1 . . ? N1 Zn17 N1 179.999(1) . 5_656 ? N1 Zn17 N2 90.000(11) . 5_656 ? N1 Zn17 N2 90.000(11) 5_656 5_656 ? N1 Zn17 N2 90.000(11) . . ? N1 Zn17 N2 90.000(11) 5_656 . ? N2 Zn17 N2 180.0 5_656 . ? N1 Zn17 O18 93.7(2) . 5_656 ? N1 Zn17 O18 86.3(2) 5_656 5_656 ? N2 Zn17 O18 90.000(10) 5_656 5_656 ? N2 Zn17 O18 90.000(9) . 5_656 ? N1 Zn17 O18 86.3(2) . . ? N1 Zn17 O18 93.7(2) 5_656 . ? N2 Zn17 O18 90.000(9) 5_656 . ? N2 Zn17 O18 90.000(10) . . ? O18 Zn17 O18 180.0 5_656 . ? Zn17 O18 H18A 129.2 . . ? Zn17 O18 H18B 124.8 . . ? H18A O18 H18B 106.1 . . ? _diffrn_measured_fraction_theta_max 0.452 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.452 _refine_diff_density_max 0.404 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.053 #=============END=============================================