# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1563 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H54 N12 O12 Zn3' _chemical_formula_weight 1187.14 _chemical_melting_point ? _chemical_compound_source ? 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 Rhombohedral _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 17.661(2) _cell_length_b 17.661(2) _cell_length_c 20.722(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5597.5(14) _cell_formula_units_Z 3 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 15.57 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.057 _exptl_crystal_density_method ? _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8041 _exptl_absorpt_correction_T_max 0.9416 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.89 _diffrn_reflns_number 2385 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.96 _reflns_number_total 2081 _reflns_number_observed 938 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 40 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1209P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(8) _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 0.00 _refine_ls_number_reflns 2041 _refine_ls_number_parameters 115 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_obs 0.0684 _refine_ls_wR_factor_all 0.3411 _refine_ls_wR_factor_obs 0.1641 _refine_ls_goodness_of_fit_all 0.811 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.582 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn Zn 0.70262(8) 1.0000 1.0000 0.1122(8) Uani 1 d S . O1 O 0.7014(7) 1.0967(9) 0.9677(4) 0.215(6) Uani 1 d D . O2 O 0.5794(7) 1.0144(7) 0.9143(6) 0.220(5) Uani 1 d D . N1 N 0.7415(5) 0.9457(5) 0.9311(3) 0.103(2) Uani 1 d D . N2 N 0.7804(4) 0.9180(5) 0.8386(3) 0.089(2) Uani 1 d . . C1 C 0.7438(6) 0.8708(7) 0.9362(5) 0.113(2) Uani 1 d . . H1 H 0.7307(6) 0.8362(7) 0.9729(5) 0.136 Uiso 1 calc R . C2 C 0.7685(6) 0.8548(6) 0.8781(5) 0.107(3) Uani 1 d . . H2 H 0.7756(6) 0.8074(6) 0.8681(5) 0.129 Uiso 1 calc R . C3 C 0.7645(5) 0.9721(5) 0.8710(3) 0.094(2) Uani 1 d D . H3 H 0.7688(5) 1.0228(5) 0.8538(3) 0.113 Uiso 1 calc R . C4 C 0.8108(5) 0.9290(6) 0.7727(4) 0.101(2) Uani 1 d . . H4A H 0.7960(5) 0.9680(6) 0.7502(4) 0.122 Uiso 1 calc R . H4B H 0.7822(5) 0.8729(6) 0.7508(4) 0.122 Uiso 1 calc R . C5 C 0.9120(5) 0.9677(6) 0.7715(3) 0.079(2) Uani 1 d . . C6 C 0.9674(6) 1.0551(6) 0.7706(3) 0.087(2) Uani 1 d . . H6 H 0.9452(6) 1.0930(6) 0.7693(3) 0.104 Uiso 1 calc R . C7 C 0.6378(7) 1.0863(7) 0.9349(6) 0.215(10) Uani 1 d D . C8 C 0.6359(22) 1.1668(13) 0.9249(6) 0.335(19) Uani 1 d D . H8A H 0.6865(22) 1.2146(13) 0.9445(6) 0.335 Uiso 1 calc R . H8B H 0.5840(22) 1.1615(13) 0.9442(6) 0.335 Uiso 1 calc R . H8C H 0.6359(22) 1.1773(13) 0.8795(6) 0.335 Uiso 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 Zn 0.1088(9) 0.1370(15) 0.1003(9) -0.0347(10) -0.0173(5) 0.0685(7) O1 0.202(10) 0.337(16) 0.127(6) -0.082(8) -0.058(7) 0.150(10) O2 0.293(14) 0.189(10) 0.213(10) -0.080(9) -0.060(10) 0.148(10) N1 0.106(5) 0.100(6) 0.109(5) -0.016(4) -0.016(4) 0.055(4) N2 0.081(4) 0.096(5) 0.093(4) -0.009(5) -0.005(4) 0.047(3) C1 0.112(7) 0.115(7) 0.110(6) -0.002(6) 0.006(5) 0.055(6) C2 0.103(6) 0.095(6) 0.127(7) -0.018(6) -0.001(5) 0.052(5) C3 0.082(5) 0.101(6) 0.100(6) -0.009(5) -0.014(4) 0.047(5) C4 0.087(6) 0.131(7) 0.089(5) -0.018(5) -0.025(4) 0.057(5) C5 0.069(5) 0.092(6) 0.068(4) -0.002(4) -0.007(3) 0.034(5) C6 0.098(7) 0.104(7) 0.077(4) 0.004(4) -0.016(4) 0.064(6) C7 0.404(34) 0.135(12) 0.158(13) -0.015(11) 0.059(18) 0.173(18) C8 0.702(61) 0.374(34) 0.113(9) -0.024(13) 0.018(17) 0.408(44) _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 Zn O1 1.84(2) 5_677 ? Zn O1 1.84(2) . ? Zn N1 2.022(7) 5_677 ? Zn N1 2.022(7) . ? O1 C7 1.246(4) . ? O2 C7 1.245(4) . ? N1 C3 1.322(4) . ? N1 C1 1.348(12) . ? N2 C3 1.308(9) . ? N2 C2 1.314(10) . ? N2 C4 1.444(10) . ? C1 C2 1.357(12) . ? C4 C5 1.562(11) . ? C5 C6 1.353(10) . ? C5 C6 1.365(10) 2_765 ? C6 C5 1.365(10) 3_675 ? C7 C8 1.452(4) . ? 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 O1 Zn O1 123.3(7) 5_677 . ? O1 Zn N1 110.3(4) 5_677 5_677 ? O1 Zn N1 101.5(4) . 5_677 ? O1 Zn N1 101.5(4) 5_677 . ? O1 Zn N1 110.3(4) . . ? N1 Zn N1 109.6(4) 5_677 . ? C7 O1 Zn 119.2(10) . . ? C3 N1 C1 105.4(7) . . ? C3 N1 Zn 128.0(6) . . ? C1 N1 Zn 126.5(6) . . ? C3 N2 C2 107.4(6) . . ? C3 N2 C4 126.0(8) . . ? C2 N2 C4 126.5(7) . . ? N1 C1 C2 107.8(9) . . ? N2 C2 C1 107.9(8) . . ? N2 C3 N1 111.5(7) . . ? N2 C4 C5 109.9(6) . . ? C6 C5 C6 119.5(8) . 2_765 ? C6 C5 C4 121.1(8) . . ? C6 C5 C4 119.4(8) 2_765 . ? C5 C6 C5 120.4(8) . 3_675 ? O2 C7 O1 124.2(11) . . ? O2 C7 C8 122.5(16) . . ? O1 C7 C8 113.2(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn O1 C7 -39.0(10) 5_677 . . . ? N1 Zn O1 C7 -163.0(10) 5_677 . . . ? N1 Zn O1 C7 80.9(11) . . . . ? O1 Zn N1 C3 133.0(8) 5_677 . . . ? O1 Zn N1 C3 0.6(8) . . . . ? N1 Zn N1 C3 -110.4(8) 5_677 . . . ? O1 Zn N1 C1 -42.4(8) 5_677 . . . ? O1 Zn N1 C1 -174.7(7) . . . . ? N1 Zn N1 C1 74.3(7) 5_677 . . . ? C3 N1 C1 C2 0.0(10) . . . . ? Zn N1 C1 C2 176.2(6) . . . . ? C3 N2 C2 C1 0.5(9) . . . . ? C4 N2 C2 C1 177.0(8) . . . . ? N1 C1 C2 N2 -0.3(10) . . . . ? C2 N2 C3 N1 -0.5(9) . . . . ? C4 N2 C3 N1 -177.1(7) . . . . ? C1 N1 C3 N2 0.3(9) . . . . ? Zn N1 C3 N2 -175.8(5) . . . . ? C3 N2 C4 C5 98.0(8) . . . . ? C2 N2 C4 C5 -78.0(11) . . . . ? N2 C4 C5 C6 -89.9(9) . . . . ? N2 C4 C5 C6 90.9(8) . . . 2_765 ? C6 C5 C6 C5 -2.8(13) 2_765 . . 3_675 ? C4 C5 C6 C5 178.0(5) . . . 3_675 ? Zn O1 C7 O2 -10.6(19) . . . . ? Zn O1 C7 C8 167.1(10) . . . . ? _refine_diff_density_max 0.434 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.073 #===END